CN1061364C - Silicon propyl resin for paint and its producing method - Google Patents
Silicon propyl resin for paint and its producing method Download PDFInfo
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- CN1061364C CN1061364C CN97106656A CN97106656A CN1061364C CN 1061364 C CN1061364 C CN 1061364C CN 97106656 A CN97106656 A CN 97106656A CN 97106656 A CN97106656 A CN 97106656A CN 1061364 C CN1061364 C CN 1061364C
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- organosilicon
- acrylic resin
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- cyclotetrasiloxanes
- acrylate monomer
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- 239000011347 resin Substances 0.000 title claims abstract description 14
- 229920005989 resin Polymers 0.000 title claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 13
- 239000010703 silicon Substances 0.000 title claims abstract description 13
- 239000003973 paint Substances 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 14
- 239000000178 monomer Substances 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 6
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 5
- 230000003197 catalytic effect Effects 0.000 claims abstract description 4
- 239000004925 Acrylic resin Substances 0.000 claims description 49
- 229920000178 Acrylic resin Polymers 0.000 claims description 49
- 238000000576 coating method Methods 0.000 claims description 24
- 239000011248 coating agent Substances 0.000 claims description 23
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 12
- JGWUKKFNKOUBPW-UHFFFAOYSA-N 2-ethenyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical class C=C[SiH]1O[SiH2]O[SiH2]O[SiH2]O1 JGWUKKFNKOUBPW-UHFFFAOYSA-N 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- -1 alkyl cyclotetrasiloxanes Chemical class 0.000 claims description 9
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical compound CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- 239000006096 absorbing agent Substances 0.000 claims description 5
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 5
- 239000013530 defoamer Substances 0.000 claims description 5
- 239000006224 matting agent Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000908 ammonium hydroxide Substances 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- 239000000470 constituent Substances 0.000 claims description 4
- 239000012046 mixed solvent Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 3
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 2
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000009472 formulation Methods 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 230000032683 aging Effects 0.000 abstract description 6
- 230000005855 radiation Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- DDJSWKLBKSLAAZ-UHFFFAOYSA-N cyclotetrasiloxane Chemical compound O1[SiH2]O[SiH2]O[SiH2]O[SiH2]1 DDJSWKLBKSLAAZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000003921 oil Substances 0.000 abstract 1
- RSNQKPMXXVDJFG-UHFFFAOYSA-N tetrasiloxane Chemical compound [SiH3]O[SiH2]O[SiH2]O[SiH3] RSNQKPMXXVDJFG-UHFFFAOYSA-N 0.000 abstract 1
- 239000000543 intermediate Substances 0.000 description 20
- 238000002360 preparation method Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 238000013019 agitation Methods 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 2
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 235000010215 titanium dioxide Nutrition 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- SWSGIYIOESGFJN-UHFFFAOYSA-N 2-butyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical class C(CCC)[SiH]1O[SiH2]O[SiH2]O[SiH2]O1 SWSGIYIOESGFJN-UHFFFAOYSA-N 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- CVQVSVBUMVSJES-UHFFFAOYSA-N dimethoxy-methyl-phenylsilane Chemical compound CO[Si](C)(OC)C1=CC=CC=C1 CVQVSVBUMVSJES-UHFFFAOYSA-N 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- MJEMIOXXNCZZFK-UHFFFAOYSA-N ethylone Chemical compound CCNC(C)C(=O)C1=CC=C2OCOC2=C1 MJEMIOXXNCZZFK-UHFFFAOYSA-N 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical class C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
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- Paints Or Removers (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The present invention relates to silicon propyl resin for paint and a production method thereof. The silicon propyl resin is prepared by the copolymerization of a linear organosilicon intermediate substance and an acrylate monomer, wherein the linear organosilicon intermediate substance is produced by the catalytic polymerization of octavinyl cyclo tetrasiloxane and octa-alkylcyclo tetrasiloxane. The product of the silicon propyl resin has the advantages of regular structure, high transparence and high stability. The silicon propyl resin has the advantages of simple production technology, energy saving and low cost. Paint prepared by the silicon propyl resin can be formed into films at normal temperature or low temperature, and the paint has good performance of oil stain resistance, aging resistance, ultraviolet radiation resistance, hard coated film and good adhesive force.
Description
The present invention relates to a kind of organosilicon acrylic resin and production method thereof.
Organosilicon acrylic resin coating is a kind of coating with weathering resistance and anti-stain characteristic, is widely used in high level, multi-storey building metope, bridge, and highway ground etc. are as protective layer and decoration.
Organosilicon acrylic resin is by line style organosilicon intermediate and acrylate monomer copolymerization and make, owing to introduced organosilicon functional group in the acrylic resin, utilize organosilicon Si-O key that bigger ionic dissociation energy is arranged, improved heat, light stability, thereby improved the weathering resistance of organosilicon acrylic resin, thermotolerance, hydrophobic nature and anti-stain characteristic.
The organosilicon intermediate is one of raw material of synthetic organosilicon acrylic resin, and bibliographical information has two types basically.A kind of is the organosilicon intermediate that contains methoxy or ethoxy, mainly be to be raw material with phenyltrimethoxysila,e and phenyl methyl dimethoxy silane, through partial hydrolysis and or be raw material with the Ethoxysilane, in the presence of acid, get (war Feng Chang through partial hydrolysis, " tailor-(made) coating ", P.114, Chemical Industry Press); Another kind is the organosilicon intermediate of hydroxyl, is to make (Liu Changyin, Shanghai coating, No.1, i.e. .28-34,1992) by the phenyl-trichloro-silicane hydrolysis.By containing methoxy or ethoxy organosilicon intermediate is the organosilicon acrylic resin that raw material is made, water tolerance is relatively poor, and the organosilicon intermediate of hydroxyl then has in reaction from the condensation tendency, has reduced the polymerization chance with acrylic resin, make organosilicon acrylic resin structure irregularity, resin is muddy shape.Therefore be that the performance of the organosilicon acrylic resin that makes of raw material all can not be satisfactory by above two types organosilicon intermediate.
As everyone knows, the performance of organosilicon acrylic resin coating depends primarily on the performance of organosilicon acrylic resin, and therefore synthetic new organosilicon acrylic resin makes it to have more excellent performance, also just can make the organosilicon acrylic resin coating of preparation have more excellent ageing resistance and anti-stain characteristic, be a research work highly significant.
For this reason, the object of the invention provides a kind of silicon propyl resin for paint and production method thereof.Organosilicon acrylic resin is by forming through line style organosilicon intermediate and the acrylate monomer copolymerization that catalytic polymerization generates with eight vinyl cyclotetrasiloxanes and eight alkyl cyclotetrasiloxanes.The organosilicon acrylic resin product structure is regular, transparency height, good stability.Organosilicon acrylic resin coating with this organosilicon acrylic resin preparation has excellent ageing resistance and anti-stain characteristic.
Silicon propyl resin for paint of the present invention is the product that is formed by line style organosilicon intermediate and acrylate monomer copolymerization, described line style organosilicon intermediate is to be generated through catalytic polymerization by eight vinyl cyclotetrasiloxanes and eight alkyl cyclotetrasiloxanes, and its structural formula can be represented by the formula:
R=C in the formula
1-C
4Alkyl, n=5-10.
The production method of silicon propyl resin for paint of the present invention comprises:
The first step is earlier carried out polyreaction with eight vinyl cyclotetrasiloxanes and eight alkyl cyclotetrasiloxanes and is got above-mentioned line style organosilicon intermediate under alkali metal hydroxide catalysis.The catalyzer alkali metal hydroxide can be a sodium hydroxide, one or more in potassium hydroxide or the ammonium hydroxide etc., and consumption is 0.5-2% (weight %).The part by weight of eight vinyl cyclotetrasiloxanes and eight alkyl cyclotetrasiloxanes is 1-4: 1, and temperature of reaction 70-150 ℃, reaction times 5-8 hour.
Gained organosilicon intermediate product water white transparency, purity 100%, viscosity (being coated with-4 glasss) is 180～200 seconds, molecular weight Mn is 700～1000 (VPO)
Second step then carried out copolyreaction with above-mentioned line style organosilicon intermediate and acrylate monomer and promptly gets organosilicon acrylic resin.The weight percent of reactant each component is as follows in this copolyreaction:
Reactant each component weight %
Organosilicon intermediate 0.8-1.2
Acrylate monomer 38-48
Vinylformic acid 0.3-0.5
Dimethylbenzene and N-BUTYL ACETATE mixed solvent (7: 3 proportionings) 50-60
Benzoyl peroxide 0.3-0.8
Acrylate monomer can be a methyl methacrylate, methyl acrylate, ethyl propenoate, one or more in propyl acrylate or the butyl acrylate etc.
Polymeric reaction temperature 120-130 ℃, 5 hours reaction times.
The production method of organosilicon acrylic resin of the present invention is not because the first step and the second step reaction all have by product produces, must aftertreatment, so processing method is simple and convenient, and energy conservation, cost is low.Product organosilicon acrylic resin compound with regular structure, outward appearance is as clear as crystal, does not have mechanical impurity, has good film forming properties under normal temperature or low temperature, and storage stability is good, and viscosity is 2000-4000CPS (rotary viscosity method), and molecular weight Mn is 2.5 * 10
4-3.0 * 10
4
Adopt organosilicon acrylic resin of the present invention, can be mixed with coating routinely, bottom closing paint, mill base etc.For example adopt organosilicon acrylic resin of the present invention, add color stuffing by following proportioning, methodology such as dispersion agent, flow agent, matting agent, ultraviolet absorbers, defoamer and solvent etc. routinely mix, and grind through high speed dispersion and can make versicolor organosilicon acrylic resin coating.Coating stirs in container, no caking phenomenon.
Organosilicon acrylic resin coating is formed by following prescription:
Constituent weight %
Organosilicon acrylic resin 40-50
Color stuffing 20-25
Dispersion agent 0.5-1
Flow agent 0.5-1
Matting agent 5-10
Defoamer 0.5-1
Ultraviolet absorbers 0.5-1
Solvent 15-30
Each constituent is the present invention except silicon third resin in the above-mentioned prescription, and all the other all are the commercial goods, and the color of pigment can need be selected from the commercial goods by the coating color matching, and solvent can be dimethylbenzene or N-BUTYL ACETATE.
The performance of listing the coating (B) that coating (A) that organosilicon acrylic resin of the present invention is made into and commercially available organosilicon acrylic resin be made into below is relatively:
| Performance project | Coating (A) | Coating (B) |
| Anti-stain characteristic (5 circulations) | ＜7％ | 10-15％ |
| Ageing resistance (non-foaming, as not peel off flawless) | 3500 hours | 1000 hours |
| Ultraviolet radiation resisting | 2000 hours | 500 hours |
| Wear resistance (510N, 1000 times) | 0.031 gram | 0.05 gram |
| Permeability resistance (upstream face) MPa | ＞1.5 | 1.4 |
Show that by above-listed coating (A) and performance project contrasting data (B) coating that organosilicon acrylic resin of the present invention is made into has excellent anti-stain characteristic, ageing resistance, ultraviolet radiation resisting, wear resistance and permeability resistance.
Advantage of the present invention: because organosilicon acrylic resin of the present invention is to form by line style organosilicon intermediate and the acrylate monomer copolymerization that is generated by eight vinyl cyclotetrasiloxanes and eight alkyl cyclotetrasiloxane polyreactions, therefore the organosilicon acrylic resin product structure is regular, appearance transparence is good, and storage stability is good.With this organosilicon acrylic resin coatings formulated can be under normal temperature or cold condition film forming, have excellent anti-stain characteristic, ageing resistance, ultraviolet radiation resisting and wear resistance, it is hard to film, sticking power is good.The production method of organosilicon acrylic resin of the present invention is not because the first step and the second step reaction all have by product produces, must aftertreatment, so processing method is easy, and energy conservation, cost is low.
The present invention is further elaborated by following examples, but does not place restrictions on scope of the present invention.
Embodiment 1, the preparation of organosilicon intermediate
With 49.5 parts of eight vinyl cyclotetrasiloxanes, 49.5 parts of octamethylcyclotetrasiloxanes, add in the reactor, under agitation condition, add potassium hydroxide, each 0.5 part in ammonium hydroxide in 70-80 ℃ of reaction 8 hours, promptly gets the organosilicon intermediate, viscosity 180 seconds (being coated with-4 glasss), molecular weight Mn724.
Embodiment 2, the preparation of organosilicon intermediate
With 74 parts of eight vinyl cyclotetrasiloxanes, 24 parts of eight butyl cyclotetrasiloxanes, add in the reactor, under agitation condition, add sodium hydroxide, each 1 part in ammonium hydroxide in 140-150 ℃ of reaction 5 hours, promptly gets the organosilicon intermediate, viscosity 200 seconds (being coated with-4 glasss), molecular weight Mn980.
Embodiment 3, the organosilicon acrylic resin preparation
0.8 part of organosilicon intermediate is added in the reactor, add 60 parts of dimethylbenzene and ester acid butyl ester mixed solvents (7: 3 proportionings), be warmed up to 120-130 ℃, drip following mixed solution: 28 parts of methyl methacrylates, 10 parts of butyl acrylates, 0.5 part in vinylformic acid reaches 0.7 part of benzoyl peroxide, react after 5 hours, be cooled to 50 ℃ with bottom discharge, filter, get organosilicon acrylic resin, viscosity is 2000CPS (rotary viscosity method), and molecular weight Mn is 2.5 * 10
4, contain 40% solids content, package spare.
Embodiment 4, the organosilicon acrylic resin preparation
1.2 parts of organosilicon intermediates are added in the reactor, add 50 parts of dimethylbenzene and ester acid butyl ester mixed solvents (7: 3 proportionings), be warmed up to 120-130 ℃, drip following mixed solution: 32 parts of methyl methacrylates, 16 parts of ethyl propenoates, 0.3 part in vinylformic acid reaches 0.5 part of benzoyl peroxide, react after 5 hours, be cooled to 50 ℃ with bottom discharge, filter, get organosilicon acrylic resin, viscosity is 4000CPS (rotary viscosity method), and molecular weight Mn is 3.0 * 10
4, contain 50% solids content, package spare.
Embodiment 5, the preparation of organosilicon acrylic resin coating
With 40 parts of organosilicon acrylic resins (solids content 50%), 25 parts of titanium dioxides, 0.5 part of dispersion agent, 5 parts of matting agents, 0.5 part of ultraviolet absorbers, 0.5 part of defoamer, 0.5 part of flow agent, 28 parts of dimethylbenzene, mix, high speed dispersion 15-20 minute, enter sand mill and grind, fineness≤45 μ m is the finished product whitewash.
Embodiment 6, the preparation of organosilicon acrylic resin coating
With 50 parts of organosilicon acrylic resins (solids content 40%), 10 parts of titanium dioxides, 10 parts of phthalocyanine blues, 1 part of dispersion agent, 10 parts of matting agents, 1 part of ultraviolet absorbers, 1 part of defoamer, 1 part of flow agent, 16 parts of acetic acid fourth vinegar mix, high speed dispersion 15-20 minute, enter sand mill and grind, fineness≤45 μ m is the blue look coating of finished product.
Claims (6)
1, a kind of silicon propyl resin for paint, it is the product that is formed by line style organosilicon intermediate and acrylate monomer copolymerization, it is characterized in that described line style organosilicon intermediate is to be got through catalytic polymerization by eight vinyl cyclotetrasiloxanes and eight alkyl cyclotetrasiloxanes, its structural formula can be represented by the formula:
The part by weight of eight vinyl cyclotetrasiloxanes and eight alkyl cyclotetrasiloxanes is 1-4: 1, the organosilicon intermediate accounts for 0.8-1.2 weight % in the copolyreaction of organosilicon intermediate and acrylate monomer, acrylate monomer accounts for 38-48 weight %, the molecular weight Mn of organosilicon intermediate is 700-1000, and the molecular weight Mn of organosilicon acrylic resin is 2.5 * 10
4-3.0 * 10
4
2, the production method of the described silicon propyl resin for paint of claim 1 is characterized in that it comprises:
Polyreaction under alkali metal hydroxide catalysis makes line style organosilicon intermediate to the first step with eight vinyl cyclotetrasiloxanes and eight alkyl cyclotetrasiloxanes earlier, the part by weight of eight vinyl cyclotetrasiloxanes and eight alkyl cyclotetrasiloxanes is 1-4 in the reaction: 1, catalyzer alkali metal hydroxide consumption is 0.5-2% (weight %), temperature of reaction 70-150 ℃, reaction times 5-8 hour, the molecular weight Mn of gained organosilicon intermediate was 700-1000;
Second step then carried out copolyreaction with above-mentioned line style organosilicon intermediate and acrylate monomer and promptly gets organosilicon acrylic resin, and the weight percent of reactant each component is as follows in this copolyreaction:
Reactant each component weight %
Organosilicon intermediate 0.8-1.2
Acrylate monomer 38-48
Vinylformic acid 0.3-0.5
Dimethylbenzene and N-BUTYL ACETATE mixed solvent (7: 3 proportionings) 50-60
Benzoyl peroxide 0.3-0.8
Polymeric reaction temperature 120-130 ℃, in 5 hours reaction times, the molecular weight Mn of gained organosilicon acrylic resin is 2.5 * 10
4-3.0 * 10
4
3, production method according to claim 2 is characterized in that catalyzer alkali metal hydroxide described in the first step reaction is one or more in sodium hydroxide, potassium hydroxide, the ammonium hydroxide.
4, production method according to claim 2 is characterized in that acrylate monomer described in the reaction of second step is one or more in methyl methacrylate, methyl acrylate, ethyl propenoate, propyl acrylate or the butyl acrylate.
5, the purposes of the described organosilicon acrylic resin of claim 1 is characterized in that it can be applicable to become organosilicon acrylic resin coating by following constituent formulated:
Constituent weight %
Organosilicon acrylic resin 40-50
Color stuffing 20-25
Dispersion agent 0.5-1
Flow agent 0.5-1
Matting agent 5-10
Defoamer 0.5-1
Ultraviolet absorbers 0.5-1
Solvent 15-30
6,, it is characterized in that solvent used in the organosilicon acrylic resin formulation for coating material is dimethylbenzene or N-BUTYL ACETATE according to the purposes of the described organosilicon acrylic resin of claim 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97106656A CN1061364C (en) | 1997-10-15 | 1997-10-15 | Silicon propyl resin for paint and its producing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97106656A CN1061364C (en) | 1997-10-15 | 1997-10-15 | Silicon propyl resin for paint and its producing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1178819A CN1178819A (en) | 1998-04-15 |
| CN1061364C true CN1061364C (en) | 2001-01-31 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97106656A Expired - Fee Related CN1061364C (en) | 1997-10-15 | 1997-10-15 | Silicon propyl resin for paint and its producing method |
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| CN (1) | CN1061364C (en) |
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| DE102006037270A1 (en) | 2006-08-09 | 2008-02-14 | Wacker Chemie Ag | Self-dispersible silicone copolymers and process for their preparation and their use |
| ATE477065T1 (en) * | 2007-06-22 | 2010-08-15 | Thyssenkrupp Steel Europe Ag | FLAT PRODUCT MADE OF A METAL MATERIAL, IN PARTICULAR A STEEL MATERIAL, USE OF SUCH A FLAT PRODUCT AND ROLLER AND METHOD FOR PRODUCING SUCH FLAT PRODUCTS |
| CN101880485B (en) * | 2010-07-09 | 2012-02-29 | 重庆航利实业有限责任公司 | Rare earth sol modified composite zinc-aluminum low temperature sintering coating slurry |
| CN102585108A (en) * | 2012-01-17 | 2012-07-18 | 杭州日耀科技有限公司 | Polyester-modified organic fluorine-silicon acrylic resin and preparation method thereof as well as paint using resin |
| CN102627900A (en) * | 2012-03-20 | 2012-08-08 | 江苏同辉照明科技有限公司 | Preparation method of anti-ultraviolet paint |
| CN106977666A (en) * | 2017-04-27 | 2017-07-25 | 重庆三峡油漆股份有限公司 | Coating NC Nitroncellulose substitute and preparation method thereof |
| US12479945B2 (en) | 2020-07-29 | 2025-11-25 | Dow Global Technologies Llc | Crosslinked polymers of ethylene and monocyclic organosiloxane and process |
| CN113527977B (en) * | 2021-06-16 | 2022-10-11 | 广州大学 | Silicone-acrylic resin coating and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61236786A (en) * | 1985-04-11 | 1986-10-22 | Shin Etsu Chem Co Ltd | Cyclic siloxane and its manufacturing method |
| CN85101534A (en) * | 1984-06-22 | 1987-01-17 | N·V·菲利浦斯光灯制造厂 | Curable synthetic resin coating and method of making copolymer |
| JPH04261454A (en) * | 1991-02-15 | 1992-09-17 | Japan Synthetic Rubber Co Ltd | Polyorganosiloxane emulsion |
-
1997
- 1997-10-15 CN CN97106656A patent/CN1061364C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85101534A (en) * | 1984-06-22 | 1987-01-17 | N·V·菲利浦斯光灯制造厂 | Curable synthetic resin coating and method of making copolymer |
| JPS61236786A (en) * | 1985-04-11 | 1986-10-22 | Shin Etsu Chem Co Ltd | Cyclic siloxane and its manufacturing method |
| JPH04261454A (en) * | 1991-02-15 | 1992-09-17 | Japan Synthetic Rubber Co Ltd | Polyorganosiloxane emulsion |
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|---|---|
| CN1178819A (en) | 1998-04-15 |
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