CN101787577B - Novel method for preparing gel fiber - Google Patents
Novel method for preparing gel fiber Download PDFInfo
- Publication number
- CN101787577B CN101787577B CN2010100231807A CN201010023180A CN101787577B CN 101787577 B CN101787577 B CN 101787577B CN 2010100231807 A CN2010100231807 A CN 2010100231807A CN 201010023180 A CN201010023180 A CN 201010023180A CN 101787577 B CN101787577 B CN 101787577B
- Authority
- CN
- China
- Prior art keywords
- solvent
- spinning
- temperature
- polymer
- screw rod
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention provides a method for preparing gel fiber, in particular providing a method for preparing gel fiber by improving the concentration of spinning solution through the steps of dissolving, pelleting, deoiling, melting spinning, pre-stretching and winding. The method is implemented as follows: mixing polymer powder and solvent, heating and stirring, preparing into melt strips after the polymer powder is completely dissolved, cooling to lead the melt strips to be in gel fiber shape and pelleting, removing part of solvent from the pellets after pelleting, melting spinning the polymer gel fiber pellets after solvent removal, and pre-stretching and winding after a coagulating bath to prepare the polymer gel fiber with high solid content. The invention greatly improves the solid content of the polymer in the gel fiber in the prior art so as to enhance the production efficiency and single yield of the existing equipment, reduces the utilization and consumption of solvent and extractant of production capacity per unit, lessens emission, is favor of environment protection and energy conservation, and brings down the production cost.
Description
Technical field
The present invention relates to a kind of preparation method of gel fiber; Particularly relate to a kind of method that improves spinning solution prepared at concentrations gel fiber that adopts, specifically a kind of preparation method of the gel fiber through dissolving, granulation, de-oiling, melt spinning, predraft coiling step.
Background technology
Along with the progress of science and technology and the demand in market, various high performance macromolecular materials have caused people's very big concern, and are one of them important parts to the research of high modulus and strength fiber.
The aromatic polyamide that early seventies occurs has shown the high strength that rigid molecule brought; Succeeding in developing also of late nineteen seventies high-strength high-modulus polyethylene shows; Even typical flexible chain macromolecule; Its degree of orientation and degree of crystallinity be if can improve to heavens, the modulus and the intensity that are equal to iron and steel then can be obtained being enough to.These researchs make to produce and variously prepare the method for high-strength high-modulus fibre from the flexible chain high polymer, if these methods can be divided into methods such as the high pressure solid phase is extruded, plasticising molten spinning crystalline growth method, gel spinning, single-chip stretching by the process technology classification.Because the value in theoretical and the practicality, the gel spinning technology more and more receives people's attention.Can pass through the research of the polymeric system of freezing method formation frozen glue is also progressively strengthening for UHMWPE, UHMWPP, UHMWPAN, UHMWPVA, UHMWPET, UHMWPVC, nylon etc.
Ultra-high molecular weight polyethylene (UHMWPE) fiber is a kind of high-performance fiber with high strength, high-modulus that is formed at the spinning of the polyethylene more than 1,000,000 by average molecular mass.The bulletproof anti-puncturing clothing that superhigh molecular weight polyethylene fibers can be made, rope, parachute, sports equipment, fishing net, fishing, operation sewing thread.It at first is by Paul Smith that gel spinning prepares flexible chain high molecule mass polyethylene fiber technology; Et al at first invents; And obtained BP GB2042414 and GB2051667, and the patent that DSM N. V. at first discloses gel spinning spinning UHMWPE fiber comprises NL7900990, NL7904990 and US4344908 etc., Allied-Signal company is (afterwards with the Honeywell company amalgamation; Claim Honeywell company); Having developed with kerosene or white oil on this basis is solvent, and Freon 113 is the gel spinning technology of extractant, and patent comprises US4413110, US430577, EP0064167, EP0205960 etc.Toyobo company and DSM N. V. reach the industrialization development cooperation agreement, and developing jointly with the decahydronaphthalene is the dry method gel spinning industrialization technology of solvent.Chinese patent 200710177044.1 also disclosed each dry-method spinning technique of a kind of superhigh molecular weight polyethylene fibers system.
As high molecular another the big class of polyolefin; The thermal property of UHMWPP, rheological property, creep-resistant property and processability all are much better than polyethylene, but its crystalline rate is slow than polyethylene, and degree of crystallinity also is lower than polyethylene; And crystallization nucleation need be through " induction period " after a while; The intrinsic helical conformation of molecule can make and form in the process of gel spun fiber in quenching that the mobile variation of molecule segment is difficulty more, is difficult to form favourable crystallite; After processing the polypropylene gel fiber; Can cause gel fiber instability even the fracture of wire that stretches in hot ultra-drawing process, to occur,, propose to prepare the polyolefin mixture as nucleator and fining agent with glucitol derivative like U.S. Pat 5574174 so add nucleator in the preparation process.The frozen glue spinning that one Chinese patent application numbers 200710037871.0 is applied for is equipped with the method for high-strength polypropylene fibre.The fiber of preparation has high mechanical performance, thermal property and low creep rate, and have resistance to chemical attack, higher to good stability, the serviceability temperature of water, can be widely used in the various industries.
Being used for making more high performance carbon fiber, is that the carbon fiber combination property of presoma preparation is best with the polyacrylonitrile fibril, and output accounts for more than 90%.The polyacrylonitrile base carbon fibre integrates high mechanical properties, high-modulus, low-density, high temperature resistant, chemical resistance and good electricity physical and mechanical properties; Its good performance and unique function, Aeronautics and Astronautics, weapons, naval vessels, automobile, machine-building, through spin, fields such as industrial circle such as chemical industry, electronics, communication, medical equipment and physical culture have opened up application prospects.UHMWPAN also can prepare the fiber of high-strength and high-modulus PAN through the gel spinning technology; MIT (European Patent 255109) is to being that certain research has been done in the dissolving of the UHMWPAN of solvent with dimethyl formamide (DMF), thinks to add swelling and the dissolving that 2%～5% water helps UHMWPAN.Chinese patent 200710064246.5 discloses a kind of method for preparing the high-performance polyacrylonitrile-based carbon fiber spinning solution.Chinese patent 03107165.1 also discloses the production method of a kind of high strength, high modulus polypropylene nitrile fiber; The fibre strength that the method is produced is greater than 100cN/tex; And initial modulus is that standard is greater than 15N/tex with 100% percentage elongation; Compare with the fiber of produced in conventional processes, not only intensity is high, initial modulus is big, and pull resistance obviously improves.
The strand of polyvinyl alcohol has plane sawtooth pattern structure, and theoretical modulus is high, thereby has the potentiality of producing high-strength high-modulus fibre.The crystallization modulus of polyvinyl alcohol also is very high with the complete intensity of orientation fibers, reach 250GPa-300GPa and 30GPa respectively, and the fusing point of polyvinyl alcohol is higher about 100 ℃ than polyethylene, polyvinyl alcohol thereby bigger development space is also arranged.Relevant polyvinyl alcohol high-strength high-modulus fibre patent is obtained by the Allied Corporation application of the U.S.; They are with the polyvinyl alcohol of the degree of polymerization 30,000; Carry out gel spinning with polyethylene glycol and glycerine as solvent, obtain the high strength fibre of intensity 11.6cN/dtex-16.9cN/dtex through desolventizing with after stretching.High strength high modulus polyvinyl alcohol fiber is except having the good resistance to acids and bases of conventional vinal, weatherability; Also have characteristics such as intensity height, modulus height; Therefore be the good raw material of industry cloth, building, packing, high-performance hawser; Also be desirable asbestos, the replacement article of glass fibre simultaneously, have extensive use.(JPolym Sci in the document " Gel Spinning of Poly (vinyl Alcohol) from Dimethyl Sulfoxide/water Mixture "; Part B:Polymer Physics; 1994,32 (2), 297-304) a kind of technology that adopts the mixed solvent of the inferior maple/water of dimethyl as the polyvinyl alcohol gel spun spin solvent is disclosed; Prepared as-spun fibre can stretch 45 times, and the TENSILE STRENGTH of fiber is 2.8GPa; It is solvent with ethylene glycol that Chinese patent 93112363.1 discloses a kind of, with the polyvinyl alcohol dissolving, extracts with ethanol, and making fibre strength is that 12g/d, modulus are the vinal of 300g/d.Patent 87103211 also discloses preparation high strength high modulus polyvinyl alcohol fiber method in addition.
Utilizing HMW PET to carry out gel spinning is a kind of important method of producing high-strength and high-modulus PET fiber at present.High-strength and high-modulus PET fiber is compared with other fiber, and special benefits is arranged, and not only low price is of many uses, and its dry heat resistance, damp and hot temperature all higher (about 200 ℃), and its birth will be captured the part market of aramid fiber and high-strength polyethylene.At present; It mainly is to adopt the gel spinning technology that overseas utilization HMW PET produces high-strength high-modulus fibre; Patent JP62030024A, the JP2223333A of Japan TOYOB0 company disclose preparation high-strength and high-modulus PET fiber and have got method, and fibre strength can reach more than the 10d/g.UHMWPVC, nylon etc. can prepare high-strength high-modulus fibre through the frozen glue method in addition; Gel spinning technology to nylon 6; All also be in the exploratory stage at present both at home and abroad; To prepare high performance nylon 6 fibers with gel spinning, at first will prepare super high molecular weight nylon 6, carry out spinning after selecting suitable solvent preparation spinning frozen glue stoste then for use.Matsuo etc. had once studied the deformation mechanism of nylon 6 films that make through gelation/crystallization with the mixed solution of formic acid/chloroform, and to the research of phenmethylol/PA6 frozen glue system.Chinese patent 200710055153.6 discloses the method for preparing nylon powder, and dissolving method also can be used as the method for preparing the high-strength high-modulus fibre spinning solution in this invention.
The letter of present stage polymer gel spinning key step is chatted as follows: ultra-high molecular weight polyethylene is added in the suitable solvent stirring and dissolving process solution; Solution is extruded by screw extruder or process spinning barrel; Through the spinneret orifice extrusion molding; Cool off then, extraction, dry ultra-drawing, finally obtain finished fiber.Produce the super high molecular weight polyethylene gel spinning technique now in the world and mainly contain two big types, one type is spun the dry spinning method into representative, the another kind of wet spinning process of representing with Honeywell with DSM and Japan.Both main distinctions are to have adopted different solvents and subsequent technique.Extracting process is with volatilizable extractant first solvent exchange to be come out in the wet spinning technology, in one technology in back, adopts heat treatment and drawing process to get rid of the volatility extractant.Solvent generally adopts higher boiling white oil, paraffin oil, kerosene etc., and extractant then adopts low boilers, like xylene, gasoline, acetone, trichorotrifluoroethane etc.Dry spinning then be utilize heat energy etc. in spinning process with solvent evaporates, process fiber through super drawing again, utilize again after solvent then reclaims.
Polypropylene frozen glue spinning process flow process is that ultra-high molecular weight isotactic polypropylene, solvent and nucleator are dissolved through swelling; Be mixed with polypropylene solution; Spinning solution is through metering, filament spinning component, and quenching in coagulating bath forms the polypropylene gel fiber; Gel fiber forms the polypropylene fibre finished product through extraction, dry, multistage stretching after the HEAT SETTING.The preparation were established of high-strength and high-modulus PAN fiber is that UHMWPAN homopolymers powder is dissolved in the certain amount of organic solvent; Leave standstill at 30-50 ℃ then; Deaeration, obtaining solid content is the 5-25wt% spinning solution, puts into the spinning barrel then; Obtain gel fiber through spinnerets, coagulating bath, gel fiber obtains high-strength and high-modulus PAN fiber through extraction, drying, multistage stretching.The gel spinning technology of polymer such as UHMWPVA, UHMWPET, UHMWPVC, nylon is similar with the gel spinning process route of UHMWPAN; Just solvent, auxiliary agent, coagulating agent, extractant are distinguished to some extent; But from above technology, can find out, when polymer is configured to spinning solution and prepares gel fiber, though solid content has nothing in common with each other; But prepared gel fiber also can consume a large amount of extractants all not containing a large amount of solvents before the extraction in follow-up extraction process.It is thus clear that because non-volatile solvents content is high in the gel fiber, polymer solids level is low, makes spinning efficiency low; In extraction process; Also make volatilizable extractant agent consumption big, cause extracting the cost height, equipment investment is big; The cost recovery cycle is long, and a large amount of uses of solvent simultaneously can bring potential safety hazard and problem of environmental pollution.
Chinese patent 200610118733.0 also discloses new extraction process; Be with the preliminary treatment of gel fiber through the hydrocarbon extractant; Extraction more continuously; Solvent/extractant mixture by producing in bath and the ultrasonic extraction groove is quantitatively transferred to the fractionation retracting device by delivery pump, and the extractant that fractionation is reclaimed can be directly be delivered to respectively in extraction bath and the ultrasonic extraction groove with pump, and solvent is delivered to preceding road dissolution process through filtering, taking off after mixing.But this technology does not reduce the content of preceding first solvent of gel fiber extraction yet, in extraction process, does not reduce the consumption of extractant, so do not have too many reducing cost and enhancing productivity yet.Chinese patent 200810034216.4 also disclosed in producing UHMWPE fiber process with Chinese patent 200810034215.X, improve solid content through improving the obtain solution method, but the solid content of its raising did not yet reach desirable production demand.
Can know by above narration; The defective of prior art comprises: the polymer powders concentration of (1) dissolving or swelling is too low; As in the UHMWPE wet spinning technology,, be configured to 5%-25% solution with DMSO in the UHMWPAN gel spinning technology, be configured to 25%-30% solution with DMF in the UHMWPVA gel spinning technology with solvent preparation 8%-10% solution; Owing to contain a large amount of solvents, production efficiency is just too low; (2) existence of solvent certainly will produce environmental pollution; Though especially can be mixed with 20%-30% solution with decahydronaphthalene in the UHMWPE dry process; But decahydronaphthalene is as solvent; Toxicity is bigger, and used DMF, DMSO etc. can both contaminated environment in spinning for the frozen glue of other polymer in addition, endanger healthy; (3) must introduce extractant in the extraction process, solid content is low, when solvent is high, will improve the use amount of extractant, and the mixture of solvent and extractant also must separate, filter, reclaim in process of production, causes the production cost rising.
Summary of the invention
In order to solve the defective that above prior art exists; The invention provides a kind of preparation method of gel fiber; A kind of method that improves spinning solution prepared at concentrations gel fiber that adopts just is provided, specifically a kind of preparation method of the gel fiber through dissolving, granulation, de-oiling, melt spinning, predraft coiling step.
The preparation method of a kind of gel fiber of the present invention; With polymer powders and solvent and heated and stirred, after dissolving fully, polymer powders processes the melt strip, granulation after cooling is the frozen glue shape; Then institute's granulation is sloughed partial solvent; Again the polymer gel particle behind desolventizing is carried out melt spinning, predraft is reeled after coagulating bath, makes the polymer gel silk of high solids content.
As optimized technical scheme:
The preparation method of aforesaid a kind of gel fiber; Wherein, described polymer is that molecular weight is that 1,500,000～8,000,000 UHMWPE, molecular weight are that 400,000～2,000,000 UHMWPP, molecular weight are that 100,000～300,000 UHMWPAN, molecular weight are that 100,000～200,000 UHMWPVA, molecular weight are that 50,000～200,000 UHMWPET, molecular weight are that 100,000～250,000 UHMWPVC or molecular weight are 50,000～100,000 nylon.
The preparation method of aforesaid a kind of gel fiber, wherein, described polymer powders average grain diameter is 10 μ m～200 μ m; The mixed proportion of described polymer powders and solvent is respectively:
UHMWPE or UHMWPP polymer powders and solvent are 4～10: 100 by mass ratio; The dissolving of these two kinds of polymer also comprises adding antioxidant; The addition of antioxidant is 2%～5% of a solute quality; The dissolving of UHMWPP polymer also comprises the adding nucleator, and the addition of nucleator is 5～30% of a solute quality;
UHMWPAN polymer powders and solvent are 5～25: 100 by mass ratio;
UHMWPVA polymer powders and solvent are 10～30: 100 by mass ratio;
UHMWPET polymer powders and solvent are 6～25: 100 by mass ratio;
UHMWPVC polymer powders and solvent are 10～25: 100 by mass ratio;
Nylon polymer powder and solvent are 10～25: 100 by mass ratio.
The preparation method of aforesaid a kind of gel fiber, wherein, described solvent is respectively:
Solvent for use was mineral oil, white oil, paraffin oil or kerosene when polymer was UHMWPE or UHMWPP;
Solvent for use was DMF, DMSO, DMAc or the 50%NaSCN aqueous solution when polymer was UHMWPAN;
Solvent for use was DMF, DMSO, organic hydroxy compounds, glycerine or N-Methyl pyrrolidone when polymer was UHMWPVA;
Solvent for use was trifluoroacetic acid, nitrobenzene, hexafluoroisopropanol, chloroform or chlorophenol when polymer was UHMWPET;
Solvent for use was oxolane, cyclohexanone or chloroform when polymer was UHMWPVC;
Solvent for use was nitromethane or nitroethane when polymer was nylon.
The preparation method of aforesaid a kind of gel fiber wherein, is characterized in that, described antioxidant is antioxidant 300, antioxidant 330, antioxidant 168, antioxidant 1076, antioxidant 1010, anti-oxidant DLTP or antioxidant DSTP;
Described nucleator is 1,3-2,4-two (benzal)-D-D-sorbite, 1; 3-2,4-two Asias (4-methyl) benzyl-D-D-sorbite, 1,3-2; 4-(3, the 4-dimethyl benzylidene)-D-D-sorbite, 1,3-2; 4-two (4-ethyl benzal)-D-D-sorbite, tricarballylic acid type amide compound, 1,3, one or more combination in the middle of 5-benzenetricarboxylic acid derivative, Sodium Benzoate, two (4-(tert-butyl group) benzoic acid) hydroxy Al.
The preparation method of aforesaid a kind of gel fiber, the described melt strip of processing is to adopt the method that makes through behind screw rod fusion or the spinning barrel; Wherein,
The temperature of UHMWPE or the described heated and stirred of UHMWPP polymer powders is 50 ℃～190 ℃; The screw rod melt temperature is 90 ℃～190 ℃ when processing the melt strip;
The temperature of the described heated and stirred of UHMWPAN polymer powders is 50 ℃～90 ℃; The spinning barrel temperature is 80 ℃～100 ℃ when processing the melt strip;
The temperature of the described heated and stirred of UHMWPVA polymer powders is 70 ℃～90 ℃; The spinning barrel temperature is 65 ℃～85 ℃ when processing the melt strip;
The temperature of the described heated and stirred of UHMWPET polymer powders is 170 ℃～210 ℃; The screw rod fusion is 210 ℃～270 ℃ when processing the melt strip;
The temperature of the UHMWPV ℃ of described heated and stirred of polymer powders is 50 ℃～60 ℃; The spinning barrel temperature is 50 ℃～80 ℃ when processing the melt strip;
The temperature of the described heated and stirred of nylon polymer powder is 100 ℃～150 ℃; The spinning barrel temperature is 160 ℃～240 ℃ when processing the melt strip.
The preparation method of aforesaid a kind of gel fiber, wherein, described cooling is meant and is cooled to 10 ℃～30 ℃ that cooling method is the nature cooling; The granulation of mechanical pelletizing method is adopted in described granulation, and gained pellet average grain diameter is of a size of 0.1mm～30mm.
The preparation method of aforesaid a kind of gel fiber; Wherein, The described partial solvent of sloughing is meant that obtaining solid content is that the polymer spinning raw material of 20wt%～80wt% is the polymer gel particle; Be to adopt the centrifugal physics de-oiling of high-speed rotating machine equipment, rotating speed is 500～9000 rev/mins, and the de-oiling time is 30-200min.
The preparation method of aforesaid a kind of gel fiber, wherein, described melt spinning adopts the screw rod extruding spinning, wherein,
The described screw rod spinning temperature of UHMWPE or UHMWPP polymer powders is 140 ℃～265 ℃;
The described screw rod spinning temperature of UHMWPAN polymer powders is 50 ℃～90 ℃;
The described screw rod spinning temperature of UHMWPVA polymer powders is 50 ℃～80 ℃;
The described screw rod spinning temperature of UHMWPET polymer powders is 200 ℃～280 ℃;
The described screw rod spinning temperature of UHMWPVC polymer powders is 70 ℃～90 ℃;
The described screw rod spinning temperature of nylon polymer powder is 150 ℃～250 ℃;
The coagulating agent that described coagulating bath is selected for use is:
The used coagulating agent of UHMWPE or UHMWPP is a water, and the temperature of coagulating bath is-10 ℃～10 ℃;
The used coagulating agent of UHMWPAN is the solution that water or solvent and water are made into, and described solvent and water volume ratio are 1～9: 3; The temperature range of coagulating bath is 20～110 ℃;
The used coagulating agent of UHMWPVA is methyl alcohol, ethanol, propyl alcohol, butanols, acetone or decahydronaphthalenes, and the temperature of coagulating bath is-10 ℃～0 ℃;
The used coagulating agent of UHMWPET is methyl alcohol, ethanol, propyl alcohol, acetone, and the temperature of coagulating bath is 10 ℃～50 ℃;
The used coagulating agent of UHMWPVC is a water, 0 ℃～20 ℃ of the temperature of coagulating bath;
The used coagulating agent of nylon is a water, the temperature of coagulating bath-10 ℃～20 ℃.
The preparation method of aforesaid a kind of gel fiber, wherein, described predraft multiple is 1.5～20, the solid content of the polymer gel silk of described high solids content is 20%～80%.
The preparation method's of a kind of gel fiber of the present invention basic principle be polymer in solvent swelling or the dissolving after, on screw rod, melt extrude strip, again through pelletizing; Utilize the centrifugal action of high speed machine rotation then; The solvent that pellet is surperficial and inner is separated, and these polymer beads are under the temperature of dissolving just, because big molecular entanglement is opened in course of dissolution; Flowability is greatly improved during melt spinning once more, therefore can increase substantially polymer solids level in the melt.
The invention has the beneficial effects as follows:
1, increases substantially the solid content of the polymer of prior art gel fiber, thereby improve the production efficiency and the single machine yield of existing equipment;
2, reduce the solvent of unit production capacity and using and consuming of extractant, reduce discharging, help environmental protection and energy-conservation, reduce production costs.
The specific embodiment
Below in conjunction with the specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1:
UHMWPE powder: molecular weight 1,500,000, average grain diameter 10 μ m; Solvent: kerosene; Antioxidant 300 (polyethylene powder, solvent and antioxidant are 10: 100: 0.3 by mass percentage); Polymer powders, solvent and antioxidant are mixed in dissolution kettle and heated and stirred, and temperature is 50 ℃ in the beginning still, after be raised to 170 ℃ gradually, get into screw rod after stirring swelling in the dissolution kettle; The screw rod solution temperature, feed zone: 90 ℃, the preheating zone: 115 ℃, dissolve area: 175 ℃, the compressional zone: 180 ℃, metering zone: 190 ℃; , screw rod is cooled to 10 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 30mm; Mechanical centrifuge rotating speed: 500 rev/mins; The de-oiling time: 60 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 140 ℃, the preheating zone: 165 ℃, melting zone: 180 ℃, the compressional zone: 185 ℃, metering zone: 210 ℃; Spinning manifold: 220 ℃, measuring pump: 12 rev/mins, the shower nozzle extruded velocity: 2.8 meters/minute, winding speed: 13 meters/minute, coagulating bath is-10 ℃ a frozen water, and the predraft multiple is 1.5.Record that to freeze the hank knotting solid content be 30.2wt%.
Embodiment 2:
UHMWPE powder: molecular weight 2,500,000, average grain diameter 200 μ m; Solvent: mineral oil; Antioxidant 330 (polyethylene powder, solvent and antioxidant are 10: 100: 0.2 by mass percentage); Polymer powders, solvent and antioxidant are mixed in dissolution kettle and heated and stirred, and temperature is 50 ℃ in the beginning still, after be raised to 180 ℃ gradually, stir swelling in the dissolution kettle and get into screw rod; The screw rod solution temperature, feed zone: 90 ℃, the preheating zone: 115 ℃, dissolve area: 175 ℃, the compressional zone: 180 ℃, metering zone: 185 ℃; , screw rod is cooled to 30 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 20mm; Mechanical centrifuge rotating speed: 3000 rev/mins; The de-oiling time: 30 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 140 ℃, the preheating zone: 155 ℃, melting zone: 180 ℃, the compressional zone: 185 ℃, metering zone: 180 ℃; Spinning manifold: 225 ℃, measuring pump: 12 rev/mins, the shower nozzle extruded velocity: 2.9 meters/minute, winding speed: 14 meters/minute, coagulating bath is-10 ℃ a frozen water, and the predraft multiple is 20.Record that to freeze the hank knotting solid content be 29.3wt%.
Embodiment 3:
UHMWPE powder: molecular weight 4,500,000, average grain diameter 100 μ m; Solvent: white oil; Antioxidant 1010 (polyethylene powder, solvent and antioxidant are 8: 100: 0.16 by mass percentage); Polymer powders, solvent and antioxidant are mixed in dissolution kettle and heated and stirred, and temperature is 50 ℃ in the beginning still, after be raised to 180 ℃ gradually, stir swelling in the dissolution kettle and get into screw rod; The screw rod solution temperature, feed zone: 90 ℃, the preheating zone: 115 ℃, dissolve area: 175 ℃, the compressional zone: 180 ℃, metering zone: 185 ℃; , screw rod is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 18mm; Mechanical centrifuge rotating speed: 3500 rev/mins; The de-oiling time: 80 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 155 ℃, the preheating zone: 175 ℃, melting zone: 200 ℃, the compressional zone: 210 ℃, metering zone: 220 ℃; Spinning manifold: 225 ℃, measuring pump: 12 rev/mins, the shower nozzle extruded velocity: 3.0 meters/minute, winding speed: 15 meters/minute, coagulating bath is 10 ℃ a water, and the predraft multiple is 1.5.。Record that to freeze the hank knotting solid content be 34.6wt%.
Embodiment 4:
UHMWPE powder: molecular weight 5,500,000, average grain diameter 100 μ m; Solvent: paraffin oil; Antioxidant 1076 (polyethylene powder, solvent and antioxidant are 8: 100: 0.16 by mass percentage); Polymer powders, solvent and antioxidant are mixed in dissolution kettle and heated and stirred, and temperature is 60 ℃ in the beginning still, after be raised to 180 ℃ gradually, stir swelling in the dissolution kettle and get into screw rod; The screw rod solution temperature, feed zone: 90 ℃, the preheating zone: 115 ℃, dissolve area: 175 ℃, the compressional zone: 180 ℃, metering zone: 185 ℃; , screw rod is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 16mm; Mechanical centrifuge rotating speed: 4000 rev/mins; The de-oiling time: 90 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 155 ℃, the preheating zone: 180 ℃, melting zone: 210 ℃, the compressional zone: 235 ℃, metering zone: 240 ℃; Spinning manifold: 235 ℃, measuring pump: 13 rev/mins, the shower nozzle extruded velocity: 2.8 meters/minute, winding speed: 13 meters/minute, coagulating bath is 0 ℃ a frozen water, and the predraft multiple is 4.Record that to freeze the hank knotting solid content be 40.1wt%.
Embodiment 5:
UHMWPE powder: molecular weight 6,500,000, average grain diameter 100 μ m; Solvent: white oil; Anti-oxidant DLTP (polyethylene powder, solvent and antioxidant are 7: 100: 0.35 by mass percentage); Polymer powders, solvent and antioxidant are mixed in dissolution kettle and heated and stirred, and temperature is 60 ℃ in the beginning still, after be raised to 190 ℃ gradually, stir swelling in the dissolution kettle and get into screw rod; The screw rod solution temperature, feed zone: 90 ℃, the preheating zone: 115 ℃, dissolve area: 175 ℃, the compressional zone: 180 ℃, metering zone: 185 ℃; , screw rod is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 13mm; Mechanical centrifuge rotating speed: 5000 rev/mins; The de-oiling time: 110 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 145 ℃, the preheating zone: 165 ℃, melting zone: 190 ℃, the compressional zone: 200 ℃, metering zone: 230 ℃; Spinning manifold: 255 ℃, measuring pump: 14 rev/mins, the shower nozzle extruded velocity: 3.1 meters/minute, winding speed: 15.5 meters/minute, coagulating bath is 0 ℃ a frozen water, and the predraft multiple is 4.Record that to freeze the hank knotting solid content be 45.6wt%.
Embodiment 6:
UHMWPE powder: molecular weight 8,000,000, average grain diameter 100 μ m; Solvent: white oil; Antioxidant 1010 (polyethylene powder, solvent and antioxidant are 4: 100: 0.08 by mass percentage); Polymer powders, solvent and antioxidant are mixed in dissolution kettle and heated and stirred, and temperature is 50 ℃ in the beginning still, after be raised to 190 ℃ gradually, stir swelling in the dissolution kettle and get into screw rod; The screw rod solution temperature, feed zone: 90 ℃, the preheating zone: 115 ℃, dissolve area: 175 ℃, the compressional zone: 180 ℃, metering zone: 185 ℃; , screw rod is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 4000 rev/mins; The de-oiling time: 100 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 160 ℃, the preheating zone: 180 ℃, melting zone: 190 ℃, the compressional zone: 215 ℃, metering zone: 240 ℃; Spinning manifold: 265 ℃, measuring pump: 12 rev/mins, the shower nozzle extruded velocity: 2.5 meters/minute, winding speed: 12 meters/minute, coagulating bath is 0 ℃ a frozen water, and the predraft multiple is 4.Record that to freeze the hank knotting solid content be 40.6wt%.
Embodiment 7:
UHMWPE powder: molecular weight 4,500,000, average grain diameter 100 μ m; Solvent: white oil; Antioxidant DSTP (polyethylene powder, solvent and antioxidant are 8: 100: 0.16 by mass percentage); Polymer powders, solvent and antioxidant are mixed in dissolution kettle and heated and stirred, and temperature is 50 ℃ in the beginning still, after be raised to 185 ℃ gradually, stir swelling in the dissolution kettle and get into screw rod; The screw rod solution temperature, feed zone: 90 ℃, the preheating zone: 115 ℃, dissolve area: 175 ℃, the compressional zone: 180 ℃, metering zone: 185 ℃; , screw rod is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 5mm; Mechanical centrifuge rotating speed: 6000 rev/mins; The de-oiling time: 150 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 130 ℃, the preheating zone: 145 ℃, melting zone: 190 ℃, the compressional zone: 205 ℃, metering zone: 210 ℃; Spinning manifold: 230 ℃, measuring pump: 12 rev/mins, the shower nozzle extruded velocity: 2.8 meters/minute, winding speed: 13 meters/minute, coagulating bath is 0 ℃ a frozen water, and the predraft multiple is 4.Record that to freeze the hank knotting solid content be 60.2wt%.
Embodiment 8:
UHMWPE powder: molecular weight 4,500,000, average grain diameter 100 μ m; Solvent: white oil; Antioxidant 168 (polyethylene powder, solvent and antioxidant are 9: 100: 0.18 by mass percentage); Polymer powders, solvent and antioxidant are mixed in dissolution kettle and heated and stirred, and temperature is 50 ℃ in the beginning still, after be raised to 180 ℃ gradually, stir swelling in the dissolution kettle and get into screw rod; The screw rod solution temperature, feed zone: 90 ℃, the preheating zone: 115 ℃, dissolve area: 175 ℃, the compressional zone: 180 ℃, metering zone: 185 ℃; , screw rod is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 0.1mm; Mechanical centrifuge rotating speed: 9000 rev/mins; The de-oiling time: 200 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 135 ℃, the preheating zone: 145 ℃, melting zone: 180 ℃, the compressional zone: 195 ℃, metering zone: 225 ℃; Spinning manifold: 235 ℃, measuring pump: 12 rev/mins, the shower nozzle extruded velocity: 2.8 meters/minute, winding speed: 13 meters/minute, coagulating bath is 0 ℃ a frozen water, and the predraft multiple is 4.Recording the gel fiber solid content is 68.3wt%.
Comparative Examples 1:
UHMWPE powder: molecular weight 4,500,000; Solvent: white oil; Antioxidant 1010 (polyethylene powder, solvent and antioxidant are 8: 100: 0.16 by mass percentage); Polymer powders, solvent and antioxidant are mixed and heated and stirred the swelling solution temperature in dissolution kettle: 170 ℃, mix and stir swelling entering screw rod.The screw rod solution temperature, feed zone: 90 ℃, the preheating zone: 115 ℃, dissolve area: 175 ℃, the compressional zone: 180 ℃, metering zone: 185 ℃; The gel fiber solid content that records gained is 12.4%.
Comparative Examples 2:
UHMWPE powder: molecular weight 5,000,000; Solvent: white oil; Antioxidant 1076 (polyethylene powder, solvent and antioxidant are 8: 100: 0.16 by mass percentage); Polymer powders, solvent and antioxidant are mixed and heated and stirred the swelling solution temperature in dissolution kettle: 180 ℃, mix and stir swelling entering screw rod.The screw rod solution temperature, feed zone: 90 ℃, the preheating zone: 115 ℃, dissolve area: 175 ℃, the compressional zone: 180 ℃, metering zone: 185 ℃; The gel fiber solid content that records gained is 11.3%.
Embodiment 9:
UHMWPP powder: molecular weight 400,000; Solvent: kerosene; Antioxidant 1010 (polyethylene powder, solvent and antioxidant are 4: 100: 0.12 by mass percentage); Nucleator is 1,3-2, and 4-two (benzal)-D-D-sorbite, the addition of nucleator is 5% of a solute quality; Polymer powders, solvent, antioxidant and nucleator are mixed in dissolution kettle and heated and stirred, and temperature is 50 ℃ in the beginning still, after be raised to 185 ℃ gradually, mix and stir swelling and get into screw rod.The screw rod solution temperature, feed zone: 90 ℃, the preheating zone: 115 ℃, dissolve area: 175 ℃, the compressional zone: 180 ℃, metering zone: 185 ℃; , screw rod is cooled to 10 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 4000 rev/mins; The desolventizing time: 200 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 115 ℃, the preheating zone: 150 ℃, melting zone: 180 ℃, the compressional zone: 185 ℃, metering zone: 220 ℃; Spinning manifold: 260 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating bath is 10 ℃ of water, and the predraft multiple is 1.5.The gel fiber solid content that records gained is 39.1%.
Embodiment 10:
UHMWPP powder: molecular weight 2,000,000; Solvent: mineral oil; Antioxidant 300 (polyethylene powder, solvent and antioxidant are 8: 100: 0.16 by mass percentage); Nucleator is 1,3-2, and 4-two Asias (4-methyl) benzyl-D-D-sorbite, the addition of nucleator is 30% of a solute quality; Polymer powders, solvent, antioxidant and nucleator are mixed in dissolution kettle and heated and stirred, and temperature is 80 ℃ in the beginning still, after be raised to 190 ℃ gradually, mix and stir swelling and get into screw rod.The screw rod solution temperature, feed zone: 90 ℃, the preheating zone: 115 ℃, dissolve area: 175 ℃, the compressional zone: 180 ℃, metering zone: 190 ℃; , screw rod is cooled to 30 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 20mm; Mechanical centrifuge rotating speed: 2500 rev/mins; The desolventizing time: 30 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 115 ℃, the preheating zone: 150 ℃, melting zone: 180 ℃, the compressional zone: 185 ℃, metering zone: 180 ℃; Spinning manifold: 230 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating bath is-10 ℃ of frozen water, and the predraft multiple is 20.The gel fiber solid content that records gained is 33.2%.
Embodiment 11:
UHMWPP powder: molecular weight 1,000,000; Solvent: paraffin oil; Antioxidant 330 (polyethylene powder, solvent and antioxidant are 10: 100: 0.5 by mass percentage), nucleator is 1,3-2,4-(3, the 4-dimethyl benzylidene)-D-D-sorbite, the addition of nucleator is 20% of a solute quality; Polymer powders, solvent, antioxidant and nucleator are mixed in dissolution kettle and heated and stirred, and temperature is 50 ℃ in the beginning still, after be raised to 185 ℃ gradually, mix and stir swelling and get into screw rod.The screw rod solution temperature, feed zone: 90 ℃, the preheating zone: 115 ℃, dissolve area: 175 ℃, the compressional zone: 180 ℃, metering zone: 185 ℃; , screw rod is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 10mm; Mechanical centrifuge rotating speed: 3500 rev/mins; The desolventizing time: 80 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 115 ℃, the preheating zone: 150 ℃, melting zone: 180 ℃, the compressional zone: 185 ℃, metering zone: 180 ℃; Spinning manifold: 230 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating bath is 0 ℃ of frozen water, and the predraft multiple is 4.The gel fiber solid content that records gained is 36.8%.
Embodiment 12～15
UHMWPP powder: molecular weight 1,000,000; Solvent: white oil; (polyethylene powder, solvent are 8: 100 by mass percentage), except that antioxidant, nucleator (addition of antioxidant is 2% of a solute quality, the addition of nucleator be the solute quality 20%), other experiment condition is with embodiment 11:
Comparative Examples 3:
UHMWPP powder: molecular weight 1,000,000; Solvent: white oil; Antioxidant 1010 (polyethylene powder, solvent and antioxidant are 8: 100: 0.16 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 180 ℃, mix and stir swelling entering screw rod.The screw rod solution temperature, feed zone: 115 ℃, the preheating zone: 150 ℃, dissolve area: 175 ℃, the compressional zone: 180 ℃, metering zone: 185 ℃; Obtain the UHMWPP gel fiber after extruding, the gel fiber solid content that records gained is 10.3%.
Embodiment 16:
UHMWPAN powder: molecular weight 100,000; Solvent: DMF (UHMWPAN powder, solvent are 5: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 50 ℃, mix and stirred 180 minutes.The spinning barrel temperature, 80 ℃; After the spinning barrel is extruded into the melt strip, be cooled to 10 ℃ naturally, mechanical pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3500 rev/mins; The desolventizing time: 40 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 50 ℃, the preheating zone: 60 ℃, melting zone: 60 ℃, the compressional zone: 65 ℃, metering zone: 80 ℃; Spinning manifold: 90 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is a water, and temperature is 20 ℃, and the predraft multiple is 1.5.The gel fiber solid content that records gained is 50.1%.
Embodiment 17:
UHMWPAN powder: molecular weight 300,000; Solvent: DMSO (UHMWPAN powder, solvent are 25: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 90 ℃, mix and stirred 180 minutes.The spinning barrel temperature, 100 ℃; , the spinning barrel is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3600 rev/mins; The desolventizing time: 40 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 55 ℃, the preheating zone: 60 ℃, melting zone: 60 ℃, the compressional zone: 65 ℃, metering zone: 80 ℃; Spinning manifold: 85 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is the solution (1: 3) that solvent and water are made into, and temperature is 20 ℃, and the predraft multiple is 20.The gel fiber solid content that records gained is 51.2%.
Embodiment 18:
UHMWPAN powder: molecular weight 300,000; Solvent: DMAc (UHMWPAN powder, solvent are 20: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 90 ℃, mix and stirred 180 minutes.The spinning barrel temperature, 100 ℃; , the spinning barrel is cooled to 30 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3600 rev/mins; The desolventizing time: 40 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 55 ℃, the preheating zone: 60 ℃, melting zone: 60 ℃, the compressional zone: 65 ℃, metering zone: 80 ℃; Spinning manifold: 85 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is the solution (9: 3) that solvent and water are made into, and temperature is 20 ℃, and the predraft multiple is 2.The gel fiber solid content that records gained is 51.5%.
Embodiment 19:
UHMWPAN powder: molecular weight 300,000; Solvent: the 50%NaSCN aqueous solution (UHMWPAN powder, solvent are 20: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 90 ℃, mix and stirred 180 minutes.The spinning barrel temperature, 100 ℃; , the spinning barrel is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3600 rev/mins; The desolventizing time: 40 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 55 ℃, the preheating zone: 60 ℃, melting zone: 60 ℃, the compressional zone: 65 ℃, metering zone: 80 ℃; Spinning manifold: 85 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is the solution (5: 3) that solvent and water are made into, and temperature is 60 ℃, and the predraft multiple is 3.The gel fiber solid content that records gained is 51.6%.
Comparative Examples 4:
UHMWPAN powder: molecular weight 500,000; Solvent: DMF; Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 70 ℃, mix and stirred 180 minutes.The spinning barrel temperature, 80 ℃; The shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; The gel fiber solid content that records gained is 25.4%.
Embodiment 20
UHMWPVA powder: molecular weight 100,000 (degree of polymerization about 2300); Solvent: DMF (UHMWPVA powder, solvent are 10: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 70 ℃, mix and stirred 180 minutes.The spinning barrel temperature, 65 ℃; , the spinning barrel is cooled to 10 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3500 rev/mins; The desolventizing time: 30 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 50 ℃, the preheating zone: 60 ℃, melting zone: 60 ℃, the compressional zone: 65 ℃, metering zone: 70 ℃; Spinning manifold: 75 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is a methyl alcohol, and temperature is-10 ℃, and the predraft multiple is 1.5.The gel fiber solid content that records gained is 45.1%.
Embodiment 21
UHMWPVA powder: molecular weight 200,000 (degree of polymerization about 4600); Solvent: DMSO (UHMWPVA powder, solvent are 30: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 90 ℃, mix and stirred 180 minutes.The spinning barrel temperature, 85 ℃; , the spinning barrel is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3600 rev/mins; The desolventizing time: 200 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 55 ℃, the preheating zone: 60 ℃, melting zone: 60 ℃, the compressional zone: 65 ℃, metering zone: 70 ℃; Spinning manifold: 80 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is an ethanol, and temperature is 0 ℃, and the predraft multiple is 20.The gel fiber solid content that records gained is 46.3%.
Embodiment 22
UHMWPVA powder: molecular weight 200,000 (degree of polymerization about 4600); Solvent: organic hydroxy compounds (UHMWPVA powder, solvent are 20: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 90 ℃, mix and stirred 180 minutes.The spinning barrel temperature, 85 ℃; , the spinning barrel is cooled to 30 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3600 rev/mins; The desolventizing time: 40 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 55 ℃, the preheating zone: 60 ℃, melting zone: 60 ℃, the compressional zone: 65 ℃, metering zone: 70 ℃; Spinning manifold: 80 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is butanols or propyl alcohol, and temperature is 0 ℃, and the predraft multiple is 3.The gel fiber solid content that records gained is 46.5%.
Embodiment 23
UHMWPVA powder: molecular weight 200,000 (degree of polymerization about 4600); Solvent: glycerine (UHMWPVA powder, solvent are 20: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 90 ℃, mix and stirred 180 minutes.The spinning barrel temperature, 85 ℃; , the spinning barrel is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3600 rev/mins; The desolventizing time: 60 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 55 ℃, the preheating zone: 60 ℃, melting zone: 60 ℃, the compressional zone: 65 ℃, metering zone: 70 ℃; Spinning manifold: 80 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is an acetone, and temperature is 0 ℃, and the predraft multiple is 3.The gel fiber solid content that records gained is 46.7%.
Embodiment 24
UHMWPVA powder: molecular weight 200,000 (degree of polymerization about 4600); Solvent: N-Methyl pyrrolidone (UHMWPVA powder, solvent are 20: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 90 ℃, mix and stirred 180 minutes.The spinning barrel temperature, 85 ℃; , the spinning barrel is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3600 rev/mins; The desolventizing time: 40 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 55 ℃, the preheating zone: 60 ℃, melting zone: 60 ℃, the compressional zone: 65 ℃, metering zone: 70 ℃; Spinning manifold: 80 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is a decahydronaphthalenes, and temperature is 0 ℃, and the predraft multiple is 3.The gel fiber solid content that records gained is 45.7%.
Comparative Examples 5:
UHMWPVA powder: molecular weight 100,000 (degree of polymerization about 2300); Solvent: DMSO; Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 70 ℃, mix and stirred 180 minutes.The spinning barrel temperature, 80 ℃; The shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; The gel fiber solid content that records gained is 21.6%.
Embodiment 25:
UHMWPET powder: molecular weight 50,000; Solvent: nitrobenzene (UHMWPET powder, solvent are 6: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, swelling temperature in dissolution kettle: 170 ℃, mix and stirred 50 minutes.The screw rod solution temperature, feed zone: 210 ℃, the preheating zone: 235 ℃, dissolve area: 245 ℃, the compressional zone: 260 ℃, metering zone: 270 ℃; , screw rod is cooled to 10 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3500 rev/mins; The desolventizing time: 30 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 200 ℃, the preheating zone: 250 ℃, melting zone: 260 ℃, the compressional zone: 260 ℃, metering zone: 265 ℃; Spinning manifold: 280 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is a methyl alcohol, and temperature is 10 ℃, and the predraft multiple is 1.5.The gel fiber solid content that records gained is 36.1%.
Embodiment 26:
UHMWPET powder: molecular weight 200,000; Solvent: trifluoroacetic acid (UHMWPET powder, solvent are 25: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, swelling temperature in dissolution kettle: 210 ℃, mix and stirred 60 minutes.The screw rod solution temperature, feed zone: 220 ℃, the preheating zone: 235 ℃, dissolve area: 245 ℃, the compressional zone: 260 ℃, metering zone: 260 ℃; , screw rod is cooled to 30 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3600 rev/mins; The desolventizing time: 200 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 245 ℃, the preheating zone: 250 ℃, melting zone: 260 ℃, the compressional zone: 260 ℃, metering zone: 265 ℃; Spinning manifold: 265 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is an ethanol, and temperature is 50 ℃, and the predraft multiple is 3.The gel fiber solid content that records gained is 38.7%.
Embodiment 27:
UHMWPET powder: molecular weight 200,000; Solvent: hexafluoroisopropanol (UHMWPET powder, solvent are 25: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, swelling temperature in dissolution kettle: 210 ℃, mix and stirred 60 minutes.The screw rod solution temperature, feed zone: 220 ℃, the preheating zone: 235 ℃, dissolve area: 245 ℃, the compressional zone: 260 ℃, metering zone: 260 ℃; , screw rod is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3600 rev/mins; The desolventizing time: 60 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 245 ℃, the preheating zone: 250 ℃, melting zone: 260 ℃, the compressional zone: 260 ℃, metering zone: 265 ℃; Spinning manifold: 265 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is a propyl alcohol, and temperature is 30 ℃, and the predraft multiple is 20.The gel fiber solid content that records gained is 36.7%.
Embodiment 28:
UHMWPET powder: molecular weight 200,000; Solvent: chloroform (UHMWPET powder, solvent are 20: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, swelling temperature in dissolution kettle: 210 ℃, mix and stirred 60 minutes.The screw rod solution temperature, feed zone: 220 ℃, the preheating zone: 235 ℃, dissolve area: 245 ℃, the compressional zone: 260 ℃, metering zone: 260 ℃; , screw rod is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3600 rev/mins; The desolventizing time: 60 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 245 ℃, the preheating zone: 250 ℃, melting zone: 260 ℃, the compressional zone: 260 ℃, metering zone: 265 ℃; Spinning manifold: 265 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is an acetone, and temperature is 20 ℃, and the predraft multiple is 2.The gel fiber solid content that records gained is 36.7%.
Embodiment 29:
UHMWPET powder: molecular weight 200,000; Solvent: chlorophenol (UHMWPET powder, solvent are 20: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, swelling temperature in dissolution kettle: 210 ℃, mix and stirred 60 minutes.The screw rod solution temperature, feed zone: 220 ℃, the preheating zone: 235 ℃, dissolve area: 245 ℃, the compressional zone: 260 ℃, metering zone: 260 ℃; , screw rod is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3600 rev/mins; The desolventizing time: 60 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 245 ℃, the preheating zone: 250 ℃, melting zone: 260 ℃, the compressional zone: 260 ℃, metering zone: 265 ℃; Spinning manifold: 265 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is an acetone, and temperature is 30 ℃, and the predraft multiple is 2.The gel fiber solid content that records gained is 36.7%.
Comparative Examples 6:
UHMWPET powder: molecular weight 150,000; Solvent: nitrobenzene; Polymer powders and solvent are mixed also heated and stirred, swelling temperature in dissolution kettle: 195 ℃, mix and stirred 50 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod solution temperature, feed zone: 240 ℃, the preheating zone: 250 ℃, dissolve area: 260 ℃, the compressional zone: 265 ℃, metering zone: 270 ℃; Spinning manifold: 270 ℃; Get high-strength and high-modulus PET gel fiber after extruding, the gel fiber solid content that records gained is 14.5%.
Embodiment 30
UHMWPVC powder: molecular weight 100,000; Solvent: oxolane (UHMWPVC powder, solvent are 10: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 50 ℃, mix and stirred 180 minutes.The spinning barrel temperature, 50 ℃; , the spinning barrel is cooled to 10 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3500 rev/mins; The desolventizing time: 30 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 70 ℃, the preheating zone: 70 ℃, melting zone: 75 ℃, the compressional zone: 75 ℃, metering zone: 80 ℃; Spinning manifold: 80 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is a water, and temperature is 0 ℃, and the predraft multiple is 1.5.The gel fiber solid content that records gained is 46.3%.
Embodiment 31
UHMWPVC powder: molecular weight 200,000; Solvent: cyclohexanone (UHMWPVC powder, solvent are 25: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 60 ℃, mix and stirred 180 minutes.The spinning barrel temperature, 80 ℃; , the spinning barrel is cooled to 20 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3600 rev/mins; The desolventizing time: 200 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 70 ℃, the preheating zone: 70 ℃, melting zone: 70 ℃, the compressional zone: 75 ℃, metering zone: 80 ℃; Spinning manifold: 90 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is a water, and temperature is 20 ℃, and the predraft multiple is 20.The gel fiber solid content that records gained is 50.1%.
Embodiment 32
UHMWPVC powder: molecular weight 200,000; Solvent: chloroform (UHMWPVC powder, solvent are 20: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 60 ℃, mix and stirred 180 minutes.The spinning barrel temperature, 80 ℃; , the spinning barrel is cooled to 30 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3600 rev/mins; The desolventizing time: 50 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 70 ℃, the preheating zone: 70 ℃, melting zone: 70 ℃, the compressional zone: 75 ℃, metering zone: 80 ℃; Spinning manifold: 90 ℃, measuring pump: 20 rev/mins, the shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is a water, and temperature is 10 ℃, and the predraft multiple is 2.The gel fiber solid content that records gained is 48.3%.
Embodiment 33:
Super high molecular weight nylon 6, molecular weight 50,000; Solvent: nitroethane (nylon powder, solvent are 10: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 100 ℃, mix and stirred 240 minutes.The spinning barrel temperature, 160 ℃; , the spinning barrel is cooled to 10 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3500 rev/mins; The desolventizing time: 30 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 150 ℃, the preheating zone: 155 ℃, melting zone: 170 ℃, the compressional zone: 190 ℃, metering zone: 210 ℃; Spinning manifold: 235 ℃, measuring pump: 20 rev/mins, melt shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is a water, and temperature is 0 ℃, and the predraft multiple is 1.5.The gel fiber solid content that records gained is 33.1%.
Embodiment 34:
Super high molecular weight nylon 6, molecular weight 100,000; Solvent: nitromethane (nylon powder, solvent are 25: 100 by mass percentage); Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 150 ℃, mix and stirred 240 minutes.The spinning barrel temperature, 240 ℃; , the spinning barrel is cooled to 10 ℃ after being extruded into the melt strip naturally; The machinery pelletizing is pulverized, and getting the pellet average diameter is 15mm; Mechanical centrifuge rotating speed: 3500 rev/mins; The desolventizing time: 200 minutes.Gained spinning pellet is carried out the screw rod melt spinning; The screw rod spinning temperature, feed zone: 150 ℃, the preheating zone: 155 ℃, melting zone: 170 ℃, the compressional zone: 180 ℃, metering zone: 220 ℃; Spinning manifold: 250 ℃, measuring pump: 20 rev/mins, melt shower nozzle extruded velocity: 3.2 meters/minute, winding speed: 16 meters/minute; Coagulating agent is a water, and temperature is 20 ℃, and the predraft multiple is 2.The gel fiber solid content that records gained is 35.8%.
Comparative Examples 7:
Super high molecular weight nylon 6, molecular weight 100,000; Solvent: nitroethane; Polymer powders and solvent are mixed also heated and stirred, solution temperature in dissolution kettle: 100 ℃, mix and stirred 240 minutes.The spinning barrel temperature, 130 ℃; Make high-strength and high-modulus nylon 6 gel fibers, the gel fiber solid content that records gained is 10.5%.
Claims (9)
1. the preparation method of a gel fiber; It is characterized in that: with polymer powders and solvent and heated and stirred, process the melt strip after polymer powders dissolves fully, granulation after cooling is the frozen glue shape; Then institute's granulation is sloughed partial solvent; Again the polymer gel particle behind desolventizing is carried out melt spinning, predraft is reeled after coagulating bath, makes the polymer gel silk of high solids content; The described partial solvent of sloughing is meant that obtaining solid content is that the polymer spinning raw material of 20wt%～80wt% is the polymer gel particle; Be to adopt the centrifugal physics de-oiling of high-speed rotating machine equipment; Rotating speed is 500～9000 rev/mins, and the de-oiling time is 30-200min.
2. the preparation method of a kind of gel fiber as claimed in claim 1; It is characterized in that described polymer is that molecular weight is that 1,500,000～8,000,000 UHMWPE, molecular weight are that 400,000～2,000,000 UHMWPP, molecular weight are that 100,000～300,000 UHMWPAN, molecular weight are that 100,000～200,000 UHMWPVA, molecular weight are that 50,000～200,000 UHMWPET, molecular weight are that 100,000～250,000 UHMWPVC or molecular weight are 50,000～100,000 nylon.
3. the preparation method of a kind of gel fiber as claimed in claim 1 is characterized in that, described polymer powders average grain diameter is 10 μ m～200 μ m; The mixed proportion of described polymer powders and solvent is respectively:
UHMWPE or UHMWPP polymer powders and solvent are 4～10: 100 by mass ratio; The dissolving of these two kinds of polymer also comprises adding antioxidant; The addition of antioxidant is 2%～5% of a solute quality; The dissolving of UHMWPP polymer also comprises the adding nucleator, and the addition of nucleator is 5～30% of a solute quality;
UHMWPAN polymer powders and solvent are 5～25: 100 by mass ratio;
UHMWPVA polymer powders and solvent are 10～30: 100 by mass ratio;
UHMWPET polymer powders and solvent are 6～25: 100 by mass ratio;
UHMWPVC polymer powders and solvent are 10～25: 100 by mass ratio;
Nylon polymer powder and solvent are 10～25: 100 by mass ratio.
4. like the preparation method of claim 1 or 3 described a kind of gel fibers, it is characterized in that described solvent is respectively:
Solvent for use was mineral oil, white oil, paraffin oil or kerosene when polymer was UHMWPE or UHMWPP;
Solvent for use was DMF, DMSO, DMAc or the 50% NaSCN aqueous solution when polymer was UHMWPAN;
Solvent for use was DMF, DMSO, organic hydroxy compounds, glycerine or N-Methyl pyrrolidone when polymer was UHMWPVA;
Solvent for use was trifluoroacetic acid, nitrobenzene, hexafluoroisopropanol, chloroform or chlorophenol when polymer was UHMWPET;
Solvent for use was oxolane, cyclohexanone or chloroform when polymer was UHMWPVC;
Solvent for use was nitromethane or nitroethane when polymer was nylon.
5. the preparation method of a kind of gel fiber as claimed in claim 3 is characterized in that, described antioxidant is antioxidant 300, antioxidant 330, antioxidant 168, antioxidant 1076, antioxidant 1010, anti-oxidant DLTP or antioxidant DSTP;
Described nucleator is a tricarballylic acid type amide compound, 1,3, one or more combination in the middle of 5-benzenetricarboxylic acid derivative, Sodium Benzoate, two (4-(tert-butyl group) benzoic acid) hydroxy Al.
6. the preparation method of a kind of gel fiber as claimed in claim 1 is characterized in that, the described melt strip of processing is to adopt the method that makes through behind screw rod fusion or the spinning barrel; The temperature of described heated and stirred does;
The temperature of UHMWPE or the described heated and stirred of UHMWPP polymer powders is 50 ℃～190 ℃; The screw rod melt temperature is 90 ℃～190 ℃ when processing the melt strip;
The temperature of the described heated and stirred of UHMWPAN polymer powders is 50 ℃～90 ℃; The spinning barrel temperature is 80 ℃～100 ℃ when processing the melt strip;
The temperature of the described heated and stirred of UHMWPVA polymer powders is 70 ℃～90 ℃; The spinning barrel temperature is 65 ℃～85 ℃ when processing the melt strip;
The temperature of the described heated and stirred of UHMWPET polymer powders is 170 ℃～210 ℃; The screw rod fusion is 210 ℃～270 ℃ when processing the melt strip;
The temperature of the described heated and stirred of UHMWPVC polymer powders is 50 ℃～60 ℃; The spinning barrel temperature is 50 ℃～80 ℃ when processing the melt strip;
The temperature of the described heated and stirred of nylon polymer powder is 100 ℃～150 ℃; The spinning barrel temperature is 160 ℃～240 ℃ when processing the melt strip.
7. the preparation method of a kind of gel fiber as claimed in claim 1 is characterized in that, described cooling is meant and is cooled to 10 ℃～30 ℃ that cooling method is the nature cooling; The granulation of mechanical pelletizing method is adopted in described granulation, and gained pellet average grain diameter is of a size of 0.1mm～30mm.
8. the preparation method of a kind of gel fiber as claimed in claim 1 is characterized in that, described melt spinning adopts the screw rod extruding spinning, and temperature is:
The described screw rod spinning temperature of UHMWPE or UHMWPP polymer powders is 140 ℃～265 ℃;
The described screw rod spinning temperature of UHMWPAN polymer powders is 50 ℃～90 ℃;
The described screw rod spinning temperature of UHMWPVA polymer powders is 50 ℃～80 ℃;
The described screw rod spinning temperature of UHMWPET polymer powders is 200 ℃～280 ℃;
The described screw rod spinning temperature of UHMWPVC polymer powders is 70 ℃～90 ℃;
The described screw rod spinning temperature of nylon polymer powder is 150 ℃～250 ℃;
The coagulating agent that described coagulating bath is selected for use is:
The used coagulating agent of UHMWPE or UHMWPP is a water, and temperature is-10 ℃～10 ℃;
The used coagulating agent of UHMWPAN is the solution that water or solvent and water are made into, and described solvent and water volume ratio are 1～9: 3; The temperature range of coagulating bath is 20～110 ℃;
The used coagulating agent of UHMWPVA is methyl alcohol, ethanol, propyl alcohol, butanols, acetone or decahydronaphthalenes, and temperature is-10 ℃～0 ℃;
The used coagulating agent of UHMWPET is methyl alcohol, ethanol, propyl alcohol, acetone, and temperature is 10 ℃～50 ℃;
The used coagulating agent of UHMWPVC is a water, 0 ℃～20 ℃ of the temperature of coagulating bath;
The used coagulating agent of nylon is a water, and temperature is-10 ℃～20 ℃.
9. the preparation method of a kind of gel fiber as claimed in claim 1 is characterized in that, described predraft multiple is 1.5～20, and the solid content of the polymer gel silk of described high solids content is 20%～80%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010100231807A CN101787577B (en) | 2010-01-22 | 2010-01-22 | Novel method for preparing gel fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010100231807A CN101787577B (en) | 2010-01-22 | 2010-01-22 | Novel method for preparing gel fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101787577A CN101787577A (en) | 2010-07-28 |
| CN101787577B true CN101787577B (en) | 2012-05-09 |
Family
ID=42530950
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010100231807A Active CN101787577B (en) | 2010-01-22 | 2010-01-22 | Novel method for preparing gel fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101787577B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534838B (en) * | 2010-12-07 | 2014-09-03 | 北京同益中特种纤维技术开发有限公司 | Ultra-high molecular weight polyethylene fiber spinning stock solution and preparation method thereof |
| CN102581979A (en) * | 2012-03-26 | 2012-07-18 | 江苏锵尼玛新材料有限公司 | Method for preparing ultra high molecular weight polyethylene gel granules and application of polyethylene gel granules |
| CN103541024B (en) * | 2013-10-11 | 2017-04-05 | 剑乔科技江苏有限公司 | The preparation method of ultra-high molecular weight polyethylene gel fiber |
| CN109355718A (en) * | 2018-10-31 | 2019-02-19 | 盐城优和博新材料有限公司 | A kind of production technology of high-tenacity polyethylene fibre |
| CN109943900A (en) * | 2019-03-28 | 2019-06-28 | 浙江千禧龙纤特种纤维股份有限公司 | A kind of high-tenacity polyethylene fibre gel spinning system preprocess method |
| CN113502568B (en) * | 2021-05-11 | 2023-05-12 | 浙江毅聚新材料有限公司 | Method and equipment for separating white oil contained in ultra-high molecular weight polyethylene fiber gel silk |
| CN115045037A (en) * | 2022-07-14 | 2022-09-13 | 山东莱威新材料有限公司 | Preparation method of ultrahigh molecular weight polyethylene fiber web with strength greater than 39cN/dtex |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4413110A (en) * | 1981-04-30 | 1983-11-01 | Allied Corporation | High tenacity, high modulus polyethylene and polypropylene fibers and intermediates therefore |
| CN1816587A (en) * | 2003-02-26 | 2006-08-09 | 欧姆里顿科技有限公司 | Polymer gel-processing techniques and high modulus products |
-
2010
- 2010-01-22 CN CN2010100231807A patent/CN101787577B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4413110A (en) * | 1981-04-30 | 1983-11-01 | Allied Corporation | High tenacity, high modulus polyethylene and polypropylene fibers and intermediates therefore |
| CN1816587A (en) * | 2003-02-26 | 2006-08-09 | 欧姆里顿科技有限公司 | Polymer gel-processing techniques and high modulus products |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2006-336140A 2006.12.14 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101787577A (en) | 2010-07-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101787577B (en) | Novel method for preparing gel fiber | |
| CN101775666B (en) | Preparation method of high-strength high-modulus polyethylene fiber | |
| CN101230499B (en) | Coloured high-strength polyethylene fibre and method for manufacturing same | |
| CN100339519C (en) | Method of preparing high performance polyvinyl alcohel fiber | |
| JP5144641B2 (en) | High molecular weight poly (α-olefin) solutions and articles made therefrom | |
| CN102586925B (en) | Method for preparing coloured fibers for ultrahigh molecular weight polyethylene (UHMWPE) ropes and nets | |
| CN102226300B (en) | Preparation method of high strength polyethylene fiber and special device thereof | |
| CN102776597B (en) | High-strength and high-modulus polyvinyl alcohol fiber and melt spinning method of high-strength and high-modulus polyvinyl alcohol fiber | |
| CN102505158A (en) | High-concentration preparation method for ultra-high molecular weight polyethylene fiber | |
| CN101886295A (en) | Ultra-high molecular weight polyethylene colored fibers and preparation method thereof | |
| CN106948022B (en) | The preparation method of high concentration ultra high molecular weight polyethylene fiber spinning solution | |
| CN101368300B (en) | Polyphenyl thioether/ultra-fine calcium carbonate particulate composite fiber and preparation method thereof | |
| CN109440215A (en) | A kind of preparation method of high-performance polyethylene fibres | |
| CN101575743B (en) | Preparation method of spinning solution of ultra-high molecular weight polyethylene fiber | |
| AU2012323656A1 (en) | Gelatinized pre-oriented filaments and preparation method thereof, and ultra-high molecular weight polyethylene fibers and preparation method thereof | |
| CN101718003B (en) | Method for producing ultra-high molecular weight polyethylene colored fine denier fiber | |
| CN109385689A (en) | A kind of spinning process that ultra-high molecular weight polyethylene is blended | |
| CN105885154B (en) | A kind of melt-spun pinches composite modified superhigh molecular polyethylene blend composition and preparation method thereof with molten | |
| CN109371475A (en) | A kind of spinning process of ultra-high molecular weight polyethylene | |
| CN101397697A (en) | Gel-spun ultra-high molecular weight polypropylene/ultra-high molecular weight polyethylene complex fiber and preparation method thereof | |
| CN102797050B (en) | Melt spinning method for high-strength high-modulus polyvinyl alcohol fiber | |
| CN110791821A (en) | Method for preparing novel ultrahigh-strength high-modulus polyethylene fiber by one-step method | |
| CN108004605A (en) | Strong porous superhigh molecular weight polyethylene fibers and preparation method in one kind | |
| CN101851796B (en) | Method for processing wearable blended and modified polypropylene monofilaments for manufacturing fishing rope | |
| CN103147150B (en) | Preparation method of monofilament for net cage body and trawl fishing gear |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20100728 Assignee: Jiuli Rope Co., Ltd. Assignor: Donghua University Contract record no.: 2016320000006 Denomination of invention: Novel method for preparing gel fiber Granted publication date: 20120509 License type: Exclusive License Record date: 20160114 |
|
| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model |