CN102489048A - Antifoaming agent composition and preparation method thereof - Google Patents
Antifoaming agent composition and preparation method thereof Download PDFInfo
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Abstract
The invention provides an antifoaming agent composition and a preparation method thereof. The antifoaming active matter is prepared by carrying out a reaction of hydrogen-containing polysiloxane and vinyl polysiloxane, introducing polyether modified polyorganosiloxane, mixing the mixture with silicon dioxide and silicone resin; and the obtained antifoaming active matter has excellent defoaming speed and antifoaming performance in an anion and a nonionic foaming system. The addition of the silicon polyether effectively controls the degree of crosslinking and enhances affinity of the antifoaming active matter with water. The prepared antifoaming active matter can be applied to weaving printing and dyeing, pulping papermaking and sewerage treatment, etc.
Description
Technical field
The present invention relates to a kind of based on hydrogeneous polysiloxane and the reaction of vinyl polysiloxane; And introduce the preparation of the defoaming agent composition of polyether-modified polysiloxanes therein, said composition has excellent antifoaming performance in anion, nonionic foaming system.Defoaming agent composition belongs to fine chemicals, therefore, the invention belongs to technical field of fine chemical preparations.
Background technology
Foam is a common phenomena in the live and work.But foam can bring great harm sometimes in commercial production, for example reduce machine operating efficiency, incur loss through delay working time, influence the quality of product etc.The method of eliminating harmful foam mainly contains physical method and chemical method, and the antifoaming agent froth breaking is one of chemical method.Along with the significantly raising of industrial enterprise's production scale and production efficiency, the antifoaming agent froth breaking is more widely used.At present, antifoaming agent has been widely used in the industries such as papermaking, textile printing and dyeing, oil exploitation and refining, coating, emulsion polymerisation, sewage disposal, metal cleaning, and antifoaming agent has become indispensable functional aid in the production process.
According to the difference of froth breaking active matter, antifoaming agent is divided into mineral oil origin, polyether-type and several kinds of main types such as silicone based.Compare with other antifoaming agents, poly organo siloxane antifoaming agent stable chemical performance, side effect is little, and good froth breaking ability and the lasting bubble ability that presses down are also arranged under the very low situation of consumption simultaneously, thereby, favored very much.
The froth breaking active matter is the core of antifoaming agent, and its antifoaming speed and suds suppressing properties directly influence the performance of final products.For silicone based antifoaming agent, the improvement of the antifoaming performance of its active matter is the improvement direction of silicone defoaming agent.The most original polysiloxane defoamers active matter is handled through specific process technology by dimethyl silicone polymer and silica and is obtained, and the defoaming agent composition of introducing like US3383327 comes to this.But because it can not press down bubble lastingly, promptly suds suppressing properties is poor, and therefore, domestic and international research personnel have carried out large-scale expansion research to its performance.US4338217A1 replaces common polysiloxanes and silicon dioxide granule mixed processing to make the froth breaking active matter with the alkoxyl polysiloxanes; US5824739 introducing amino silicones or carboxyl polysiloxanes obtain defoaming composition as the main body of froth breaking active matter with the silica mixed processing; EP163541B1 introduces with the polysiloxanes that contains terminal hydroxyl and under the effect of catalyst, forms the side chain polysiloxane with the polysiloxane reaction that contains other active function groups; And replace common polysiloxanes and hydrophilic silicon dioxide mixed processing with this; Prepared defoamer formulations has very high viscosity, is difficult to this emulsification is dispersed in the water.US5153258 introduces and in system, introduces the antifoaming performance that lightly crosslinked polysiloxane can improve composition; For example contain vinyl polysiloxane and hydrogeneous polysiloxane, hydroxyl polysiloxane and alkyl silicate cross-linking reaction takes place under the effect of catalyst, but crosslinking degree is difficult to control.After having introduced the reaction of hydrogeneous polysiloxane and vinyl polysiloxane among the WO2007137948A1; The dimethyl silicone polymer dilution that adds the trimethylsiloxy group end-blocking; When hydrogeneous polysiloxane and vinyl polysiloxane react in the above-mentioned patent; Viscosity is big, and is wayward, and the defoaming agent composition antifoaming performance that obtains is poor.CN1931417A discloses a kind of defoaming agent composition of high temperature resistant anti-highly basic; It is obtained by polysiloxanes and organic siliconresin cross-linking reaction, and active matter is prepared into after the emulsion bubbling test performance in black liquor, and it has suds suppressing properties preferably; But antifoaming speed remains further to be improved; And, because froth breaking active matter viscosity is bigger, be dispersed in the water it quite difficult.
The silicone antifoam agent of EP-A341952 introduction use branching and the composition of polyether-polysiloxane copolymers are used for pulp production as antifoaming agent.US5523019 introduces the composition of mineral oil and polyether-polysiloxane copolymers as antifoaming agent, it is said to have positive effect.According to WO 98/000216, the siloxanes that contains dimethyl-3-hydroxypropyl-polyoxyethylene polyoxypropylene group is a specially suitable surfactant in the defoamer formulation.
The present invention reacts based on hydrogeneous polysiloxane and vinyl polysiloxane through a kind of; And introduce polyether-modified polysiloxanes therein; With silica, organic siliconresin mixed processing, the froth breaking active matter that obtains has good antifoaming speed and suds suppressing properties in anion, nonionic foaming system.Effectively control crosslinking degree after adding polyether-modified polysiloxanes, and increased the affinity of froth breaking active matter and water.The froth breaking active matter that obtains can be used for aspects such as textile printing and dyeing, pulping and paper-making, sewage disposal.
Summary of the invention
A kind of preparation of defoaming agent composition provides a kind of defoaming composition based on polysiloxanes; It is low to have viscosity; Be prone to disperse, in various systems, have very fast antifoaming speed and good characteristics such as suds suppressing properties, can be widely used in harmful foam of eliminating in the commercial production.
Technical scheme
A kind of defoaming agent composition is characterized in that it is made up of following material:
A. polysiloxane
The general structure of polysiloxane is following:
R
aSiO
(4-a)/2
Wherein the value of a is 1.9～2.2; R in the molecular structure can be identical or different, and replacement or the non-substituted carbon number that comprises hydrogen atom or monovalence is 1～20 alkyl, specifically comprises: methyl, ethyl, propyl group, n-pro-pyl, butyl, isobutyl group; Phenyl, benzyl, amino.The dynamic viscosity of this polysiloxane in the time of 25 ℃ is 50～10,000mPas.The consumption of polysiloxane is 40～75% of a defoaming agent composition gross mass.
B. hydrogeneous polysiloxane
At least a general structure is following hydrogeneous polysiloxane:
H
cR
1 3-cSiO(SiR
1HO)
d(SiR
1 2O)
bSiR
1 3-cH
c
Substituent R
1Identical or different, be the alkyl of carbon number 1～20, the concrete alkyl that comprises is like methyl, ethyl, propyl group, n-pro-pyl, butyl, isobutyl group; Aryl, like phenyl, benzyl, preferred substituent group R more than 80%
1It is methyl.Subscript c is 0,1 or 2, and subscript d is 0 or 1～200 integer, and c+d >=1, and subscript b is 1～1000 integer, and each molecule has at least 1 silicon bonded hydrogen atom, preferably at least 2 silicon bonded hydrogen atom.
The dynamic viscosity of described hydrogeneous polysiloxane in the time of 25 ℃ is 20～5, and 000mPas, the consumption of hydrogeneous polysiloxane are 10～30% of defoaming agent composition gross mass.
C. vinyl polysiloxane
At least a general structure is following hydrogen containing siloxane:
Vi
eR
2 3-eSiO(SiR
2ViO)
f(SiR
2 2O)
gSiR
2 3-eVi
e
Substituent R
2Identical or different, be the alkyl of carbon number 1～20, the concrete alkyl that comprises is like methyl, ethyl, propyl group, n-pro-pyl, butyl, isobutyl group; Aryl, like phenyl, benzyl, preferred substituent group R more than 80%
2It is methyl.Vi is a vinyl, and subscript e is 0 or 1, and subscript f is 0 or 1～200 integer, and e+f >=1, and subscript g is 1～600 integer, and each molecule has the vinyl groups of at least 1 silicon bonding, the vinyl groups of preferred at least 2 silicon bondings.
The dynamic viscosity of described vinyl polysiloxane in the time of 25 ℃ is 50～2, and 000mPas, the consumption of vinyl polysiloxane are 1～50% of defoaming agent composition gross mass.
D. silica
It is divided into two kinds of precipitated silica and fumed silicas by manufacturing approach, is divided into two kinds of hydrophilic silicon dioxide and hydrophobic silicas by surface nature.The present invention is preferably hydrophobic silica, comprises vapor phase method hydrophobic silica and precipitation method hydrophobic silica, and its specific area is 50～500m
2/ g.The consumption of silica is 1～5% of a defoaming agent composition gross mass.
E. organic siliconresin
Organic siliconresin refers to the cancellated polysiloxane in highly cross-linked space; This cancellated polysiloxane is normally by various mixtures hydrolysis in organic solvent such as toluene of methyl trichlorosilane, dimethyldichlorosilane, phenyl trichlorosilane, diphenyl dichlorosilane or dichloromethyl phenylsilane; Obtain the acidic hydrolysis thing; Remove disacidify through washing then, obtain product.The organic siliconresin that the present invention uses is by chain link CH
3SiO
1/2(being called the M unit in the organosilicon chemistry) and chain link SiO
4/2The MQ resin that the unit of (Q unit) is formed, the mol ratio between the two is (0.4～1.2): 1.0, preferred (0.5～0.8): 1.0.The consumption of organic siliconresin is 2～10% of a defoaming agent composition gross mass.
F. catalyst
Catalyst is used for hydrogeneous polysiloxane of catalyst component and vinyl polysiloxane polymerization reaction take place.Catalyst is selected from platinum-alcohol complex, platinum-alkene complex, platinum-alkoxide complexes, platinum-ether complexes, platinum-ketone complex compound, isopropyl alcohol solution of chloroplatinic acid, platinum-vinyl complex compound.Said catalyst consumption is 0.01～0.05% of a defoaming agent composition gross mass.
G, polyether-modified polysiloxanes
Take place under the effect of catalyst by hydrogen containing siloxane and the polyethers that contains unsaturated bond that addition reaction prepares.The said polyether-modified polysiloxanes preferably average viscosity under 25 ℃ is 10～30, and 000mPas is preferably at 25 ℃ and descends 60～5,000mPas.The structural formula of polyether-modified polysiloxanes is following:
MD
x(CH
3GSiO)
yM
Wherein, M is identical with M unit in the organic siliconresin, is chain link CH
3SiO
1/2, D is chain link CH
2SiO
2/2G is a polyether group, representes with following general structure :-(CH
2)
zO (EO)
h(PO)
iR
3, R
3For the replacement of hydrogen atom, carboxyl, methoxyl group or monovalence or non-substituted carbon number are 1～4 alkyl, comprise methyl, ethyl, propyl group, butyl, EO is an oxirane, PO is an expoxy propane; Above-mentioned each structural formula subscript x, y, z, h, i are the degree of polymerization, x is 10～500 integer; Y is 1～50 integer; Z is 2～6 integer; H is 1～36 integer; I is 0～50 integer.The consumption of polyether-modified polysiloxanes is 1～10% of a defoaming agent composition gross mass.
The preparation method of defoaming agent composition according to the invention is following:
1. polysiloxane, hydrogeneous polysiloxane, vinyl polysiloxane, polyether-modified polysiloxanes and/or hydrophobic silica are mixed in beaker, and heating, in the time of 40～140 ℃, add acidic catalyst, reaction 0.5～5h;
2. after reaction finishes, add organic siliconresin, and/or hydrophobic silica, and at 60～150 ℃ of reaction 1～5h;
3. after reaction finishes, with mixture-0.01～-keep 0.1～1.5h under the 0.08MPa vacuum, last cool to room temperature promptly gets defoaming agent composition.
The specific embodiment
Embodiment 1
In the 1000mL beaker, dropping into 200g viscosity is the dimethyl silicone polymer of the trimethylsiloxy group end-blocking of 100mPas, and 100g viscosity is hydrogeneous gathering of the side chain of 20mPas radical siloxane Me to be arranged
3SiO (MeHSiO)
2(Me
2SiO)
20SiMe
3, 60g viscosity is the bi-vinyl end-blocking polysiloxane ViMe of 150mPas
2SiO (Me
2SiO)
135SiMe
2The polyether-modified polysiloxanes of Vi and 36g (x=100, y=20, z=3, h=20, i=40, R
3=-H).Heat temperature raising adds the 0.096g isopropyl alcohol solution of chloroplatinic acid in the time of 60 ℃, insulation 0.5h; Adding the 18g specific area then is 200m
2The vapor phase method hydrophobic silica of/g and 18gMQ resin (M: Q=0.75: 1); System is warming up to 120 ℃, and after keeping 4h under this temperature, under the vacuum of-0.03MPa, keeps 0.5h; It is 7 that cool to room temperature obtains viscosity, the defoaming agent composition of 000mPas.
Embodiment 2
In the 1000mL beaker, dropping into 200g viscosity is 1, the dimethyl silicone polymer of the phenyl dimethylsilyl bis end-blocking of 000mPas, and 100g viscosity is the hydrogeneous dimethyl silicone polymer Me of 100mPas side chain
3SiO (MeHSiO)
3(Me
2SiO)
69SiMe
3, 78g viscosity is the bi-vinyl end-blocking polysiloxane ViMe of 600mPas
2SiO (Me
2SiO)
380SiMe
2The polyether-modified polysiloxanes of Vi and 15g (x=50, y=8, z=3, h=14, i=8, R
3=-CH
3).Heat temperature raising adds the 0.1g isopropyl alcohol solution of chloroplatinic acid in the time of 100 ℃, insulation 0.25h; Adding the 15g specific area then is 150m
2The vapor phase method hydrophobic silica of/g and 38g MQ resin (M: Q=0.65: 1); System is warming up to 140 ℃, and after keeping 3h under this temperature, under the vacuum of-0.03MPa, keeps 0.5h; It is 10 that cool to room temperature obtains viscosity, the defoaming agent composition of 000mPas.
Embodiment 3
In the 1000mL beaker, dropping into 200g viscosity is 1, the dimethyl silicone polymer of the amino dimethylsilyl bis end-blocking of 000mPas, and 100g viscosity is the hydrogeneous dimethyl silicone polymer Me of 1500mPas side chain
3SiO (MeHSiO)
36(Me
2SiO)
500SiMe
3, 38g viscosity is the bi-vinyl end-blocking polysiloxane ViMe of 1000mPas
2SiO (Me
2SiO)
450SiMe
2The polyether-modified polysiloxanes of Vi and 15g (x=150, y=10, z=3, h=20, i=7, R
3=-CH
3).Heat temperature raising adds the 0.1g isopropyl alcohol solution of chloroplatinic acid in the time of 50 ℃, insulation 2h; Adding the 15g specific area then is 90m
2(M: Q=065: 1), system is warming up to 90 ℃, and after keeping 3h under this temperature, under the vacuum of-0.06MPa, keeps 1h, and it is 12 that cool to room temperature obtains viscosity, the defoaming agent composition of 600mPas for the precipitation method hydrophobic silica of/g and 17g MQ resin.
Embodiment 4
In the 1000mL beaker, dropping into 200g viscosity is the dimethyl silicone polymer of the trimethylsiloxy group end-blocking of 50mPas, and 100g viscosity is the hydrogeneous dimethyl silicone polymer Me of 800mPas side chain
3SiO (MeHSiO)
18(Me
2SiO)
150SiMe
3, 315g viscosity is that the side chain of 100mPas contains vinyl polysiloxane Me
3SiO (ViMeSiO)
2(Me
2SiO)
70SiMe
3, the 30g specific area is 90m
2The precipitation method hydrophobic silica of/g and the polyether-modified polysiloxanes of 15g (x=70, y=5, z=3, h=35, i=0, R
4=-CH
2CH
3).Heat temperature raising adds the 0.3g isopropyl alcohol solution of chloroplatinic acid in the time of 80 ℃, insulation 0.5h; 1), and after keeping 3h under this temperature (M: Q=0.58:, under the vacuum of-0.06MPa, keep 1h, it is 6 that cool to room temperature obtains viscosity, the defoaming agent composition of 500mPas to add 18g MQ resin then.
Embodiment 5
In the 1000mL beaker, dropping into 460g viscosity is 10, the dimethyl silicone polymer of the amino dimethylsilyl bis end-blocking of 000mPas, and 100g viscosity is that the two hydrogen end-blockings of 30mPas gather organic hydrogen-containing siloxane HMe
2SiO (Me
2SiO)
16SiMe
2H, 15g viscosity is that the side chain of 300mPas contains vinyl polysiloxane Me
3SiO (ViMeSiO)
2(Me
2SiO)
220SiMe
3, the 23g specific area is 380m
2The vapor phase method hydrophobic silica of/g and the polyether-modified polysiloxanes of 12g (x=100, y=40, z=3, h=1, i=50, R
3=-H).Heat temperature raising adds the 0.08g isopropyl alcohol solution of chloroplatinic acid in the time of 120 ℃, insulation 0.5h; (M: Q=0.8: 1), be warming up to 150 ℃, after keeping 3h under this temperature, under the vacuum of-0.06MPa, keep 1.5h, it is 35 that cool to room temperature obtains viscosity, the defoaming agent composition of 000mPas to add 45g MQ resin then.
Embodiment 6
In the 1000mL beaker, dropping into 640g viscosity is the dimethyl silicone polymer of the trimethylsiloxy group end-blocking of 1000mPas, and 100g viscosity is that the two hydrogen end-blockings of 50mPas gather organic hydrogen-containing siloxane HMe
2SiO (Me
2SiO)
66SiMe
2H, 28g viscosity is the bi-vinyl end-blocking polysiloxane ViMe of 2000mPas
2SiO (Me
2SiO)
510SiMe
2Vi, the 23g specific area is 110m
2The precipitation method hydrophobic silica of/g and the polyether-modified polysiloxanes of 38g (x=150, y=40, z=3, h=4, i=6, R
4=-COCH
3).Heat temperature raising adds the 0.13g isopropyl alcohol solution of chloroplatinic acid in the time of 130 ℃, insulation 3h; 1), and after keeping 5h under this temperature (M: Q=0.65:, under the vacuum of-0.08MPa, keep 1h, it is 9 that cool to room temperature obtains viscosity, the defoaming agent composition of 500mPas to add 38g MQ resin then.
Comparative Examples 1
In the 1000mL beaker, dropping into 200g viscosity is 1, the dimethyl silicone polymer of the amino dimethylsilyl bis end-blocking of 000mPas, and 100g viscosity is the hydrogeneous dimethyl silicone polymer Me of 1500mPas side chain
3SiO (MeHSiO)
36(Me
2SiO)
500SiMe
3With 38g viscosity be the bi-vinyl end-blocking polysiloxane ViMe of 1000mPas
2SiO (Me
2SiO)
450SiMe
2Vi.Heat temperature raising adds the 0.1g isopropyl alcohol solution of chloroplatinic acid in the time of 50 ℃, insulation 2h; Adding the 15g specific area then is 90m
2The precipitation method hydrophobic silica of/g and 17g MQ resin (M: Q=0.65: 1); System is warming up to 90 ℃, and after keeping 3h under this temperature, under the vacuum of-0.06MPa, keeps 1h; It is 482 that cool to room temperature obtains viscosity, the defoaming agent composition of 600mPas.
Comparative Examples 2
In the 1000mL beaker, dropping into 200g viscosity is the dimethyl silicone polymer of the trimethylsiloxy group end-blocking of 50mPas, and 100g viscosity is the hydrogeneous dimethyl silicone polymer Me of 800mPas side chain
3SiO (MeHSiO)
18(Me
2SiO)
350SiMe
3, 315g viscosity is that the side chain of 100mPas contains vinyl polysiloxane Me
3SiO (ViMeSiO)
2(Me
2SiO)
70SiMe
3, the 30g specific area is 90m
2The precipitation method hydrophobic silica of/g.Heat temperature raising adds the 0.3g isopropyl alcohol solution of chloroplatinic acid in the time of 80 ℃, insulation 0.5h; 1), and after keeping 3h under this temperature (M: Q=0.58:, under the vacuum of-0.06MPa, keep 1h, it is 262 that cool to room temperature obtains viscosity, the defoaming agent composition of 500mPas to add 18g MQ resin then.
The defoaming agent composition performance test
Method of testing: the sodium dodecyl benzene sulfonate aqueous solution with 0.5% (mass percent) is the foaming medium; The above-mentioned foaming medium of addition 50mL in the 100mL tool plug graduated cylinder; The defoaming agent composition that adds 0.010g then; Leave standstill behind the shake 50 times in vertical direction, the record foam disappears to the liquid level time occurring, is foam time T
50, shake writes down foam time T 50 times again
100, every jolting is just write down foam time 50 times, reaches till 400 times until always shaking a bottle number of times, and under the identical jolting number of times, foam time is short more, and it is good more to represent that disappearing of defoaming agent composition pressed down the bubble effect.Test result is seen table 1:
The antifoam performance contrast of table 1 defoaming agent composition
| Foam time/s | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Comparative Examples 1 | Comparative Examples 2 |
| T 50 | 5 | 4 | 2 | 3 | 6 | 3 | 5 | 5 |
| T 100 | 5 | 4 | 2 | 4 | 5 | 3 | 10 | 5 |
| T 150 | 6 | 4 | 3 | 4 | 6 | 4 | 11 | 7 |
| T 200 | 7 | 5 | 3 | 4 | 6 | 3 | 19 | 10 |
| T 250 | 8 | 4 | 4 | 3 | 7 | 3 | - | 14 |
| T 300 | 7 | 6 | 5 | 4 | 8 | 4 | - | 16 |
| T 350 | 9 | 6 | 5 | 6 | 9 | 6 | - | 19 |
| T 400 | 10 | 7 | 5 | 5 | 9 | 6 | - | 21 |
Can find out that from last table result the antifoam performance of the defoaming agent composition of embodiment 1～6 is superior to Comparative Examples, this explains that defoaming agent composition of the present invention has stronger froth breaking ability in the anion system.And the defoaming agent composition viscosity that the present invention obtains is obviously little than resulting defoaming agent composition in the Comparative Examples, and the defoaming agent composition viscosity that Comparative Examples obtains is very big, is difficult to emulsification and disperses.
Claims (4)
1. defoaming agent composition and preparation method thereof is characterized in that, described defoaming agent composition is composed of the following components:
(1) polysiloxane, general structure is: R
aSiO
(4-a)/2, wherein the value of a is 1.9～2.2, R is that replacement or the non-substituted carbon number of hydrogen atom or monovalence is 1～20 alkyl, can be identical or different; The dynamic viscosity of said polysiloxane in the time of 25 ℃ is 50～10, and 000mPas, consumption are 40～75% of defoaming agent composition gross mass;
(2) hydrogeneous polysiloxane comprises a kind of following general structure at least:
H
cR
1 3-cSiO(SiR
1HO)
d(SiR
1 2O)
bSiR
1 3-cH
c
Wherein, R
1For the alkyl of carbon number 1～20, identical or different, methyl preferably; Subscript c is 0,1 or 2, and subscript d is 0 or 1～200 integer, and c+d>=1, and subscript b is 1～1000 integer, and each molecule has at least 1 silicon bonded hydrogen atom, preferably at least 2 silicon bonded hydrogen atom; The dynamic viscosity of described hydrogeneous polysiloxane in the time of 25 ℃ is 20～5, and 000mPas, consumption are 10～30% of defoaming agent composition gross mass;
(3) vinyl polysiloxane comprises a kind of following general structure at least:
Vi
eR
2 3-eSiO(SiR
2ViO)
f(SiR
2 2O)
gSiR
2 3-eVi
e
R wherein
2Span and R
1Identical; Vi is a vinyl, and subscript e is 0 or 1, and subscript f is 0 or 1～200 integer, and e+f>=1, and subscript g is 1～600 integer, and each molecule has the vinyl groups of at least 1 silicon bonding, the vinyl groups of preferred at least 2 silicon bondings; The dynamic viscosity of described vinyl polysiloxane in the time of 25 ℃ is 50～2, and 000mPas, consumption are 1%～50% of defoaming agent composition gross mass;
(4) silica, consumption are 1～5% of defoaming agent composition gross mass;
(5) organic siliconresin is for by chain link CH
3SiO
1/2With chain link SiO
4/2The organic siliconresin of forming, the mol ratio between the two is (0.4～1.2): 1.0, consumption is 2～10% of a defoaming agent composition gross mass;
(6) catalyst is selected from platinum-alcohol complex, platinum-alkene complex, platinum-alkoxide complexes, platinum-ether complexes, platinum-ketone complex compound, isopropyl alcohol solution of chloroplatinic acid, platinum-vinyl complex compound, and consumption is 0.01～0.05% of a defoaming agent composition gross mass;
(7) polyether-modified polysiloxanes, structural formula is: MD
x(CH
3GSiO)
yM, wherein, M chain link CH
3SiO
1/2, D is chain link CH
2SiO
2/2G is a polyether group, representes with following general structure :-(CH
2)
zO (EO)
h(PO)
iR
3, R
3For the replacement of hydrogen atom, carboxyl, methoxyl group or monovalence or non-substituted carbon number are 1～4 alkyl, EO is an oxirane, and PO is an expoxy propane; Subscript x, y, z, h, i are the degree of polymerization, x is 10～500 integer; Y is 1～50 integer; Z is 2～6 integer; H is 1～36 integer; I is 0～50 integer; Average viscosity under 25 ℃ is 10～30, and 000mPas, consumption are 1～10% of defoaming agent composition gross mass;
The preparation method is following:
1. with polysiloxane, hydrogeneous polysiloxane, vinyl polysiloxane, polyether-modified polysiloxanes and/
Or silica mixes in beaker, and heating, in the time of 40～140 ℃, adds acidic catalyst, reaction 0.5～5h;
2. after reaction finishes, add organic siliconresin, and/or silica, and at 60～150 ℃ of reaction 1～5h;
3. after reaction finishes, with mixture-0.01～-keep 0.1～1.5h under the 0.08MPa vacuum, last cool to room temperature promptly gets defoaming agent composition.
2. a kind of defoaming agent composition according to claim 1 and preparation method thereof, wherein (4) described silica is hydrophobic silica, its specific area is 50～500m
2/ g.
3. a kind of defoaming agent composition according to claim 1 and preparation method thereof, wherein chain link CH in (5) described organic siliconresin
3SiO
1/2With chain link SiO
4/2Mol ratio is preferably (0.5～0.8): 1.0.
4. a kind of defoaming agent composition according to claim 1 and preparation method thereof, wherein (7) described polyether-modified polysiloxanes is preferably 60～5,000mPas at 25 ℃ of following average viscosities.
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| CN102698475A (en) * | 2012-06-29 | 2012-10-03 | 南京四新科技应用研究所有限公司 | Defoaming composition |
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| CN107115694B (en) * | 2016-08-31 | 2019-11-08 | 江苏四新科技应用研究所股份有限公司 | A kind of silicon composition and its preparation, application |
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