CN104274998B

CN104274998B - A kind of silicon composition, preparation method and application

Info

Publication number: CN104274998B
Application number: CN201310290304.1A
Authority: CN
Inventors: 吴飞; 池跃芹; 曹添; 杨有忠; 章强; 黄伟
Original assignee: Jiangsu Sixin Scientific-Technological Application Research Institute Co Ltd
Current assignee: Jiangsu Sixin Scientific-Technological Application Research Institute Co Ltd
Priority date: 2013-07-11
Filing date: 2013-07-11
Publication date: 2016-12-28
Anticipated expiration: 2033-07-11
Also published as: WO2015003407A1; CN104274998A; CL2015000712A1

Abstract

The present invention relates to a kind of based on adding a kind of cross-linking agent containing active group after hydrogeneous polysiloxane and organic siliconresin, unsaturated hydrocarbons generation additive reaction, the polymer of cross-linked structure that silicon dioxide obtains through processing, antifoam performance improves, suds effect is good, ease handling and processing, the addition of emulsifying agent will not cut down its suds effect that disappears.Its suds suppressing properties is good, unattenuated, and the polymer formed is prone to processed.

Description

A kind of silicon composition, preparation method and application

Technical field

The present invention relates to technical field of fine chemical preparations, be specifically related to a kind of silicon composition, preparation method and Application in terms of preparing solid defoaming agent or defoamer.

Background technology

Foam is phenomenon common in live and work.Such as at food processing, textile dyeing, paper production, sewage Process and clean in the many Aquo Systems used in occasion, need to control or prevent the generation of foam.Specifically, when certainly When dynamic washing machine, roller washing machine wash, being formed under acceptable level of foam need to be kept.Too much foam will Cause cleaning mixture in floor overflow and the efficiency of reduction washing operation itself.In detergent industry, it is intended to use more High efficiency composition of detergent.Increase surface-active contents, use has the distribution of higher foam than conventional surfactants Surfactant can cause more foam.It is thus desirable to exploitation addition is few and more effective Sudo controlling compositions adds In composition of detergent.

Silicon composition is the core of defoamer, and its antifoaming speed and suds suppressing properties directly affect the property of final products Energy.For the defoamer of silicone, the improvement of the antifoaming performance of its active matter is the improvement side of organic silicon defoamer To.The most original polysiloxane defoaming agent active matter is through specific process technology by polydimethylsiloxane and silicon dioxide Reason obtains, and the defoaming agent composition introduced such as US3383327 is exactly such, but due to its can not lasting suds, i.e. Suds suppressing properties is poor.Therefore, research worker both domestic and external has all carried out large-scale expansion research to its performance.With chain alkyl it is The polysiloxane synthesis defoamer of side chain is highly effective in detergent, and such as EP-A-1075683 discloses one Planting foam controller, it includes that (A) has the organopolysiloxane material of the substituent group of at least one silicon bonding of molecular formula X-Ph Material, wherein X represents that divalent aliphatic alkyl and Ph represent aryl, (B) water-insoluble organic liquid, and (C) organic siliconresin and (D) dredge Water packing.Water-insoluble organic liquid (B) can be mineral oil, liquid polyisobutene, isoparaffinic oil or vegetable oil.EP- A-1075684 discloses the foam controller of a kind of similar composition.Except that it does not contains water-insoluble organic liquid (B).EP-A-578424 discloses a kind of foam controller, and it contains the polydiorganosiloxanepolyurea of the side chain of band alkyl, described In alkyl side chain, each alkyl side chain contains 9～35 carbon atoms.Polydiorganosiloxanepolyurea is with fine hydrophobic granular material such as Hydrophobic silica and optional MQ organic siliconresin are used together.EP-A-1076526 discloses and comprises additionally in stabilization aid Such a Sudo controlling compositions, described stabilization aid be fusing point be the organic compound of 40～80 DEG C, preferred fatty acid, fat Fat alcohol or alkyl phosphate.US005486306A, CN1674967A, CN101048212A, WO2012/075962A1 disclose one Plant the foam controller of similar composition.Except that CN1674967A contains fusing point 35～100 DEG C of non-polar organic material. In CN101048212A, the carbon atom average of whole group R is 3～6.Containing fusing point 45～100 DEG C in WO2012/075962A The outer organic polymer possibly together with static electrification lotus of organic material.Mention in above patent is all the polymerizable organosilicon not cross-linked Thing, is effective defoamer at composition of detergent, but this compositions suds suppressing properties is poor, and adding emulsifying agent can be greatly Reduce its antifoaming performance, easily decay, defoaming as the intervention of surfactant and significantly weaken, and table in detergent Face activating agent is indispensable component.Improving silicon composition viscosity is to solve the effective ways of this problem, such as EP- Described in A301531, it is said that use has been elastomeric partial cross-linked polydimethylsiloxane Being favorably improved the effect of defoamer, suds is good, adds emulsifying agent and is difficult to reduce its antifoaming performance, can join about this point As usual such as US-2,632,736, EP-A-273448 and EP-A434060, these products have the highest viscosity, but also because Branched or the crosslinking degree that reaches is higher makes its difficulties in dispersion in system, is difficult to process further or processing.

Additionally, as solid defoaming agent in addition to should possessing as the corresponding performance requirement of antifoam additives, the compatibility and Froth breaking stability is also one of very important index.Use the low viscous silicone grease of substantial amounts of emulsifier can make emulsion grain Footpath controls about 20 μm, and the compatibility is preferable, but such defoamer defoaming effect is the most undesirable, and suds suppressing properties is worse；For Reach more preferable froth breaking, suds effect, be necessary for the high viscosity crosslinking silicone grease using suds effect higher, but this silicone grease is only Rely on a small amount of emulsifier difficulty, disperse uneven, can not uniform adsorption when can cause carrier adsorption silicone grease；Emulsifying dosage is big Aridity, hardness, adsorbance and the antifoaming performance of solid defoaming agent self can be affected again；How to make self shape of solid defoaming agent State is unaffected, takes into account again the defoaming of defoamer, is also a lot of expert and scholar's concern.

Summary of the invention

The present invention relates to a kind of based on hydrogeneous polysiloxane and organic siliconresin, unsaturated hydrocarbons generation additive reaction after Add a kind of cross-linking agent containing active group and the organosilicon of cross-linked structure that silicon dioxide obtains through processing Compositions, can be used for the foam control composition in commercial production.

The present invention also provides for a kind of solid defoaming agent using silicon composition of the present invention to prepare, and this solid The preparation method of defoamer, is consolidated by the silicone active thing prepared by silicon composition of the present invention is finally prepared Body defoamer, decreases silicone grease and is difficult to problem pockety in emulsion dispersion, agglomeration to carrier, it is ensured that disappearing of defoamer Bubble property and the compatibility so that whole cleaning process can fully froth breaking and suds.

For solving the problem of above-mentioned prior art existence and reaching the purpose of the present invention, the technical solution used in the present invention For: a kind of silicon composition, it is characterised in that its raw material and each raw material account for silicon composition gross mass percentage ratio and be:

The most hydrogeneous polysiloxane 45 ~ 75%

The hydrogeneous polysiloxane that at least one formula is following:

H_cR⁰ _3-cSiO (R⁰HSiO)_d (R⁰ ₂SiO)_bSiR⁰ _3-cH_c

Wherein, substituent R⁰Identical or different, for the alkyl of carbon number 1～20, concrete includes alkyl, as methyl, Ethyl, n-pro-pyl, normal-butyl, isobutyl group, n-pentyl, cyclopenta, n-hexyl, n-heptyl, n-octyl, iso-octyl, n-nonyl, just Decyl, dodecyl and n-octadecane base；Aryl, such as phenyl, benzyl, the substituted radical R of preferably more than 80%⁰It it is methyl. SubscriptcIt is 0,1 or 2, subscriptdIt is the integer of 0 or 1 ~ 200, the integer of preferably 10 ~ 180, the integer of most preferably 40 ~ 160, Andc+d>=1, subscriptbIt is the integer of 1 ~ 1000, the integer of preferably 50 ~ 800, the integer of most preferably 100 ~ 500, Mei Gefen Son has the hydrogen atom of at least 1 silicon bonding, the hydrogen atom of preferably at least 2 silicon bondings.Hydrogeneous polysiloxane preferentially selects Select the hydrogeneous polysiloxane of the hydrogeneous polysiloxane of side chain and side；

B. cross-linking agent 0.1 ~ 5%

Described cross-linking agent is the following polysiloxanes of at least one structural formula: wherein R¹Identical or different, it is 1 for carbon number Alkyl, hydrogen atom or the vinyl of ~ 10；R²Identical or different, for alkyl, hydrogen atom or vinyl, R that carbon number is 1 ~ 10² Base is preferably methyl；SubscriptmIt is the integer of 0 ~ 50, the integer of preferably 5 ~ 40, the integer of most preferably 10 ~ 30；nIt is 0 ~ 5 Integer, the integer of preferably 1 ~ 3；S is the integer of 0 ~ 30, the integer of preferably 2 ~ 25, the integer of most preferably 5 ~ 20.Each point Son has hydrogen atom or the vinyl of at least 1 silicon bonding, the hydrogen atom of preferably at least 2 silicon bondings or vinyl；

Or formula is (R³HSiO)_fRing-type hydrogeneous polysiloxane, R³For the alkyl of carbon number 1 ~ 10, such as methyl , ethyl, propyl group, n-pro-pyl, butyl, isobutyl group,fIt it is the integer of 3 ~ 6；

Or formula is [CH₂=CH(Me)SiO]_gCyclic vinyl polysiloxane, Me is methyl,gIt it is the integer of 3 ~ 5；

Above cross-linking agent prioritizing selection: the hydrogeneous or vinyl polysiloxane of (1) straight chain, or vinyl hydrogeneous with side chain is Main；(2) ring-type hydrogeneous polysiloxane and vinyl polysiloxane,fWithgMain value is all 4 and 5；R³Mainly Select methyl and ethyl；

C. organic siliconresin 1 ~ 10%

The conventional organic siliconresin that organic siliconresin is a kind of space structure, preferred silicone-containing unit R_aSiO_4-a/2, wherein R is hydroxyl, alkyl or oxyl, and a is 0.5 ~ 2.4；The more preferably R Han M functional group^* ₃SiO_1/2With Q official SiO can be rolled into a ball_4/2, wherein R^*For univalence hydrocarbyl, the mol ratio of M:Q is (0.4 ~ 1.2): 1.0, is preferably (0.5 ~ 0.8): 1.0.? Preferably organic siliconresin is only made up of M unit as defined above and Q unit but it also may uses and comprises M unit, trivalent R^* SiO_3/2(T) unit and the resin of Q unit.Organic siliconresin can also contain divalent unit R^*SiO_2/2, preferably it is less than institute Have existence siloxane unit 20%.Group R(and R^*) preferably there is the alkyl of 1 ~ 6 carbon atom, the most substantially institute There is R(and R of existence^*) base is methyl.Also other alkyl can be there is, such as with having that dimethylvinylsilyl exists The alkenyl of 1 ~ 6 carbon atom, it is also possible to there is the hydroxyl and/or alkoxyl being bonded with silicon, such as methoxyl group.Such as can pass through Hydrolyze some silane material, in a solvent or produced in situ.Particularly preferably at solvent, such as, in the presence of dimethylbenzene, make tetravalence Siloxy groups, such as four ortho-silicates, tetraethylorthosilicise, poly-ethyl silicate or the precursor of sodium silicate and monovalence Trialkylsiloxy unit, such as, trim,ethylchlorosilane, trimethylethoxysilane, hexamethyl disiloxane or pregnancy The precursor hydrolysis of base disilazane is also condensed.If it is required, gained MQ resin can further trimethylsilylation with reaction Fall the Si-OH base of residual, maybe can heat it in the presence of base to make resin self condense by elimination Si-OH base；

D. unsaturated hydrocarbons 10 ~ 50%

Including alkene and alkynes, described alkene is the alpha-olefin of straight chain, alicyclic olefin, aromatic olefin or branching type The mixing of any one or more in alkene；Described alkynes is in acetylene, propine, butine, pentyne, hexin, heptyne, octyne The mixing of any one or more；

E. catalyst 0.01 ~ 0.2%

Described catalyst is used for the hydrogeneous polysiloxane of catalyst component and organic siliconresin, alkene occur polymerization anti- Should.Described catalyst is selected from platinum-ol complex, platinum-alkene complex, platinum-ol salt complex, platinum-ether complexes, platinum-one Complex, isopropyl alcohol solution of chloroplatinic acid or platinum-vinyl complex.The platinum content of described catalyst is 1 ~ 20ppm, preferably chlorine Platinic acid aqueous isopropanol；

F. silicon dioxide 2 ~ 6%

Silicon dioxide is divided into precipitated silica and fumed silica two kinds by manufacture method, divides by surface nature For hydrophilic silicon dioxide and hydrophobic silica two kinds.The present invention is preferably hydrophobic silica, and specific surface area is 50 ~ 500m²/ G, including vapor phase method hydrophobic silica and sedimentation method hydrophobic silica.By using methyl substituted organosilicon material to carry out Hydrophobization processes.Suitably water-repelling agent includes polydimethylsiloxane, silanol or the alkoxy end-capped dimethyl being bonded with silicon Siloxane polymer, hexamethyldisiloxane and hexamethyl disiloxane.At at least 80 DEG C, generally carry out hydrophobization process.

The hydrogeneous polysiloxane described in the A dynamic viscosity when 25 DEG C is 10 ~ 2000mPa s further, is preferably 100 ~ 1500 mPa s, the dynamic viscosity when 25 DEG C of the cross-linking agent described in B is 5 ~ 50 mPa s, preferably 10 ~ 40 mPa s.

The alpha-olefin of the straight chain described in D is α-hexene, α-octene, α-decene, α-laurylene, α-ten four further Alkene, α-hexadecylene, α-octadecylene, α-icosa alkene, the α-C20 ~ mixture of C24 alkene, the α-C24 ~ mixture of C28 alkene, α- 30 alkene；Described alicyclic olefin is pinene, camphene, dipentene, cyclopentenes, norborene；Described aromatic olefin be α- Methyl styrene or styrene；Described ramiform aliphatic group: such as iso-amylene, isooctene.Preferred unsaturated olefin is: The mixing of any one or more in the alpha-olefin of the straight chain of below C24, camphene or α-methyl styrene.

The preparation method of a kind of described silicon composition, specifically comprises the following steps that

1. hydrogeneous polysiloxane A and organic siliconresin C, unsaturated hydrocarbons D are joined in reaction vessel, be warming up to 50 ~ 80 DEG C, it is incubated 0.2～5h, makes organic siliconresin dissolve；

2. add catalyst E, after 100 ~ 200 DEG C of reaction 1 ~ 3h, add crosslinking agent B and silicon dioxide F, at 150 ~ 200 DEG C

Insulation 0.5 ~ 5h, forms the polymer of crosslinking；

3. after insulation terminates, and under-0.01 ~-0.08MPa vacuum, 0.1～1.5h is maintained；Finally, it is cooled to room Temperature i.e. obtains

The cross-linked silicone compositions of thickness, viscosity is 20,000 ~ 100,000mPa s.

The application in preparing silicone active thing of the described silicon composition.

Silicone active thing prepared by a kind of described silicon composition, its raw material and each raw material account for organosilicon active matter The percentage ratio of gross mass is:

I. silicon composition 35 ~ 65% of the present invention；

II. emulsifying agent, for nonionic surfactant 5 ~ 35%；

III. structural agent 9～50%；

Wherein, described emulsifying agent is nonionic surfactant, including NPE, octyl phenol polyoxyethylene Ether, lauric acid polyoxyethylene ether, oleic acid polyoxyethylene, polyoxyethylene lauryl ether, hexadecanol polyoxyethylene ether, octadecanol are poly- Oxygen vinyl Ether, sorbitan mono-laurate, sorbitan monopalmitate, sorbitan monostearate, dehydration Sorbitol monooleate, anhydrous sorbitol tristearate, sorbitan trioleate, anhydrous sorbitol monostearate polyoxy Ethylene ether-ether, anhydrous sorbitol list oleic acid polyoxyethylene ester, anhydrous sorbitol three stearic acid polyoxyethylene ether ester, Oleum Ricini are poly- Oxygen vinyl Ether and the like, is used alone or is used in mixed way；

Described structural agent is acrylic polymer, cellulose ether, citric acid or citric acid salt or polyvinyl pyrrole The mixing of any one or more in alkanone.

The most described acrylic polymer is polyacrylic acid or its partial sodium salt, maleic acrylic copolymer； Described cellulose ether refers to water miscible or water swellable cellulose ether, such as sodium carboxymethyl cellulose；Described citric acid or lemon Lemon Barbiturates is sodium citrate, potassium citrate；These structural agents can be used alone, it is also possible to arbitrary proportion is used in mixed way.

The preparation method of a kind of described silicone active thing: by the silicon composition of formula ratio, emulsifying agent and structural agent It is mixed directly, loads in container after colloid mill homogenizes 0.1 ~ 0.5h, the abundant mixing of warming while stirring to 80 DEG C 0.5 ~ 2h, obtaining viscosity is 1000 ~ 10, the silicone active thing of 000mPa s.

Viscosity of the present invention is that the silicon composition of 20,000 ~ 100,000mPa s is in the mistake preparing silicone active thing Cheng Zhong, used colloid mill to homogenize process, decreased the usage amount of emulsifying agent, can control particle diameter about 20 μm simultaneously；? In Homogenization, silicone active thing is after Strong shear, and viscosity is reduced, and is reduced to: 1000 ~ 10,000mPa s； Make it easy to mix with carrier, it is ensured that the compatibility of silicone active thing and antifoaming performance.

Solid defoaming agent prepared by a kind of described silicone active thing, its raw material and each raw material account for solid defoaming agent gross mass Percentage ratio be:

Silicone active thing 18 ~ 45% of the present invention；

Carrier 50 ~ 75%；

Solvent 2 ~ 10%；

Wherein, described carrier is selected from sulfate, carbonate, phosphate, Quadrafos, starch, cellulose or aluminosilicate In the mixing of any one or more, be solid under these carrier room temperatures, preferably starch, particle diameter are more than the sulphuric acid of 300 mesh Salt or carbonate；

Described solvent is the solvent being easy to remove in dry run, and their evaporation can be internally formed at solid particle Hole, adds the specific surface area of solid particle, and specifically, solvent is any one or more in alcohols material or water Mixing, preferably methanol, ethanol, isopropanol, more preferably ethanol or water.

The preparation method of a kind of described solid defoaming agent, concrete operation step is as follows: first by the organosilicon of formula ratio Active matter and carrier join in blender, are added thereto to the solvent mixing of formula ratio after stirring, and pelletize is dried.

The present invention relates to one add again based on after hydrogeneous polysiloxane and organic siliconresin, alkene generation additive reaction Enter cross-linking agent, the polymer of cross-linked structure that silicon dioxide obtains through processing, antifoam performance improves, suds effect Good, it is easy to processing and process, the addition of emulsifying agent will not cut down its suds effect that disappears.Its principle is to utilize to have low viscosity and contain The polysiloxane of active group, this polyorganosiloxane has the highest reactivity, the functional group's energy on its chain link Reacting to each other with Si-H, form new chemical bond, Linear Polymer structure is just changed into polymer three-dimensional network structure, i.e. cross-links Structure, while macromolecule forms cross-linked structure, organic siliconresin, silicon dioxide embed crosslink polymer network structure, due to Network structure is coupled together by intermolecular chemical bond.So its suds suppressing properties is good, unattenuated, it is disappeared and presses down by emulsifying agent Bubble impaired performance is inconspicuous, and the polymer formed is prone to further processed, made by this silicon composition The solid defoaming agent that standby silicone active thing is finally obtained, it is ensured that the antifoam performance of defoamer and the compatibility so that whole Individual cleaning process can fully froth breaking and suds.

Detailed description of the invention

Embodiment 1

A kind of silicon composition, it is characterised in that include following raw material, and each raw material accounts for organosilicon gross mass percentage ratio For:

A. viscosity is the Me of 600mPa s₃SiO(MeHSiO)₄₅(Me₂SiO)₂₆₀SiMe₃ 500g

B. viscosity is the Me of 20mPa s₃SiO(MeHSiO)₁₀SiMe₃ 3.5g

The organic siliconresin 18g of C.M:Q=0.75:1

D. α-laurylene 165g

E. platinum content is the isopropyl alcohol solution of chloroplatinic acid 1.1g of 11ppm

F. specific surface area is 90m²The sedimentation method hydrophobic silica 30g of/g

Add the hydrogeneous polysiloxane Me that 500g viscosity is 600mPa s in a reservoir₃SiO(MeHSiO)₄₅ (Me₂SiO)₂₆₀SiMe₃, the organic siliconresin of M:Q=0.75:1 of 18g, add 165g α-laurylene 70 DEG C of insulations After 0.5h, 60 DEG C add the isopropyl alcohol solution of chloroplatinic acid that 1.1g platinum content is 11ppm, react 1h at 120 DEG C, add 3.5g Me₃SiO(MeHSiO)₁₀SiMe₃It is 90m with 30g specific surface area²The sedimentation method hydrophobic silica of/g, is warming up to 150 DEG C of reactions Insulation 0.5h, after forming the silicon composition of crosslinking, maintains 0.8h, after being down to room temperature and get final product under-0.05MPa vacuum To the flaxen thick silicon composition S1 that viscosity is 30000mPa s.

Embodiment 2

Embodiment 2 is with the difference of embodiment 1, the raw material of described silicon composition, and each raw material accounts for organosilicon Gross mass percentage ratio is:

A. viscosity is the (C of 1200mPa s₂H₅)₂HSiO(MeHSiO)₁₃₀(Me₂SiO)₄₅₀Si H(C₂H₅)₂ 450g

B. viscosity is the (CH of 6mPa s₂=CH)Me₂ SiOSiMe₂ (CH=CH₂) 20g

The organic siliconresin 10g of C.M:Q=0.5:1

D. dipentene 458g

E. platinum content is the platinum-ol salt complex 2g of 3ppm

F. specific surface area is 50m²The sedimentation method hydrophobic silica 60g of/g.

Embodiment 3

Embodiment 3 is with the difference of embodiment 1, the raw material of described silicon composition, and each raw material accounts for organosilicon Gross mass percentage ratio is:

A. viscosity is the Me of 1500mPa s₃SiO(MeHSiO)₁₅₅(Me₂SiO)₅₀₀SiMe₃ 750g

B. viscosity is the Me of 7mPa s₃SiO(MeHSiO)₂SiMe₃ 30g

The organic siliconresin 50g of C.M:Q=0.8:1

D. styrene 150g

E. platinum content is the platinum-alkene complex 0.1g of 7ppm

F. specific surface area is 420m²The sedimentation method hydrophobic silica 20g of/g.

Embodiment 4

Embodiment 4 is with the difference of embodiment 1, the raw material of described silicon composition, and each raw material accounts for organosilicon Gross mass percentage ratio is:

A. viscosity is the Me of 15mPa s₃SiO(MeHSiO)₅(Me₂SiO)₁₀SiMe₃ 500g

B. viscosity is the Me of 50mPa s₃SiO(MeHSiO)₄₀SiMe₃ 1g

The organic siliconresin 100g of C.M:Q=1.2:1

D. α-octene 368.2g

E. platinum content is the isopropyl alcohol solution of chloroplatinic acid 0.8g of 14ppm

F. specific surface area is 500m²The vapor phase method hydrophobic silica 30g of/g.

Embodiment 5

Embodiment 5 is with the difference of embodiment 1, the raw material of described silicon composition, and each raw material accounts for organosilicon Gross mass percentage ratio is:

A. viscosity is the Me of 1000mPa s₂HSiO(MeHSiO)₁₀₅(Me₂SiO)₃₀₀SiHMe₂ 600g

B. viscosity is the Me of 32mPa s₃SiO(Me(CH₂=CH)SiO)₂₀SiMe₃ 2g

The organic siliconresin 80g of C.M:Q=0.7:1

D. α-octadecylene 219g

E. platinum content is the platinum-ether complexes 1g of 9ppm

F. specific surface area is 250m²The vapor phase method hydrophobic silica 50g of/g.

Embodiment 6

A kind of silicon composition, it is characterised in that include following raw material, and each raw material accounts for organosilicon gross mass percentage ratio and is:

A. viscosity is the Me of 100mPa s₃SiO(MeHSiO)₅₅(Me₂SiO)₅₀SiMe₃ 500g

B. viscosity be 10mPa s (MeHSiO)₄ 45g

The organic siliconresin 45g of C.M:Q=0.65:1

D. α-decene 275g

E. platinum content is the isopropyl alcohol solution of chloroplatinic acid 1.2g of 5ppm

F. specific surface area is 80m²The vapor phase method hydrophobic silica 45g of/g

Add the hydrogeneous polysiloxane Me that 500g viscosity is 100mPa s in a reservoir₃SiO(MeHSiO)₅₅ (Me₂SiO)₅₀SiMe₃, the organic siliconresin of 45g M:Q=0.65:1, add 275g α-decene 50 DEG C insulation 5h after, 70 DEG C add the isopropyl alcohol solution of chloroplatinic acid that 1.2g platinum content is 5ppm, react 1.2h at 150 DEG C, add 45g (MeHSiO)₄And 45g Specific surface area is 80m²The vapor phase method hydrophobic silica of/g, is warming up to 160 DEG C of reaction insulation 2h, forms the organosilicon group of crosslinking After compound, maintaining 1.5h under-0.01MPa vacuum, i.e. obtaining viscosity after being down to room temperature is the faint yellow of 45000mPa s Thick silicon composition S2.

Embodiment 7

Embodiment 7 is from the different of embodiment 6: the raw material of described silicon composition, and each raw material accounts for organosilicon Gross mass percentage ratio is:

A. viscosity is the Me of 180mPa s₃SiO(MeHSiO)₁₆₀Me₂SiOSiMe₃ 748.8g

B. viscosity is the (Me (CH of 9mPa s₂=CH)SiO)₃ 40g

The organic siliconresin 60g of C.M:Q=0.72:1

D. α-hexene 10g

E. platinum content is the platinum-vinyl complex 1.2g of 11ppm

F. specific surface area is 160m²The vapor phase method hydrophobic silica 55g of/g.

Embodiment 8

Embodiment 8 is from the different of embodiment 6: the raw material of described silicon composition, and each raw material accounts for organosilicon Gross mass percentage ratio is:

A. viscosity is the Me of 1850mPa s₃SiO(MeHSiO)₆₅(Me₂SiO)₈₀₀SiMe₃ 460g

B. viscosity is (MeHSiO) of 16mPa s₆ 1g

The organic siliconresin 10g of C.M:Q=0.78:1

D. α-hexadecylene 500g

E. platinum content is the platinum-ol complex 1g of 16ppm

F. specific surface area is 360m²The vapor phase method hydrophobic silica 28g of/g.

Embodiment 9

Embodiment 9 is from the different of embodiment 6: the raw material of described silicon composition, and each raw material accounts for organosilicon Gross mass percentage ratio is:

A. viscosity is the Me of 1500mPa s₂HSiO(MeHSiO)₁₅₅(Me₂SiO)₅₀₀SiHMe₂ 510g

B. viscosity is the Me of 13mPa s₃SiO(MeHSiO)₅SiMe₃ 10g

The organic siliconresin 30g of C.M:Q=0.8:1

D. α-methyl styrene 400g

E. platinum content is the platinum-alkene complex 1.7g of 15ppm

F. specific surface area is 420m²The sedimentation method hydrophobic silica 48.3g of/g.

Embodiment 10

A. viscosity is the Me of 120mPa s₃SiO(MeHSiO)₄₀(Me₂SiO)₇₀SiMe₃ 500g

B. viscosity is the Me of 36mPa s₃SiO(MeHSiO)₂₅SiMe₃ 33g

The organic siliconresin 35g of C.M:Q=0.75:1

D. propine 728g

E. platinum content is the isopropyl alcohol solution of chloroplatinic acid 1.05g of 9ppm

F. specific surface area is 380m²The vapor phase method hydrophobic silica 28g of/g

Add the hydrogeneous polysiloxane Me that 500g viscosity is 120mPa s in a reservoir₃SiO(MeHSiO)₄₀ (Me₂SiO)₇₀SiMe₃, the organic siliconresin of 35g M:Q=0.75:1, add 728g propine, 80 DEG C insulation 0.2h after, 80 DEG C add the isopropyl alcohol solution of chloroplatinic acid that 1.05g platinum content is 9ppm, react 2h at 170 DEG C, add 33g Me₃SiO (MeHSiO)₂₅SiMe₃It is 380m with 28g specific surface area²The vapor phase method hydrophobic silica of/g, is warming up to 200 DEG C of reaction insulations 1h, maintains 0.1h under-0.05MPa vacuum after forming the silicon composition of crosslinking, i.e. obtaining viscosity after being down to room temperature is The flaxen thick silicon composition S3 of 60000mPa s.

Embodiment 11

Embodiment 11 is with the difference of embodiment 10, the raw material of described silicon composition, and each raw material occupies machine Silicon gross mass percentage ratio is:

A. viscosity is the Me of 800mPa s₃SiO(MeHSiO)₁₆₀(Me₂SiO)₁₈₀SiMe₃ 600g

B. viscosity is (MeHSiO) of 16mPa s₆ 44g

The organic siliconresin 70g of C.M:Q=0.78:1

D. camphene 25g

E. platinum content is the platinum-ol complex 0.5g of 20ppm

F. specific surface area is 300m²The sedimentation method hydrophobic silica 35.5g of/g.

Embodiment 12

Embodiment 12 is with the difference of embodiment 10, the raw material of described silicon composition, and each raw material occupies machine Silicon gross mass percentage ratio is:

A. viscosity is the Me of 250mPa s₃SiO(MeHSiO)₁₀₀(Me₂SiO)₁₀₀SiMe₃ 610g

B. viscosity is the Me of 32mPa s₃SiO(MeHSiO)₂₀SiMe₃ 28g

The organic siliconresin 20g of C.M:Q=0.77:1

D. α-icosa alkene 300g

E. platinum content is the platinum-ol complex 1.5g of 17ppm

F. specific surface area is 100m²The vapor phase method hydrophobic silica 40.5g of/g.

Embodiment 13

Embodiment 13 is with the difference of embodiment 10, the raw material of described silicon composition, and each raw material occupies machine Silicon gross mass percentage ratio is:

A. viscosity is the Me of 300mPa s₃SiO(MeHSiO)₂₀₀(Me₂SiO)₅₀SiMe₃ 620g

B. viscosity is the Me of 40mPa s₃SiO(MeHSiO)₃₀SiMe₃ 16g

The organic siliconresin 40g of C.M:Q=0.73:1

D. α-methyl styrene 8g, australene 9g, α-hexadecylene 11g

E. platinum content is the isopropyl alcohol solution of chloroplatinic acid 1.5g of 6ppm

F. specific surface area is 250m²The sedimentation method hydrophobic silica 42.5g of/g.

Embodiment 14

A. viscosity is the Me of 550mPa s₃SiO(MeHSiO)₂₀₀(Me₂SiO)₁₀₀SiMe₃ 500g

B. viscosity is the Me of 45mPa s₃SiO(MeHSiO)₃₅SiMe₃ 33g

The organic siliconresin 35g of C.M:Q=0.68:1

D. α-methyl styrene 54g, dipentene 70g, α-hexadecylene 784g

E. platinum content is the isopropyl alcohol solution of chloroplatinic acid 1.05g of 15ppm

Add the hydrogeneous polysiloxane Me that 500g viscosity is 550mPa s in a reservoir₃SiO(MeHSiO)₂₀₀ (Me₂SiO)₁₀₀SiMe₃, the organic siliconresin of 35g M:Q=0.68:1, add 54g α-methyl styrene, 70g dipentene, 784g α-hexadecylene is after 70 DEG C of insulation 0.5h, and 60 DEG C add the isopropyl alcohol solution of chloroplatinic acid that 1.05g platinum content is 15ppm, 110 DEG C of reaction 2.5h, add 33g Me₃SiO(MeHSiO)₃₅SiMe₃It is 380m with 28g specific surface area²The vapor phase method hydrophobic two of/g Silicon oxide, is warming up to 180 DEG C of reaction insulation 2.5h, ties up after forming the silicon composition of crosslinking under-0.06MPa vacuum Hold 0.9h, after being down to room temperature, i.e. obtain the flaxen thick silicon composition S4 that viscosity is 73000mPa s.

Embodiment 15

Embodiment 15 is with the difference of embodiment 14, the raw material of described silicon composition, and each raw material occupies machine Silicon gross mass percentage ratio is:

A. viscosity is the Me of 1700mPa s₃SiO(MeHSiO)₃₅(Me₂SiO)₇₀₀SiMe₃ 660g

B. viscosity is (MeHSiO) of 13mPa s₅ 25g

The organic siliconresin 90g of C.M:Q=0.4:1

D. α-hexene 200g

E. platinum content is the isopropyl alcohol solution of chloroplatinic acid 1.4g of 10ppm

F. specific surface area is 450m²The sedimentation method hydrophobic silica 23.6g of/g.

Embodiment 16

Embodiment 16 is with the difference of embodiment 14, the raw material of described silicon composition, and each raw material occupies machine Silicon gross mass percentage ratio is:

A. viscosity is the Me of 2000mPa s₃SiO(MeHSiO)₁₈₀(Me₂SiO)₈₀₀SiMe₃ 560g

B. viscosity is the Me of 40mPa s₃SiO(Me(CH₂=CH)SiO)₃₀SiMe₃ 35g

The organic siliconresin 50g of C.M:Q=0.9:1

D. australene 320g

E. platinum content is the platinum-ol complex 1.6g of 6ppm

F. specific surface area is 320m²The vapor phase method hydrophobic silica 33.4g of/g.

Embodiment 17

A. viscosity is the Me of 250mPa s₃SiO(MeHSiO)₁₀₀(Me₂SiO)₁₀₀SiMe₃ 500g

B. viscosity is the (Me (CH of 13mPa s₂=CH)SiO)₅ 10g

The organic siliconresin 62g of C.M:Q=0.75:1

D. α-laurylene 301g, dipentene 99g, styrene 123g

E. platinum content is the isopropyl alcohol solution of chloroplatinic acid 1.0g of 14ppm

F. specific surface area is 150m²The sedimentation method hydrophobic silica 40g of/g

Add the hydrogeneous polysiloxane Me that 500g viscosity is 250mPa s in a reservoir₃SiO(MeHSiO)₁₀₀ (Me₂SiO)₁₀₀SiMe₃, the organic siliconresin of 62g M:Q=0.75:1, add 301g α-laurylene, 99g dipentene, 123g Cinnamic mixture is after 70 DEG C of insulation 0.5h, and 60 DEG C add the isopropyl alcohol solution of chloroplatinic acid that 1.0g platinum content is 14ppm, 180 DEG C of reaction 3h, add 10g (Me (CH₂=CH)SiO)₅It is 150m with 40g specific surface area²The sedimentation method hydrophobic titanium dioxide of/g Silicon, is warming up to 200 DEG C of reaction insulation 3h, after forming the silicon composition of crosslinking, maintains 0.1 under-0.08MPa vacuum ～1.5h, i.e. obtain the flaxen thick silicon composition S5 that viscosity is 65000mPa s after being down to room temperature.

Embodiment 18

A. viscosity is the Me of 170mPa s₃SiO(MeHSiO)₇₅(Me₂SiO)₈₀SiMe₃ 500g

B. viscosity is the Me of 5mPa s₂HSiOSiHMe₂ 35g

The organic siliconresin 39g of C.M:Q=0.75:1

D. α-octadecylene 885g

E. platinum content is the isopropyl alcohol solution of chloroplatinic acid 1.1g of 16ppm

F. specific surface area is 130m²The sedimentation method hydrophobic silica 40g of/g

Add the hydrogeneous polysiloxane Me that 500g viscosity is 170mPa s in a reservoir₃SiO(MeHSiO)₇₅ (Me₂SiO)₈₀SiMe₃, the organic siliconresin of 39g M:Q=0.75:1, add 885g α-octadecylene, 70 DEG C be incubated 0.5h After, 70 DEG C add the isopropyl alcohol solution of chloroplatinic acid that 1.1g platinum content is 16ppm, react 1.5h at 130 DEG C, add 35g Me₂HSiOSiHMe₂It is 130m with 40g specific surface area²The sedimentation method hydrophobic silica of/g, is warming up to 150 DEG C of reaction insulations 0.8h, after forming the silicon composition of crosslinking, maintains 0.1～1.5h, after being down to room temperature and get final product under-0.08MPa vacuum To the flaxen thick silicon composition S6 that viscosity is 35000mPa s.

Embodiment 19

Embodiment 19 is with the difference of embodiment 18, the B choice structure formula in the raw material of described silicon composition As follows, viscosity is the branched chain silicones of 34mPa s.

Embodiment 20

Embodiment 20 is with the difference of embodiment 18, the B choice structure formula in the raw material of described silicon composition As follows, viscosity is the branched chain silicones of 39mPa s.

Embodiment 21

Embodiment 21 is with the difference of embodiment 18, the B choice structure formula in the raw material of described silicon composition As follows, viscosity is the branched chain silicones of 48mPa s.

Embodiment 22

Embodiment 22 is with the difference of embodiment 18, the B choice structure formula in the raw material of described silicon composition As follows, viscosity is the branched chain silicones of 52mPa s.

Embodiment 23

Embodiment 23 is with the difference of embodiment 18, the B choice structure formula in the raw material of described silicon composition As follows, viscosity is the branched chain silicones of 60mPa s.

Comparative example 1

The organic siliconresin 45g of B.M:Q=0.65:1

C. α-decene 275g

D. platinum content is the isopropyl alcohol solution of chloroplatinic acid 1.2g of 10ppm

E. specific surface area is 200m²The sedimentation method hydrophobic silica 45g of/g

Add the hydrogeneous polysiloxane Me that 500g viscosity is 550mPa s in a reservoir₃SiO(MeHSiO)₂₀₀ (Me₂SiO)₁₀₀SiMe₃, the organic siliconresin of 45g M:Q=0.65:1, add 275g α-decene 70 DEG C insulation 0.5h after, 70 DEG C add the isopropyl alcohol solution of chloroplatinic acid that 1.2g platinum content is 10ppm, react 2.5h at 110 DEG C, add 45g specific surface area and are 200m²The sedimentation method hydrophobic silica of/g, is warming up to 160 DEG C of reaction insulation 2h, maintains 0.1 under-0.06MPa vacuum ～1.5h, i.e. obtain the flaxen thick silicon composition FS1 that viscosity is 1500mPa s after being down to room temperature.

Comparative example 2:

Silicon composition FS2 is prepared according to patent [CN200610040821.3] embodiment [1].

Embodiment 24

Silicone active thing prepared by the silicon composition S1 described in embodiment 1: by the silicon composition S1 of 35g, The lauric acid polyoxyethylene ether of 20g and the polyacrylic acid of 45g directly mix, and then cross colloid mill and homogenize and load container after 0.2h In, warming while stirring to 80 DEG C abundant mixing 0.5h i.e. obtains silicone active thing AS1, and viscosity is 2000mPa s.

Embodiment 25

Silicone active thing prepared by the silicon composition S2 described in embodiment 6: by the silicon composition S2 of 65g, The sorbitan trioleate of 5g and the sodium carboxymethyl cellulose of 30g directly mix, and then cross colloid mill and homogenize 0.5h In rear loading container, warming while stirring to 80 DEG C abundant mixing 0.7h, obtain silicone active thing AS2, viscosity is 2900mPa·s。

Embodiment 26

Silicone active thing prepared by the silicon composition S3 described in embodiment 10: by the silicon composition S3 of 57g, The oleic acid polyoxyethylene of 30g and the sodium citrate of 13g directly mix, and then cross colloid and homogenize and load after 0.2h in container, Warming while stirring, to 80 DEG C of abundant mixing 1h, obtains silicone active thing AS3, and viscosity is 3500mPa s.

Embodiment 27

Silicone active thing prepared by the silicon composition S4 described in embodiment 14: by the silicon composition of 48g The castor oil polyoxyethylene ether of S4,17g and the potassium citrate of 35g directly mix, and then cross colloid and homogenize to load after 0.4h and hold In device, warming while stirring to 80 DEG C abundant mixing 1.5h, obtain silicone active thing AS4, viscosity is 4100mPa s.

The silicon composition that embodiment 24 ~ 27 uses the present invention to prepare prepares silicone active thing, wherein uses glue Body grinds the process that homogenizes, and the compatibility of the silicone active thing obtained is good, and antifoaming performance is more excellent.

Comparative example 3

Silicone active thing prepared by the silicon composition FS1 described in comparative example 1: by the silicon composition of 65g FS1,15g lauric acid polyoxyethylene ether and 20g sodium carboxymethyl cellulose directly mix, and then cross colloid mill and homogenize and fill after 0.1h Entering in container, stirring limit is warming up to 80 DEG C of abundant mixing 0.5h, obtains silicone active thing AFS1, and viscosity is 6000mPa s.

Comparative example 4

Silicone active thing prepared by the silicon composition S5 described in embodiment 17: by the silicon composition S5 of 47g, The lauric acid polyoxyethylene ether of 33g and the sodium citrate of 20g directly mix, and stirring limit is warming up to 80 DEG C of abundant mixing 2h, to obtain final product Silicone active thing AFS2, viscosity is 30,000mPa s.

Comparative example 5

Silicone active thing prepared by the silicon composition FS2 described in comparative example 2: by the silicon composition of 52g Lauric acid polyoxyethylene ether and the 25g sodium citrate of FS2,23g directly mix, and then cross colloid mill and homogenize to load after 0.1h and hold In device, stirring limit is warming up to 80 DEG C of abundant mixing 0.5h, obtains silicone active thing AFS3, and viscosity is 20,000mPa s.

Example 2 below 8 ~ 31, comparative example 6 ~ 8 are respectively adopted different silicone active thing and prepare solid defoaming agent.

Embodiment 28

75g starch and 45g silicone active thing AS1 are joined in blender, be added thereto to after stirring 10g without Water-ethanol；After stirring, the mixture pelleting obtained is dried, i.e. obtain prepared solid defoaming agent.

Embodiment 29

60g sodium sulfate (800 mesh) and 18g silicone active thing AS2 are joined in blender, after stirring wherein Add 3g dehydrated alcohol and 3g deionized water；After stirring, the mixture pelleting obtained is dried, i.e. obtain prepared consolidating Body defoamer.

Embodiment 30

50g sodium aluminosilicate and 20g silicone active thing AS3 are joined in blender, is added thereto to after stirring 2g deionized water；After stirring, the mixture pelleting obtained is dried, i.e. obtain prepared solid defoaming agent.

Embodiment 31

65g starch and 35g silicone active thing AS4 are joined in blender, be added thereto to after stirring 7g without Water-ethanol；After stirring, the mixture pelleting obtained is dried, i.e. obtain prepared solid defoaming agent.

Comparative example 6

75g starch and 45g silicone active thing AFS1 are joined in blender, after stirring, is added thereto to 10g Dehydrated alcohol；After stirring, the mixture pelleting obtained is dried, i.e. obtain prepared solid defoaming agent.

Comparative example 7

75g starch and 45g silicone active thing AFS2 are joined in blender, after stirring, is added thereto to 10g Dehydrated alcohol；After stirring, the mixture pelleting obtained is dried, i.e. obtain prepared solid defoaming agent.

Comparative example 8

75g starch and 45g silicone active thing AFS3 are joined in blender, after stirring, is added thereto to 10g Water；After stirring, the mixture pelleting obtained is dried, i.e. obtain prepared solid defoaming agent.

Antifoaming performance is tested

The solid defoaming agent sample of the solid defoaming agent of embodiment 28-31 with comparative example 6 ~ 8 is surveyed as follows Examination.

1. washing machine test

Method of testing: adding the commercially available detergent of 150g in the roller washing machine that capacity is 7.5kg, 0.75g solid disappears Infusion, test program is bafta program.The door of washing machine is marked with 0,10,20 that 10 tolerance signs, respectively door are high, 30…..100.And respectively it is designated as " 0 ", " 10 ", " 20 ", " 30 " ... .. " 100 "." 0 " is initial, represents non-foam, " 100 " table Show full foam.Every 5min records a foam height, record during shutdown.Numerical value is the biggest, shows the foam height in washing machine The highest, suds is the poorest；In the identical time, foam height is the lowest, illustrates that product suds suppressing properties is the best.Test result is as follows:

Table 1 washing machine test result

Can be shown by upper table, the solid defoaming agent in embodiment 28-31 is to use silicon composition of the present invention, warp Cross colloid mill homogenize process obtain what silicone active thing was prepared from, described solid defoaming agent washing early stage foam rich Richness, good in later stage rinse stage suds effect, save cost.The solid defoaming agent of comparative example 7 uses the organosilicon of the present invention Prepared by compositions, but owing to silicon composition does not carries out the process that homogenizes, and viscosity is big, and carrier is difficult to mix homogeneously, and Test process is difficult to diffusion sprawl, causes poor-performing.

2. horizontal circulation Bubbling method:

Method of testing: the glass of horizontal circulation bubbling instrument (Nanjing Sixin Science Application Research Institute Co., Ltd's manufacture) is shown on trial Subscript 0,1,2,3 four tolerance indicate." 0 " is initial, represents non-foam, and " 3 " represent full foam.At horizontal circulation bubbling Add 0.3% sodium dodecyl benzene sulfonate aqueous solution (pH value is 13) of 14kg in instrument, then open temperature detect switch (TDS), by foam liquid Being heated to testing temperature 80 DEG C, the foam such as ON cycle pump rises to certain altitude and (rises to time of certain altitude when being blank Between) time, then it is added thereto to 0.5g defoamer, record foam height Changing Pattern over time.Foam rises to same a moment Time used by degree is the longest, illustrates that suds suppressing properties is the best.Test result is shown in Table 2:

Table 2 horizontal circulation test result

By above-mentioned test, it can be seen that homogenized by colloid mill when preparing silicone active thing and can make organosilicon group Compound and emulsifying agent are sufficiently mixed, and reduce viscosity, then are adsorbed onto on carrier, and the defoamer froth breaking of gained is preferable, completely Meet and exceed the defoamer performance that normal process prepares.

Claims

1. a silicon composition, it is characterised in that its raw material and each raw material account for silicon composition gross mass percentage ratio and be:

The hydrogeneous polysiloxane of A 45 ~ 75%

At least one formula is H_cR⁰ _3-cSiO (R⁰HSiO)_d (R⁰ ₂SiO)_bSiR⁰ _3-cH_cHydrogeneous polysiloxane；Wherein, Substituent R⁰Identical or different, for the alkyl of carbon number 1～20；SubscriptcIt is 0,1 or 2, subscriptdBe 0 or 1 ~ 200 whole Number, andc+d>=1, subscriptbBeing the integer of 1 ~ 1000, each molecule has the hydrogen atom of at least 1 silicon bonding；

B cross-linking agent 0.1 ~ 5%

Described cross-linking agent is the following polysiloxanes of at least one structural formula: wherein R¹Identical or different, it is 1 ~ 10 for carbon number Alkyl, hydrogen atom or vinyl；R²Identical or different, for alkyl, hydrogen atom or vinyl that carbon number is 1 ~ 10；Subscript m It it is the integer of 0 ~ 50；N is the integer of 0 ~ 5；S is the integer of 0 ~ 30；Each molecule has hydrogen atom or the second of at least 1 silicon bonding Thiazolinyl；

Or formula is (R³HSiO)_fRing-type hydrogeneous polysiloxane, R³For the alkyl of carbon number 1 ~ 10,fBe 3 ~ 6 whole Number；

C silicone-containing unit R_aSiO_4-a/2Organic siliconresin 1 ~ 10%

D unsaturated hydrocarbons 10 ~ 50%

Described unsaturated hydrocarbons includes that alkene and alkynes, described alkene are the alpha-olefin of straight chain, alicyclic olefin, aromatic olefin Or the mixing of any one or more in branching type alkene；Described alkynes is acetylene, propine, butine, pentyne, hexin, heptan The mixing of any one or more in alkynes or octyne；

E catalyst 0.01 ~ 0.2%

Described catalyst is selected from platinum-ol complex, platinum-alkene complex, platinum-ol salt complex, platinum-ether complexes, platinum-one Complex, isopropyl alcohol solution of chloroplatinic acid or platinum-vinyl complex；The platinum content of described catalyst is 1 ~ 20ppm；

F silicon dioxide 2 ~ 6%；

Being specially hydrophobic silica, specific surface area is 50 ~ 500m²/ g, hydrophobic including vapor phase method hydrophobic silica and the sedimentation method Silicon dioxide；

The preparation method of described silicon composition, specifically comprises the following steps that

1. hydrogeneous polysiloxane A, organic siliconresin C and unsaturated hydrocarbons D are joined in reaction vessel, be warming up to 50 ~ 80 DEG C, it is incubated 0.2～5h, makes organic siliconresin dissolve；

2. add catalyst E, after 100 ~ 200 DEG C of reaction 1 ~ 3h, add crosslinking agent B and silicon dioxide F, 150 ~ 200 DEG C of insulations Until forming the polymer of crosslinking；

3. after insulation terminates, and under-0.01 ~-0.08MPa vacuum, 0.1～1.5h is maintained；Finally, room temperature it is cooled to i.e. Obtaining the cross-linked silicone compositions of thickness, viscosity is 20,000 ~ 100,000mPa s.

Silicon composition the most according to claim 1, it is characterised in that: in described A, hydrogeneous polysiloxane exists Dynamic viscosity when 25 DEG C is 10 ~ 2000mPa s, and the dynamic viscosity when 25 DEG C of the cross-linking agent described in B is 5 ~ 50 mPa s。

Silicon composition the most according to claim 1, it is characterised in that: in the described polysiloxanes in B: R²Base is Methyl；Subscript m is the integer of 5 ~ 40, and n is the integer of 1 ~ 3；S is the integer of 2 ~ 25.

Silicon composition the most according to claim 1, it is characterised in that: in described D the alpha-olefin of straight chain be α-oneself Alkene, α-octene, α-decene, α-laurylene, α-tetradecene, α-hexadecylene, α-octadecylene, α-icosa alkene, α-C20 ~ C24 alkene The mixture of mixture, α-C24 ~ C28 alkene or α-three ten alkene；Described alicyclic olefin is pinene, camphene, dipentene, ring penta Alkene or norborene；Described aromatic olefin is α-methyl styrene or styrene；Described ramiform alkene is iso-amylene Or isooctene.

5. the silicone active thing that prepared by the silicon composition described in any one of claim 1-4, its raw material and each former Material accounts for the percentage ratio of organosilicon active matter gross mass:

I. the silicon composition 35 ~ 65% described in any one of claim 1-4；

II. emulsifying agent, for nonionic surfactant 5 ~ 35%；

III. structural agent 9～50%；

Wherein, described emulsifying agent is nonionic surfactant；Described structural agent be acrylic polymer, cellulose ether, The mixing of any one or more in citric acid or citric acid salt or polyvinylpyrrolidone.

Silicone active thing the most according to claim 5, it is characterised in that: described acrylic polymer is maleic acid propylene Acid copolymer, polyacrylic acid or its partial sodium salt；Described cellulose ether refers to water miscible or water swellable cellulose ether；Described Citric acid salt is sodium citrate or potassium citrate；These structural agents can be used alone, it is also possible to arbitrary proportion is used in mixed way.

7. the preparation method of the silicone active thing described in a claim 5: by the silicon composition of formula ratio, emulsifying agent It is mixed directly with structural agent, loads in container after colloid mill homogenizes 0.1 ~ 0.5h, warming while stirring to 80 DEG C Fully mixing 0.5 ~ 2h, obtaining viscosity is 1000 ~ 10, the silicone active thing of 000mPa s.

8. the solid defoaming agent that prepared by the silicone active thing described in claim 5, its raw material and each raw material account for solid and disappear The percentage ratio of infusion gross mass is:

Silicone active thing 18 ~ 45% described in claim 5；

Carrier 50 ~ 75%；

Solvent 2 ~ 10%；

Wherein, described carrier is in sulfate, carbonate, phosphate, Quadrafos, starch, cellulose or aluminosilicate The mixing of any one or more；

Described solvent is the mixing of any one or more in alcohols material or water.

9. a preparation method for the solid defoaming agent described in claim 8, concrete operation step is as follows: first by formula ratio Silicone active thing and carrier join in blender, are added thereto to the solvent mixing of formula ratio after stirring, and pelletize is dried Dry.