CN103756659A - Flexible particle diverter and preparation method thereof - Google Patents
Flexible particle diverter and preparation method thereof Download PDFInfo
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- CN103756659A CN103756659A CN201310756260.7A CN201310756260A CN103756659A CN 103756659 A CN103756659 A CN 103756659A CN 201310756260 A CN201310756260 A CN 201310756260A CN 103756659 A CN103756659 A CN 103756659A
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- diisopropyl azodicarboxylate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/5083—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
Abstract
The invention belongs to a flexible particle diverter and a preparation method thereof. The diverter is prepared from the following raw materials in parts by weight: 30-40 parts of polyacrylate liquid rubber, 100-120 parts of bisphenol A epoxy resin, 0.05-0.1 part of a peroxide initiator and 0.5-2 parts of an epoxy resin curing agent, wherein the polyacrylate liquid rubber is prepared from the following raw materials: n-butyl alcohol, butyl acrylate, ethyl acrylate, glycidyl acrylate, azodiisobutyronitrile and nitrogen; the peroxide initiator is either benzoyl peroxide or tert-butyl peroxybenzoate; the epoxy resin curing agent is one of polysebacic polyanhydride, polyazelaic polyanhydride, maleic anhydride and tung oil anhydride. The flexible particle diverter, which has flexible particles, has the advantages of no toxicity, good plugging effect on narrow cracks, temperature resistant, mineralization resistant and excellent in shearing resistance.
Description
Technical field
The invention belongs to oilfield chemical technical field, be specifically related to a kind of flexible particle diversion agent and preparation method thereof.
Background technology
Refracturing is as the technical measures of old oil and water well (oil well and the water injection well) comprehensive regulation, is the great difficult problem that urgent need that each oil field faces solves.According to research both domestic and external and experiment, show, for this old well, adopt suitable refracturing can continue to obtain greatly volume increase or augmented injection effect.
Continuing to extend primary fracture is before this more general refracturing concept, but the refracturing of this mode presses rear stable production period shorter, and effect of increasing production is undesirable; Meanwhile, along with the continuous exploitation in oil field, the increase of fracturing fracture length is achieved by a variety of factors again and can not unconfinedly increases, so make the refracturing effect of carrying out under this guiding theory worse and worse.
It is to utilize special crack stifled diversion agent temporarily that crack turns to multiple fracturing technique, first fracturing fracture is carried out to effective shutoff, in the direction that is parallel to first pressure break supporting crack, realizing operation pressure stops, change refracturing fracture orientation, the drainage area that first pressure break is not fed through to is effectively transformed, thereby improve the effect of increasing production of refracturing, for the water injection well that fracturing reform is crossed, crack steering-effecting due to refracturing, can make waterflood direction depart from the first crack that has been subject to severe contamination for the first time, thereby reduction water injection pressure, improve water regain and waterflood swept area.
Existing diversion agent has easy construction, can go deep into oil deposit deep part and dynamically involve effective advantage; But there is following defect: 1, pellet hardness is large simultaneously, large to well bore wall harm; 2, for narrow and small crack shutoff weak effect, do not reach the effect that deep turns to; 3, toxicity is large; 4, heatproof, resistance to salinity and endurance of cutting can be poor.
Summary of the invention
The object of the invention is to overcome defect of the prior art, and a kind of flexible particle, nontoxicity,, heatproof effective to the shutoff of narrow and small crack are provided, flexible particle diversion agent that resistance to salinity and endurance of cutting can be good and preparation method thereof.
The object of the present invention is achieved like this: this diversion agent comprises that following raw materials according is formulated according to parts by weight: 30 parts～40 parts of polyacrylic ester fluid rubbers, 100 parts～120 parts of bisphenol A type epoxy resins, 0.5 part～2 parts of 0.05 part～0.1 part of peroxide initiator and epoxy curing agents; Described polyacrylic ester fluid rubber comprises that following raw materials according is according to formulated: propyl carbinol, butyl acrylate, ethyl propenoate, glycidyl acrylate, Diisopropyl azodicarboxylate and nitrogen; Described peroxide initiator is one of benzoyl peroxide or peroxidized t-butyl perbenzoate; Described epoxy curing agent is poly sebacic polyanhydride, poly-nonane diacid acid anhydride, one of MALEIC ANHYDRIDE or tung oil acid anhydride.Described polyacrylic ester fluid rubber comprises that following raw materials according is formulated according to parts by weight: 20 parts of propyl carbinols, 5 parts of butyl acrylates, 5 parts of ethyl propenoates, 2.5 parts of glycidyl acrylates, 20 parts of 0.01 part of Diisopropyl azodicarboxylate and nitrogen.
A preparation method for flexible particle diversion agent, this preparation method comprises the steps:
One, by butyl acrylate, ethyl propenoate and glycidyl acrylate are put into propyl carbinol, evenly mix, and make mixing solutions;
Two, at room temperature Diisopropyl azodicarboxylate is added in the mixing solutions of step 1;
Three, make to add in step 2 the mixing solutions of Diisopropyl azodicarboxylate under nitrogen protection, be heated to 100 ℃ and react, the reaction times is 3 hours;
Four, by reacted solution in step 3 by underpressure distillation, underpressure distillation goes out unreacted monomer and solvent, can obtain polyacrylic ester fluid rubber;
Five,, by polyacrylic ester fluid rubber and bisphenol A type epoxy resin in step 4, peroxide initiator and epoxy curing agent, be evenly mixed to get mixture;
Six, by the mixture in step 5 in mixing facilities mixing 5 minutes～10 minutes, melting temperature was 130 ℃～150 ℃, obtains blend;
Seven, the blend in step 6 is cooled to after 80 ℃～100 ℃, puts into the granulation of DY180 series forcing machine.
A flexible particle diversion agent, this diversion agent comprises that following raw materials according is formulated according to parts by weight: 33 parts of polyacrylic ester fluid rubbers, 106 parts of bisphenol A type epoxy resins, 0.9 part of 0.09 part of peroxide initiator and epoxy curing agent; Described polyacrylic ester fluid rubber comprises that following raw materials according is formulated according to parts by weight: 20 parts of propyl carbinols, 5 parts of butyl acrylates, 5 parts of ethyl propenoates, 2.5 parts of glycidyl acrylates, 20 parts of 0.01 part of Diisopropyl azodicarboxylate and nitrogen; Described peroxide initiator is peroxidized t-butyl perbenzoate; Described epoxy curing agent is tung oil acid anhydride; Preparation method comprises the steps:
One, by butyl acrylate, ethyl propenoate and glycidyl acrylate are put into propyl carbinol, evenly mix, and make mixing solutions;
Two, at room temperature Diisopropyl azodicarboxylate is added in the mixing solutions of step 1;
Three, make to add in step 2 the mixing solutions of Diisopropyl azodicarboxylate under nitrogen protection, be heated to 100 ℃ and react, the reaction times is 3 hours;
Four, by reacted solution in step 3 by underpressure distillation, underpressure distillation goes out unreacted monomer and solvent, can obtain polyacrylic ester fluid rubber;
Five,, by polyacrylic ester fluid rubber and bisphenol A type epoxy resin in step 4, peroxidized t-butyl perbenzoate and tung oil acid anhydride, be evenly mixed to get mixture;
Six, by the mixture in step 5 in mixing facilities mixing 5 minutes～10 minutes, melting temperature was 130 ℃～150 ℃, obtains blend;
Seven, the blend in step 6 is cooled to after 80 ℃～100 ℃, puts into the granulation of DY180 series forcing machine.
A flexible particle diversion agent, this diversion agent comprises that following raw materials according is formulated according to parts by weight: 38 parts of polyacrylic ester fluid rubbers, 117 parts of bisphenol A type epoxy resins, 1.2 parts of 0.07 part of peroxide initiator and epoxy curing agents; Described polyacrylic ester fluid rubber comprises that following raw materials according is formulated according to parts by weight: 20 parts of propyl carbinols, 5 parts of butyl acrylates, 5 parts of ethyl propenoates, 2.5 parts of glycidyl acrylates, 20 parts of 0.01 part of Diisopropyl azodicarboxylate and nitrogen; Described peroxide initiator is benzoyl peroxide; Described epoxy curing agent is poly-nonane diacid acid anhydride, and preparation method comprises the steps:
One, by butyl acrylate, ethyl propenoate and glycidyl acrylate are put into propyl carbinol, evenly mix, and make mixing solutions;
Two, at room temperature Diisopropyl azodicarboxylate is added in the mixing solutions of step 1;
Three, make to add in step 2 the mixing solutions of Diisopropyl azodicarboxylate under nitrogen protection, be heated to 100 ℃ and react, the reaction times is 3 hours;
Four, by reacted solution in step 3 by underpressure distillation, underpressure distillation goes out unreacted monomer and solvent, can obtain polyacrylic ester fluid rubber;
Five,, by polyacrylic ester fluid rubber and bisphenol A type epoxy resin in step 4, peroxide initiator and epoxy curing agent, be evenly mixed to get mixture;
Six, by the mixture in step 5 in mixing facilities mixing 5 minutes～10 minutes, melting temperature was 130 ℃～150 ℃, obtains blend;
Seven, the blend in step 6 is cooled to after 80 ℃～100 ℃, puts into the granulation of DY180 series forcing machine.
A flexible particle diversion agent, this diversion agent comprises that following raw materials according is formulated according to parts by weight: 32 parts of polyacrylic ester fluid rubbers, 119 parts of bisphenol A type epoxy resins, 0.6 part of 0.08 part of peroxide initiator and epoxy curing agent; Described polyacrylic ester fluid rubber comprises that following raw materials according is formulated according to parts by weight: 20 parts of propyl carbinols, 5 parts of butyl acrylates, 5 parts of ethyl propenoates, 2.5 parts of glycidyl acrylates, 20 parts of 0.01 part of Diisopropyl azodicarboxylate and nitrogen; Described peroxide initiator is one of benzoyl peroxide or peroxidized t-butyl perbenzoate; Described epoxy curing agent is poly sebacic polyanhydride, poly-nonane diacid acid anhydride, one of MALEIC ANHYDRIDE or tung oil acid anhydride, and preparation method comprises the steps:
One, by butyl acrylate, ethyl propenoate and glycidyl acrylate are put into propyl carbinol, evenly mix, and make mixing solutions;
Two, at room temperature Diisopropyl azodicarboxylate is added in the mixing solutions of step 1;
Three, make to add in step 2 the mixing solutions of Diisopropyl azodicarboxylate under nitrogen protection, be heated to 100 ℃ and react, the reaction times is 3 hours;
Four, by reacted solution in step 3 by underpressure distillation, underpressure distillation goes out unreacted monomer and solvent, can obtain polyacrylic ester fluid rubber;
Five,, by polyacrylic ester fluid rubber and bisphenol A type epoxy resin in step 4, peroxide initiator and epoxy curing agent, be evenly mixed to get mixture;
Six, by the mixture in step 5 in mixing facilities mixing 5 minutes～10 minutes, melting temperature was 130 ℃～150 ℃, obtains blend;
Seven, the blend in step 6 is cooled to after 80 ℃～100 ℃, puts into the granulation of DY180 series forcing machine.
Performance evaluation of the present invention is:
1, hardness: it is 0 degree that Shore durometer is measured hardness.
2, elasticity: measure elasticity of the present invention by vertical resilience test instrument, measurement result 25%, illustrates that product elasticity of the present invention is fine.
3, waterpower high pressure is broken through experiment: the present invention is made to 2mm thin slice, carry out waterpower high pressure break through experiment by the water-fast column test instrument of high pressure, with 567kPa/min pressurization, to 12.6kPa, just start water breakthrough infiltration, illustrate that toughness of the present invention is fine.
4, salt tolerance and temperature tolerance:
Table 1 salt tolerant, temperature tolerance are investigated result
By above result, show and show: the present invention have be flexiblely easy to infusion, toughness is high, the advantages such as heatproof and salt resistant character excellence.
Tool of the present invention has the following advantages:
1, under certain pressure reduction, can be out of shape by hole and shout, inhomogeneous formation is had to the feature of " self-adaptation ", there is larger " permission "; 2, by distortion, temporary stifled, pulsating flow, at ground floor height, ooze position and produce dynamically along journey resistance to flow, cause follow-up injected water to turn to and go to hypotonic position; 3, along not being sheared destruction in journey migration process; 4, in macropore migration, there is larger resistance, do not enter low-permeability layer; 5, can be placed on easily earth formation deep, heat-resistant salt-resistant, formation condition is long lower steady time.
Embodiment
The present invention is flexible particle diversion agent, now in conjunction with specific embodiments the present invention is further described.Concrete embodiment is as follows:
Embodiment mono-
A flexible particle diversion agent, this diversion agent comprises that following raw materials according is formulated according to parts by weight: 30 parts of polyacrylic ester fluid rubbers, 100 parts of bisphenol A type epoxy resins, 0.5 part of 0.05 part of peroxide initiator and epoxy curing agent; Described polyacrylic ester fluid rubber comprises that following raw materials according is according to formulated: propyl carbinol, butyl acrylate, ethyl propenoate, glycidyl acrylate, Diisopropyl azodicarboxylate and nitrogen; Described peroxide initiator is benzoyl peroxide; Described epoxy curing agent is poly sebacic polyanhydride.Described polyacrylic ester fluid rubber comprises that following raw materials according is formulated according to parts by weight: 20 parts of propyl carbinols, 5 parts of butyl acrylates, 5 parts of ethyl propenoates, 2.5 parts of glycidyl acrylates, 20 parts of 0.01 part of Diisopropyl azodicarboxylate and nitrogen.Preparation method comprises the steps:
One, by butyl acrylate, ethyl propenoate and glycidyl acrylate are put into propyl carbinol, evenly mix, and make mixing solutions;
Two, at room temperature Diisopropyl azodicarboxylate is added in the mixing solutions of step 1;
Three, make to add in step 2 the mixing solutions of Diisopropyl azodicarboxylate under nitrogen protection, be heated to 100 ℃ and react, the reaction times is 3 hours;
Four, by reacted solution in step 3 by underpressure distillation, underpressure distillation goes out unreacted monomer and solvent, can obtain polyacrylic ester fluid rubber;
Five,, by polyacrylic ester fluid rubber and bisphenol A type epoxy resin in step 4, peroxide initiator and epoxy curing agent, be evenly mixed to get mixture;
Six, by the mixture in step 5 in mixing facilities mixing 5 minutes～10 minutes, melting temperature was 130 ℃～150 ℃, obtains blend;
Seven, the blend in step 6 is cooled to after 80 ℃～100 ℃, puts into the granulation of DY180 series forcing machine.
Embodiment bis-
A flexible particle diversion agent, this diversion agent comprises that following raw materials according is formulated according to parts by weight: 5 parts of polyacrylic ester fluid rubbers, 110 parts of bisphenol A type epoxy resins, 1.3 parts of 0.08 part of peroxide initiator and epoxy curing agents; Described polyacrylic ester fluid rubber comprises that following raw materials according is according to formulated: propyl carbinol, butyl acrylate, ethyl propenoate, glycidyl acrylate, Diisopropyl azodicarboxylate and nitrogen; Described peroxide initiator is peroxidized t-butyl perbenzoate; Described epoxy curing agent is poly-nonane diacid acid anhydride.Described polyacrylic ester fluid rubber comprises that following raw materials according is formulated according to parts by weight: 20 parts of propyl carbinols, 5 parts of butyl acrylates, 5 parts of ethyl propenoates, 2.5 parts of glycidyl acrylates, 20 parts of 0.01 part of Diisopropyl azodicarboxylate and nitrogen.Preparation method comprises the steps:
One, by butyl acrylate, ethyl propenoate and glycidyl acrylate are put into propyl carbinol, evenly mix, and make mixing solutions;
Two, at room temperature Diisopropyl azodicarboxylate is added in the mixing solutions of step 1;
Three, make to add in step 2 the mixing solutions of Diisopropyl azodicarboxylate under nitrogen protection, be heated to 100 ℃ and react, the reaction times is 3 hours;
Four, by reacted solution in step 3 by underpressure distillation, underpressure distillation goes out unreacted monomer and solvent, can obtain polyacrylic ester fluid rubber;
Five,, by polyacrylic ester fluid rubber and bisphenol A type epoxy resin in step 4, peroxide initiator and epoxy curing agent, be evenly mixed to get mixture;
Six, by the mixture in step 5 in mixing facilities mixing 5 minutes～10 minutes, melting temperature was 130 ℃～150 ℃, obtains blend;
Seven, the blend in step 6 is cooled to after 80 ℃～100 ℃, puts into the granulation of DY180 series forcing machine.
Embodiment tri-
A flexible particle diversion agent, this diversion agent comprises that following raw materials according is formulated according to parts by weight: 40 parts of polyacrylic ester fluid rubbers, 120 parts of bisphenol A type epoxy resins, 2 parts of 0.1 part of peroxide initiator and epoxy curing agents; Described polyacrylic ester fluid rubber comprises that following raw materials according is according to formulated: propyl carbinol, butyl acrylate, ethyl propenoate, glycidyl acrylate, Diisopropyl azodicarboxylate and nitrogen; Described peroxide initiator is benzoyl peroxide; Described epoxy curing agent is MALEIC ANHYDRIDE.Described polyacrylic ester fluid rubber comprises that following raw materials according is formulated according to parts by weight: 20 parts of propyl carbinols, 5 parts of butyl acrylates, 5 parts of ethyl propenoates, 2.5 parts of glycidyl acrylates, 20 parts of 0.01 part of Diisopropyl azodicarboxylate and nitrogen.Preparation method comprises the steps:
One, by butyl acrylate, ethyl propenoate and glycidyl acrylate are put into propyl carbinol, evenly mix, and make mixing solutions;
Two, at room temperature Diisopropyl azodicarboxylate is added in the mixing solutions of step 1;
Three, make to add in step 2 the mixing solutions of Diisopropyl azodicarboxylate under nitrogen protection, be heated to 100 ℃ and react, the reaction times is 3 hours;
Four, by reacted solution in step 3 by underpressure distillation, underpressure distillation goes out unreacted monomer and solvent, can obtain polyacrylic ester fluid rubber;
Five,, by polyacrylic ester fluid rubber and bisphenol A type epoxy resin in step 4, peroxide initiator and epoxy curing agent, be evenly mixed to get mixture;
Six, by the mixture in step 5 in mixing facilities mixing 5 minutes～10 minutes, melting temperature was 130 ℃～150 ℃, obtains blend;
Seven, the blend in step 6 is cooled to after 80 ℃～100 ℃, puts into the granulation of DY180 series forcing machine.
Embodiment tetra-
A flexible particle diversion agent, this diversion agent comprises that following raw materials according is formulated according to parts by weight: 33 parts of polyacrylic ester fluid rubbers, 106 parts of bisphenol A type epoxy resins, 0.9 part of 0.09 part of peroxide initiator and epoxy curing agent; Described polyacrylic ester fluid rubber comprises that following raw materials according is formulated according to parts by weight: 20 parts of propyl carbinols, 5 parts of butyl acrylates, 5 parts of ethyl propenoates, 2.5 parts of glycidyl acrylates, 20 parts of 0.01 part of Diisopropyl azodicarboxylate and nitrogen; Described peroxide initiator is peroxidized t-butyl perbenzoate; Described epoxy curing agent is tung oil acid anhydride; Preparation method comprises the steps:
One, by butyl acrylate, ethyl propenoate and glycidyl acrylate are put into propyl carbinol, evenly mix, and make mixing solutions;
Two, at room temperature Diisopropyl azodicarboxylate is added in the mixing solutions of step 1;
Three, make to add in step 2 the mixing solutions of Diisopropyl azodicarboxylate under nitrogen protection, be heated to 100 ℃ and react, the reaction times is 3 hours;
Four, by reacted solution in step 3 by underpressure distillation, underpressure distillation goes out unreacted monomer and solvent, can obtain polyacrylic ester fluid rubber;
Five,, by polyacrylic ester fluid rubber and bisphenol A type epoxy resin in step 4, peroxidized t-butyl perbenzoate and tung oil acid anhydride, be evenly mixed to get mixture;
Six, by the mixture in step 5 in mixing facilities mixing 5 minutes～10 minutes, melting temperature was 130 ℃～150 ℃, obtains blend;
Seven, the blend in step 6 is cooled to after 80 ℃～100 ℃, puts into the granulation of DY180 series forcing machine.
Embodiment five
A flexible particle diversion agent, this diversion agent comprises that following raw materials according is formulated according to parts by weight: 38 parts of polyacrylic ester fluid rubbers, 117 parts of bisphenol A type epoxy resins, 1.2 parts of 0.07 part of peroxide initiator and epoxy curing agents; Described polyacrylic ester fluid rubber comprises that following raw materials according is formulated according to parts by weight: 20 parts of propyl carbinols, 5 parts of butyl acrylates, 5 parts of ethyl propenoates, 2.5 parts of glycidyl acrylates, 20 parts of 0.01 part of Diisopropyl azodicarboxylate and nitrogen; Described peroxide initiator is benzoyl peroxide; Described epoxy curing agent is poly-nonane diacid acid anhydride, and preparation method comprises the steps:
One, by butyl acrylate, ethyl propenoate and glycidyl acrylate are put into propyl carbinol, evenly mix, and make mixing solutions;
Two, at room temperature Diisopropyl azodicarboxylate is added in the mixing solutions of step 1;
Three, make to add in step 2 the mixing solutions of Diisopropyl azodicarboxylate under nitrogen protection, be heated to 100 ℃ and react, the reaction times is 3 hours;
Four, by reacted solution in step 3 by underpressure distillation, underpressure distillation goes out unreacted monomer and solvent, can obtain polyacrylic ester fluid rubber;
Five,, by polyacrylic ester fluid rubber and bisphenol A type epoxy resin in step 4, peroxide initiator and epoxy curing agent, be evenly mixed to get mixture;
Six, by the mixture in step 5 in mixing facilities mixing 5 minutes～10 minutes, melting temperature was 130 ℃～150 ℃, obtains blend;
Seven, the blend in step 6 is cooled to after 80 ℃～100 ℃, puts into the granulation of DY180 series forcing machine.
Embodiment six
A flexible particle diversion agent, this diversion agent comprises that following raw materials according is formulated according to parts by weight: 32 parts of polyacrylic ester fluid rubbers, 119 parts of bisphenol A type epoxy resins, 0.6 part of 0.08 part of peroxide initiator and epoxy curing agent; Described polyacrylic ester fluid rubber comprises that following raw materials according is formulated according to parts by weight: 20 parts of propyl carbinols, 5 parts of butyl acrylates, 5 parts of ethyl propenoates, 2.5 parts of glycidyl acrylates, 20 parts of 0.01 part of Diisopropyl azodicarboxylate and nitrogen; Described peroxide initiator is one of benzoyl peroxide or peroxidized t-butyl perbenzoate; Described epoxy curing agent is poly sebacic polyanhydride, poly-nonane diacid acid anhydride, one of MALEIC ANHYDRIDE or tung oil acid anhydride, and preparation method comprises the steps:
One, by butyl acrylate, ethyl propenoate and glycidyl acrylate are put into propyl carbinol, evenly mix, and make mixing solutions;
Two, at room temperature Diisopropyl azodicarboxylate is added in the mixing solutions of step 1;
Three, make to add in step 2 the mixing solutions of Diisopropyl azodicarboxylate under nitrogen protection, be heated to 100 ℃ and react, the reaction times is 3 hours;
Four, by reacted solution in step 3 by underpressure distillation, underpressure distillation goes out unreacted monomer and solvent, can obtain polyacrylic ester fluid rubber;
Five,, by polyacrylic ester fluid rubber and bisphenol A type epoxy resin in step 4, peroxide initiator and epoxy curing agent, be evenly mixed to get mixture;
Six, by the mixture in step 5 in mixing facilities mixing 5 minutes～10 minutes, melting temperature was 130 ℃～150 ℃, obtains blend;
Seven, the blend in step 6 is cooled to after 80 ℃～100 ℃, puts into the granulation of DY180 series forcing machine.
Above-described embodiment is only for example is clearly described, and the not restriction to embodiment.For the common technique personnel in affiliated field, can also make other changes in different forms on the basis of the above description.Here exhaustive without also giving all embodiments, and the apparent variation of being amplified out thus or change are still among the protection domain in the invention claim.
Claims (6)
1. a flexible particle diversion agent, it is characterized in that: this diversion agent comprises that following raw materials according is formulated according to parts by weight: 30 parts～40 parts of polyacrylic ester fluid rubbers, 100 parts～120 parts of bisphenol A type epoxy resins, 0.5 part～2 parts of 0.05 part～0.1 part of peroxide initiator and epoxy curing agents; Described polyacrylic ester fluid rubber comprises that following raw materials according is according to formulated: propyl carbinol, butyl acrylate, ethyl propenoate, glycidyl acrylate, Diisopropyl azodicarboxylate and nitrogen; Described peroxide initiator is one of benzoyl peroxide or peroxidized t-butyl perbenzoate; Described epoxy curing agent is poly sebacic polyanhydride, poly-nonane diacid acid anhydride, one of MALEIC ANHYDRIDE or tung oil acid anhydride.
2. flexible particle diversion agent according to claim 1, it is characterized in that: described polyacrylic ester fluid rubber comprises that following raw materials according is formulated according to parts by weight: 20 parts of propyl carbinols, 5 parts of butyl acrylates, 5 parts of ethyl propenoates, 2.5 parts of glycidyl acrylates, 20 parts of 0.01 part of Diisopropyl azodicarboxylate and nitrogen.
3. the preparation method of flexible particle diversion agent according to claim 1, is characterized in that: this preparation method comprises the steps:
One, by butyl acrylate, ethyl propenoate and glycidyl acrylate are put into propyl carbinol, evenly mix, and make mixing solutions;
Two, at room temperature Diisopropyl azodicarboxylate is added in the mixing solutions of step 1;
Three, make to add in step 2 the mixing solutions of Diisopropyl azodicarboxylate under nitrogen protection, be heated to 100 ℃ and react, the reaction times is 3 hours;
Four, by reacted solution in step 3 by underpressure distillation, underpressure distillation goes out unreacted monomer and solvent, can obtain polyacrylic ester fluid rubber;
Five,, by polyacrylic ester fluid rubber and bisphenol A type epoxy resin in step 4, peroxide initiator and epoxy curing agent, be evenly mixed to get mixture;
Six, by the mixture in step 5 in mixing facilities mixing 5 minutes～10 minutes, melting temperature was 130 ℃～150 ℃, obtains blend;
Seven, the blend in step 6 is cooled to after 80 ℃～100 ℃, puts into the granulation of DY180 series forcing machine.
4. flexible particle diversion agent according to claim 1, it is characterized in that: this diversion agent comprises that following raw materials according is formulated according to parts by weight: 33 parts of polyacrylic ester fluid rubbers, 106 parts of bisphenol A type epoxy resins, 0.9 part of 0.09 part of peroxide initiator and epoxy curing agent; Described polyacrylic ester fluid rubber comprises that following raw materials according is formulated according to parts by weight: 20 parts of propyl carbinols, 5 parts of butyl acrylates, 5 parts of ethyl propenoates, 2.5 parts of glycidyl acrylates, 20 parts of 0.01 part of Diisopropyl azodicarboxylate and nitrogen; Described peroxide initiator is peroxidized t-butyl perbenzoate; Described epoxy curing agent is tung oil acid anhydride; Preparation method comprises the steps:
One, by butyl acrylate, ethyl propenoate and glycidyl acrylate are put into propyl carbinol, evenly mix, and make mixing solutions;
Two, at room temperature Diisopropyl azodicarboxylate is added in the mixing solutions of step 1;
Three, make to add in step 2 the mixing solutions of Diisopropyl azodicarboxylate under nitrogen protection, be heated to 100 ℃ and react, the reaction times is 3 hours;
Four, by reacted solution in step 3 by underpressure distillation, underpressure distillation goes out unreacted monomer and solvent, can obtain polyacrylic ester fluid rubber;
Five,, by polyacrylic ester fluid rubber and bisphenol A type epoxy resin in step 4, peroxidized t-butyl perbenzoate and tung oil acid anhydride, be evenly mixed to get mixture;
Six, by the mixture in step 5 in mixing facilities mixing 5 minutes～10 minutes, melting temperature was 130 ℃～150 ℃, obtains blend;
Seven, the blend in step 6 is cooled to after 80 ℃～100 ℃, puts into the granulation of DY180 series forcing machine.
5. flexible particle diversion agent according to claim 1, it is characterized in that: this diversion agent comprises that following raw materials according is formulated according to parts by weight: 38 parts of polyacrylic ester fluid rubbers, 117 parts of bisphenol A type epoxy resins, 1.2 parts of 0.07 part of peroxide initiator and epoxy curing agents; Described polyacrylic ester fluid rubber comprises that following raw materials according is formulated according to parts by weight: 20 parts of propyl carbinols, 5 parts of butyl acrylates, 5 parts of ethyl propenoates, 2.5 parts of glycidyl acrylates, 20 parts of 0.01 part of Diisopropyl azodicarboxylate and nitrogen; Described peroxide initiator is benzoyl peroxide; Described epoxy curing agent is poly-nonane diacid acid anhydride, and preparation method comprises the steps:
One, by butyl acrylate, ethyl propenoate and glycidyl acrylate are put into propyl carbinol, evenly mix, and make mixing solutions;
Two, at room temperature Diisopropyl azodicarboxylate is added in the mixing solutions of step 1;
Three, make to add in step 2 the mixing solutions of Diisopropyl azodicarboxylate under nitrogen protection, be heated to 100 ℃ and react, the reaction times is 3 hours;
Four, by reacted solution in step 3 by underpressure distillation, underpressure distillation goes out unreacted monomer and solvent, can obtain polyacrylic ester fluid rubber;
Five,, by polyacrylic ester fluid rubber and bisphenol A type epoxy resin in step 4, peroxide initiator and epoxy curing agent, be evenly mixed to get mixture;
Six, by the mixture in step 5 in mixing facilities mixing 5 minutes～10 minutes, melting temperature was 130 ℃～150 ℃, obtains blend;
Seven, the blend in step 6 is cooled to after 80 ℃～100 ℃, puts into the granulation of DY180 series forcing machine.
6. flexible particle diversion agent according to claim 1, it is characterized in that: this diversion agent comprises that following raw materials according is formulated according to parts by weight: 32 parts of polyacrylic ester fluid rubbers, 119 parts of bisphenol A type epoxy resins, 0.6 part of 0.08 part of peroxide initiator and epoxy curing agent; Described polyacrylic ester fluid rubber comprises that following raw materials according is formulated according to parts by weight: 20 parts of propyl carbinols, 5 parts of butyl acrylates, 5 parts of ethyl propenoates, 2.5 parts of glycidyl acrylates, 20 parts of 0.01 part of Diisopropyl azodicarboxylate and nitrogen; Described peroxide initiator is one of benzoyl peroxide or peroxidized t-butyl perbenzoate; Described epoxy curing agent is poly sebacic polyanhydride, poly-nonane diacid acid anhydride, one of MALEIC ANHYDRIDE or tung oil acid anhydride, and preparation method comprises the steps:
One, by butyl acrylate, ethyl propenoate and glycidyl acrylate are put into propyl carbinol, evenly mix, and make mixing solutions;
Two, at room temperature Diisopropyl azodicarboxylate is added in the mixing solutions of step 1;
Three, make to add in step 2 the mixing solutions of Diisopropyl azodicarboxylate under nitrogen protection, be heated to 100 ℃ and react, the reaction times is 3 hours;
Four, by reacted solution in step 3 by underpressure distillation, underpressure distillation goes out unreacted monomer and solvent, can obtain polyacrylic ester fluid rubber;
Five,, by polyacrylic ester fluid rubber and bisphenol A type epoxy resin in step 4, peroxide initiator and epoxy curing agent, be evenly mixed to get mixture;
Six, by the mixture in step 5 in mixing facilities mixing 5 minutes～10 minutes, melting temperature was 130 ℃～150 ℃, obtains blend;
Seven, the blend in step 6 is cooled to after 80 ℃～100 ℃, puts into the granulation of DY180 series forcing machine.
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| CN104099074A (en) * | 2014-06-10 | 2014-10-15 | 中国石油集团川庆钻探工程有限公司工程技术研究院 | Volume fracturing reconstruction crack plugging agent and water plugging construction method |
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| CN106426672A (en) * | 2016-11-08 | 2017-02-22 | 揭阳市越兴塑胶制品有限公司 | Epoxy resin plastic mold and preparation process thereof |
| CN109705827A (en) * | 2017-10-25 | 2019-05-03 | 中国石油化工股份有限公司 | Oil drilling leak stopping pressure-bearing agent and preparation method thereof |
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| CN103756659B (en) | 2016-08-03 |
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