CN101591503A - Solvent-free insulating paint and preparation method thereof - Google Patents
Solvent-free insulating paint and preparation method thereof Download PDFInfo
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- CN101591503A CN101591503A CNA2009101155954A CN200910115595A CN101591503A CN 101591503 A CN101591503 A CN 101591503A CN A2009101155954 A CNA2009101155954 A CN A2009101155954A CN 200910115595 A CN200910115595 A CN 200910115595A CN 101591503 A CN101591503 A CN 101591503A
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- China
- Prior art keywords
- solvent
- monomer
- sicl
- insulated paint
- free insulated
- Prior art date
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- Granted
Links
- 239000003973 paint Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000178 monomer Substances 0.000 claims abstract description 26
- 229920000548 poly(silane) polymer Polymers 0.000 claims abstract description 26
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 25
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 25
- 239000003960 organic solvent Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920005989 resin Polymers 0.000 claims abstract description 15
- 239000011347 resin Substances 0.000 claims abstract description 15
- 150000002118 epoxides Chemical class 0.000 claims abstract description 12
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 239000003999 initiator Substances 0.000 claims abstract description 5
- 239000012046 mixed solvent Substances 0.000 claims abstract description 5
- 150000002978 peroxides Chemical class 0.000 claims abstract description 5
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 30
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 8
- 239000003822 epoxy resin Substances 0.000 claims description 6
- -1 glycidyl ester Chemical class 0.000 claims description 6
- 229920000647 polyepoxide Polymers 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical group C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 4
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- 229920003986 novolac Polymers 0.000 claims description 3
- 229930185605 Bisphenol Natural products 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 125000003700 epoxy group Chemical group 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000011810 insulating material Substances 0.000 abstract description 3
- 238000010924 continuous production Methods 0.000 abstract description 2
- 239000003085 diluting agent Substances 0.000 abstract 1
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 7
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 4
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229940042795 hydrazides for tuberculosis treatment Drugs 0.000 description 2
- 239000004922 lacquer Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- KILURZWTCGSYRE-LNTINUHCSA-K (z)-4-bis[[(z)-4-oxopent-2-en-2-yl]oxy]alumanyloxypent-3-en-2-one Chemical compound CC(=O)\C=C(\C)O[Al](O\C(C)=C/C(C)=O)O\C(C)=C/C(C)=O KILURZWTCGSYRE-LNTINUHCSA-K 0.000 description 1
- OKIRBHVFJGXOIS-UHFFFAOYSA-N 1,2-di(propan-2-yl)benzene Chemical compound CC(C)C1=CC=CC=C1C(C)C OKIRBHVFJGXOIS-UHFFFAOYSA-N 0.000 description 1
- SEULWJSKCVACTH-UHFFFAOYSA-N 1-phenylimidazole Chemical compound C1=NC=CN1C1=CC=CC=C1 SEULWJSKCVACTH-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- 101000648997 Homo sapiens Tripartite motif-containing protein 44 Proteins 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 102100028017 Tripartite motif-containing protein 44 Human genes 0.000 description 1
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical class CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- XEHUIDSUOAGHBW-UHFFFAOYSA-N chromium;pentane-2,4-dione Chemical compound [Cr].CC(=O)CC(C)=O.CC(=O)CC(C)=O.CC(=O)CC(C)=O XEHUIDSUOAGHBW-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000011353 cycloaliphatic epoxy resin Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- JDVIRCVIXCMTPU-UHFFFAOYSA-N ethanamine;trifluoroborane Chemical compound CCN.FB(F)F JDVIRCVIXCMTPU-UHFFFAOYSA-N 0.000 description 1
- 229920000587 hyperbranched polymer Polymers 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005502 peroxidation Methods 0.000 description 1
- 150000004714 phosphonium salts Chemical class 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001073 sample cooling Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
Abstract
The invention relates to a solvent-free insulating paint and a preparation method thereof, wherein the insulating paint comprises a resin system and a peroxide initiator with the mass of 0.2-1.0% of the mass of the resin system, the resin system is formed by mixing vinyl hyperbranched polysilane with the viscosity of 1000-3000 at 25 ℃, an epoxide, a curing agent and a curing accelerator according to the mass ratio of 100: 5-200: 2-80: 0.05-5, and the vinyl hyperbranched polysilane is prepared by A3Monomer, A2The monomer and the end capping agent react in a mixed solvent of an organic solvent and water to prepare A3Monomer, A2The molar ratio of the monomer to the end-capping reagent is 1: 0.75-2: 0.5-2, and the use amounts of the organic solvent and the water are respectively A3Monomer, A20.5-8 times and 0.5-3 times of the total weight of the monomer and the end-capping agent. The solvent-free insulating paint disclosed by the invention does not contain an active diluent, the environmental pollution is small, the heat resistance and the dielectric property of the insulating material cured by the insulating paint are excellent, in addition, the production cost of the insulating paint is also lower, and the solvent-free insulating paint is suitable for industrial continuous production.
Description
Technical field
The present invention relates to a kind of solvent-free insulated paint and preparation method thereof.
Background technology
In the prior art, solvent-free insulated paint generally is made up of film-forming resin and reactive thinner etc., and reactive thinner can be cured reaction with film-forming resin.Most solvent-free insulated paint is in the process of film-forming, and reactive thinner has bigger volatilization and mass loss, and environment is polluted.In addition, in order to satisfy the demand of practical application, the resistance toheat of solvent-free insulated paint is also in urgent need to be improved.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, and a kind of solvent-free insulated paint that does not contain reactive thinner is provided.
The present invention also will provide a kind of preparation method of above-mentioned solvent-free insulated paint, and this method production cost is low.
For solving above technical problem, the following technical scheme that the present invention takes:
A kind of solvent-free insulated paint, it is that 0.2%～1.0% peroxide initiator of resin system quality is formed by resin system and quality, vinyl ultra-branching polysilane, epoxide, solidifying agent, the curing catalyst of viscosity between 1000～3000 mixed by mass ratio 100: 5～200: 2～80: 0.05～5 when wherein, resin system was by 25 ℃.
In preferred implementation, the content of epoxide group is more than or equal to 0.20mol/100g in the described epoxide, and it can be the public cycloaliphatic epoxy resin in bisphenol A type epoxy resin, bisphenol f type epoxy resin, novolac epoxy and other insullac field, aromatic epoxy resin or their modified resin.Epoxide can also be glycidyl ether such as methyl propenoic acid glycidyl ether or glycidyl ester such as methyl tetrahydro phthalic anhydride 2-glycidyl ester.
Described solidifying agent can be for being selected from one or more the mixture in anhydrides, boron amide class, borate ester, organic acid hydrazides class, Dyhard RU 100 and the derivative thereof.Curing catalyst can be one or more mixture of metal salt of organic carboxylic acid, acetyl acetone salt, boron amide class, imidazoles, triphenylphosphine and its phosphonium salt.
Described superoxide can be oxidation diisopropylbenzene(DIPB), benzoyl peroxide or their mixture.
Another technical scheme that the present invention takes is:
A kind of preparation method of above-mentioned solvent-free insulated paint comprises the steps:
(1), by A
3Monomer, A
2Monomer, end-capping reagent be prepared in reaction vinyl ultra-branching polysilane in the mixed solvent of organic solvent and water, A
3Monomer, A
2The mol ratio of monomer and end-capping reagent is 1: 0.75～2: 0.5～2, and the consumption of organic solvent and water is respectively A
3Monomer, A
2Monomer and end-capping reagent gross weight 0.5～8 times and 0.5～3 times;
(2), will mix by step (1) gained vinyl ultra-branching polysilane, epoxide, solidifying agent, curing catalyst and peroxide initiator by proportioning and promptly get solvent-free insulated paint.
Described A
3Monomer can be selected from CH
3(CH
2)
nSiCl
3, CH
2=CH (CH
2)
nSiCl
3, CH
2=CHCOOCH
2(CH
2)
mSiCl
3, C
6H
5SiCl
3, CH
3(CH
2) nSi (O (CH
2) mCH
3)
3, CH
2=CHCOOCH
2(CH
2)
mSi (O (CH
2) nCH
3)
3, CH
2=CH (CH
2) nSi (O (CH
2) mCH
3)
3And C
6H
5Si (O (CH
2) nCH
3)
3In one or more, wherein n, m are 0～4 integer;
Described A
2Monomer can be selected from (CH
3(CH
2)
k)
2SiCl
2, (CH
2=CH (CH
2)
k)
2SiCl
2, (CH
2=CHCOOCH
2(CH
2) i)
2SiCl
2, (Si (C
6H
5)
2O)
K+1, (C
6H
5)
2SiCl
2, (CH
3(CH
2)
k)
2Si (O (CH
2) iCH
3)
2, (CH
2=CH (CH
2)
k)
2Si (O (CH
2)
iCH
3)
2, (C
6H
5)
2Si (O (CH
2)
kCH
3)
2, (Si (CH
3)
2O)
K+1, (Si (CH
3) (CH
2=CH) O)
K+1, (Si (C
6H
5) (CH
2=CH) O)
K+1And (CH
2=CHCOOCH
2(CH
2)
i)
2Si (O (CH
2)
kCH
3)
2In one or more, wherein k, i are 0～4 integer;
Described end-capping reagent can be selected from (CH
3(CH
2)
j)
3SiCl, (CH
2=CH (CH
2)
j)
3SiCl, (C
6H
5)
3SiCl, (CH
2=CHCOOCH
2(CH
2) g)
3SiCl, (CH
3(CH
2) n)
3SiO (CH
2) gCH
3, (Si (C
6H
5)
3O)
2, (CH
2=CH (CH
2)
j)
3SiO (CH
2) gCH
3, (C
6H
5)
3SiO (CH
2)
jCH
3, (Si (CH
3)
3O)
2, (Si (CH
3)
2(CH
2=CH) O)
2And (Si (C
6H
5)
2(CH
2=CH) O)
2In one or more, wherein j, g are the integer between 0～4.
The further embodiment of step (1) is as follows: under 0～60 ℃ condition, the organic solvent that in the mixed solution of a part of organic solvent and water, slowly adds A3 monomer, A2 monomer, end-capping reagent and remainder, reacted 1～10 hour down in 10～100 ℃, finish reaction, be washed to neutrality, remove organic solvent and promptly get the vinyl ultra-branching polysilane.
Described organic solvent can be one or more the mixed solvent in benzene,toluene,xylene, ethanol, propyl alcohol, tetrahydrofuran (THF), hexanaphthene, the dioxane.
Because the enforcement of above technical scheme, the present invention compared with prior art has following advantage:
1, solvent-free insulated paint does not contain reactive thinner, has avoided the mass loss of the insullac that the volatilization of reactive thinner causes and to the pollution of environment;
2, after solvent-free insulated paint solidified, dielectric loss was little, second-order transition temperature is high and can reach 200 ℃ of temperature classifications;
3, the hyperbranched poly silane by preparation method's gained of the present invention not only has the distinctive good rheological of hyperbranched polymer, also have advantages such as viscosity is low, cost is low, good heat resistance, with epoxide jointly as the resinous principle of insullac, make insullac have good resistance toheat and dielectric properties;
4, preparation method of the present invention, raw materials cost is cheap, and is simple to operate, and production cost is low, is suitable for suitability for industrialized production.
Embodiment
The present invention will be described in detail below in conjunction with specific embodiment, but be not limited to these embodiment.
Embodiment 1
A kind of preparation method of vinyl ultra-branching polysilane, its process is: 300ml toluene and 400g water are added in the there-necked flask that prolong, agitator and thermometer are housed, at 0～10 ℃ following slow dropping 0.9mol (CH
3)
2SiCl
2, 0.8mol CH
3SiCl
3, 0.2mol CH
2=CHSiCl
3, 1.6mol (CH
3)
3The mixing solutions of SiCl and 500ml toluene, maintaining the temperature at 40～50 ℃ after dropwising reacted 8 hours down, be washed till neutrality with distilled water then, layering, obtaining viscosity after 100 ℃ of left and right sides vacuum steam organic solvent is the vinyl ultra-branching polysilane of 1150cp (25 ℃).
Embodiment 2
A kind of preparation method of vinyl ultra-branching polysilane, its process is: get 300ml dimethylbenzene and 250g water and be added in the there-necked flask that prolong, agitator and thermometer are housed, controlled temperature slowly drips 0.3mol (CH at 10～20 ℃
3)
2SiCl
2, 0.6mol (C
6H
5)
2SiCl
2, 0.4mol CH
3Si (OCH
3)
3, 0.6mol CH
2=CHSi (OCH
2CH
3)
3, 0.8mol (Si (CH
3)
3O)
2Mixing solutions with 500ml toluene, maintaining the temperature at 50～60 ℃ after dropwising reacted 6 hours down, be washed till neutrality with distilled water then, layering, obtaining viscosity after 90 ℃ of left and right sides vacuum steam organic solvent is the vinyl ultra-branching polysilane of 1050cp (25 ℃).
Embodiment 3
A kind of preparation method of vinyl ultra-branching polysilane, its process is: get 1000ml toluene, 100ml dioxane and 1000g water and be added in the there-necked flask that prolong, agitator and thermometer are housed, controlled temperature slowly drips 0.5mol (CH at 40～50 ℃
2=CH)
2SiCl
2, 0.4mol (Si (CH
3)
2O)
4, 0.2molC
6H
5SiCl
3, 0.4mol CH
2=CHSi (OCH
2CH
3)
3, 0.4mol CH
3SiCl
3, 0.3mol (Si (CH
3)
3O)
2, 0.6mol (C
6H
5)
3The mixing solutions of SiCl, 500ml toluene and 100ml tetrahydrofuran (THF), maintain the temperature at 90～100 ℃ of reactions 1 hour after dropwising, be washed till neutrality with distilled water then, layering, obtaining viscosity after 120 ℃ of left and right sides vacuum steam organic solvent is the vinyl ultra-branching polysilane of 1850cp (25 ℃).
Embodiment 4
A kind of preparation method of vinyl ultra-branching polysilane, its process is: get 700ml hexanaphthene, 200ml ethanol and 110g water and be added in the there-necked flask that prolong, agitator and thermometer are housed, controlled temperature slowly drips 0.75mol (CH at 10～20 ℃
2=CH)
2SiCl
2, 0.2mol C
6H
5SiCl
3, 0.8molCH
3SiCl
3, 1.0mol (C
6H
5)
3The mixing solutions of SiCl and 400ml toluene, maintain the temperature at 10～20 ℃ of reactions 10 hours after dropwising, be washed till neutrality with distilled water then, layering, obtaining viscosity after 110 ℃ of left and right sides vacuum steam organic solvent is the vinyl ultra-branching polysilane of 1150cp (25 ℃).
Embodiment 5
A kind of preparation method of vinyl ultra-branching polysilane, its process is: get 600ml benzene, 100ml propyl alcohol and 500g water and be added in the there-necked flask that prolong, agitator and thermometer are housed, 20～30 ℃ of controlled temperature slowly drip 0.8mol (CH
3)
2SiCl
2, 0.8mol (C
6H
5)
2SiCl
2, 0.4molCH
3Si (OCH
3)
3, 0.4mol CH
2=CHSi (OCH
2CH
3)
3, 0.8mol (Si (CH
3)
3O)
2Mixing solutions with 500ml toluene, maintain the temperature at 20～40 ℃ of reactions 5 hours after dropwising, be washed till neutrality, layering with distilled water then, obtaining viscosity after 90 ℃ of left and right sides vacuum steam organic solvent is the vinyl ultra-branching polysilane of 2350cp (25 ℃).
Embodiment 6
Solvent-free insulated paint according to present embodiment, form by resin system 138.5g and 0.3g dicumyl peroxide, wherein, resin system comprises vinyl ultra-branching polysilane, 25g bisphenol A type epoxy resin E51 (commercially available), 10g certain herbaceous plants with big flowers diacid two hydrazides (commercially available) and the 3.5g phenylimidazole (commercially available) of 100g embodiment 1 gained.
Above-mentioned solvent-free insulated paint is that each raw material and the dicumyl peroxide that will form resin system mix under room temperature all with promptly.
Embodiment 7
According to the solvent-free insulated paint of present embodiment, mix and get by vinyl ultra-branching polysilane, 5g novolac epoxy F51,2g boron trifluoride mono aminoethane, 0.05g aluminium acetylacetonate and the 0.5g peroxidation toluene of 100g embodiment 2 gained.
Embodiment 8
According to the solvent-free insulated paint of present embodiment, mix and get by vinyl ultra-branching polysilane, 100g methyl propenoic acid glycidyl ether, 40g methyl carbic anhydride, 5g triphenylphosphine and the 1.0g dicumyl peroxide of 100g embodiment 3 gained.
Embodiment 9
According to the solvent-free insulated paint of present embodiment, by vinyl ultra-branching polysilane, 30gE51,10gF51, the 9g 594 of 100g embodiment 4 gained
#(commercially available amine curing agent), 1.1g cobalt iso-octoate and 0.2g dicumyl peroxide mix and get.
Embodiment 10
According to the solvent-free insulated paint of present embodiment, mix and get by vinyl ultra-branching polysilane, 200g methyl tetrahydro phthalic anhydride 2-glycidyl ester, 80g methyl hexahydrophthalic anhydride, 2g chromium acetylacetonate and the 1.0g dicumyl peroxide of 100g embodiment 5 gained.
Viscosity and stability under the room temperature of the solvent-free insulated paint of embodiment 6～10 gained are tested, and the stability of insullac is meant insullac 50 ℃ of waters bath with thermostatic control after 96 hours, the multiple that viscosity increases.The results are shown in Table 1.In addition, the performance of the insulating material after the solvent-free insulated paint curing is tested, specific as follows:
1., the solvent-free insulated paint with embodiment 6～10 gained is cast in the mould respectively, 150 ℃ solidify 2 hours, 190 ℃ and solidify 2 hours, 210 ℃ curing 2 hours, take out the sample cooling back demoulding, room temperature is placed the performance of difference test material after 12 hours, and wherein: the tensile strength of material is tested according to ASTM D638-82a; The bending property of material is tested according to ASTM D790M-92 standard; The shock strength of material is tested according to ASTM D256-81 standard; The thermal characteristics of material (Tg) test by DSC according to ASTM3418-82, and the temperature rise rate of test is 10 ℃/min by second-order transition temperature; The heat resisting temperature of insulating material (or heat-resistance index) is measured by TGA according to JB/T2624-79 standard secant method, and the temperature rise rate of test is 5 ℃/min.
2., take by weighing the solvent-free insulated paint 12g of embodiment 6～10 in lacquer cake curing mold, solidify 2 hours, 190 ℃ at 150 ℃ respectively and solidify 2 hours, 210 ℃ curing 2 hours, then the dielectric loss factor and the voltage breakdown of coating with lacquer cake according to the requirement test of standard GB/T1409-2006.
The result of above-mentioned performance test specifically sees the table 1 of the 6th page in specification sheets.
The performance of the solvent-free insulated paint of table 1 embodiment 6～10 with and the performance index of solidifying the back material
As seen from Table 1, solvent-free insulated paint of the present invention has characteristics such as low volatilization, dielectric loss are low, excellent heat stability.In addition, this preparation method's technology is simple, and the material cost of employing is cheap, helps the industrialization continuous production.
More than the present invention has been done detailed description; its purpose is to allow the personage that is familiar with this art can understand content of the present invention and is implemented; can not limit protection scope of the present invention with this; all equivalences of doing according to spirit of the present invention change or modify, and all should be encompassed in protection scope of the present invention.
Claims (10)
1, a kind of solvent-free insulated paint, it is characterized in that: insullac is that 0.2%～1.0% peroxide initiator of resin system quality is formed by resin system and quality, vinyl ultra-branching polysilane, epoxide, solidifying agent, the curing catalyst of viscosity between 1000～3000 mixed by mass ratio 100: 5～200: 2～80: 0.05～5 when wherein, resin system was by 25 ℃.
2, solvent-free insulated paint according to claim 1 is characterized in that: in the described epoxide, epoxy group content is more than or equal to 0.20mol/100g.
3, solvent-free insulated paint according to claim 1 and 2 is characterized in that: described epoxide is selected from one or more the mixture in bisphenol A type epoxy resin, bisphenol f type epoxy resin, the novolac epoxy.
4, solvent-free insulated paint according to claim 1 and 2 is characterized in that: described epoxide is glycidyl ether or glycidyl ester or their mixture.
5, the preparation method of the described solvent-free insulated paint of a kind of claim 1 is characterized in that: comprise the steps:
(1), by A
3Monomer, A
2Monomer and end-capping reagent be prepared in reaction vinyl ultra-branching polysilane in the mixed solvent of organic solvent and water, A
3Monomer, A
2The mol ratio of monomer and end-capping reagent is 1: 0.75～2: 0.5～2, and the consumption of organic solvent and water is respectively A
3Monomer, A
2Monomer and end-capping reagent gross weight 0.5～8 times and 0.5～3 times;
(2), will mix by step (1) gained vinyl ultra-branching polysilane, epoxide, solidifying agent, curing catalyst and peroxide initiator by proportioning and promptly get solvent-free insulated paint.
6, the preparation method of solvent-free insulated paint according to claim 5 is characterized in that: described A
3Monomer is selected from CH
3(CH
2) nSiCl
3, CH
2=CH (CH
2) nSiCl
3, CH
2=CHCOOCH
2(CH
2) mSiCl
3, C
6H
5SiCl
3, CH
3(CH
2) nSi (O (CH
2) mCH
3)
3, CH
2=CHCOOCH
2(CH
2) mSi (O (CH
2) nCH
3)
3, C
6H
5Si (O (CH
2) nCH
3)
3And CH
2=CH (CH
2) nSi (O (CH
2) mCH
3)
3One or more, wherein n, m are 0～4 integer.
7, the preparation method of solvent-free insulated paint according to claim 5 is characterized in that: described A
2Monomer is selected from (CH
3(CH
2) k)
2SiCl
2, (CH
2=CH (CH
2)
k)
2SiCl
2, (CH
2=CHCOOCH
2(CH
2)
i)
2SiCl
2, (Si (C
6H
5)
2O)
K+1, (C
6H
5)
2SiCl
2, (CH
3(CH
2)
k)
2Si (O (CH
2)
iCH
3)
2, (CH
2=CH (CH
2)
k)
2Si (O (CH
2)
iCH
3)
2, (C
6H
5)
2Si (O (CH
2)
kCH
3)
2, (Si (CH
3)
2O)
K+1, (Si (CH
3) (CH
2=CH) O)
K+1, (Si (C
6H
5) (CH
2=CH) O)
K+1And (CH
2=CHCOOCH
2(CH
2)
i)
2Si (O (CH
2)
kCH
3)
2In one or more, wherein k, i are 0～4 integer.
8, the preparation method of solvent-free insulated paint according to claim 5 is characterized in that: described end-capping reagent is selected from (CH
3(CH
2)
j)
3SiCl, (CH
2=CH (CH
2)
j)
3SiCl, (C
6H
5)
3SiCl, (CH
2=CHCOOCH
2(CH
2) g)
3SiCl, (CH
3(CH
2) n)
3SiO (CH
2) gCH
3, (Si (C
6H
5)
3O)
2, (CH
2=CH (CH
2)
j)
3SiO (CH
2) gCH
3, (C
6H
5)
3SiO (CH
2)
jCH
3, (Si (CH
3)
3O)
2, (Si (CH
3)
2(CH
2=CH) O)
2And (Si (C
6H
5)
2(CH
2=CH) O)
2In one or more, wherein j, g are the integer between 0～4.
9, the preparation method of solvent-free insulated paint according to claim 5 is characterized in that: in the step (1), the reaction detailed process is: under 0～60 ℃ condition, slowly add A in the mixed solution of a part of organic solvent and water
3Monomer, A
2The organic solvent of monomer, end-capping reagent and remainder reacted 1～10 hour down in 10～100 ℃, finished reaction, was washed to neutrality, removed organic solvent and obtained described vinyl ultra-branching polysilane.
10, the preparation method of solvent-free insulated paint according to claim 9 is characterized in that: described organic solvent is one or more the mixed solvent in benzene,toluene,xylene, ethanol, propyl alcohol, tetrahydrofuran (THF), hexanaphthene, the dioxane.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101155954A CN101591503B (en) | 2009-06-23 | 2009-06-23 | Solvent-free insulating paint and preparation method thereof |
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| CN101591503B CN101591503B (en) | 2011-08-10 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103146304A (en) * | 2013-03-20 | 2013-06-12 | 苏州太湖电工新材料股份有限公司 | Solventless insulating paint |
| CN109013567A (en) * | 2018-07-18 | 2018-12-18 | 中车兰州机车有限公司 | Method for cleaning insulating paint sample |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2403722A (en) * | 2003-07-11 | 2005-01-12 | Sun Chemical Ltd | Process for the preparation of a low viscosity, hyperbranched polymer |
| CN101077897A (en) * | 2007-06-29 | 2007-11-28 | 西北工业大学 | Super-branching silicon-base macromolecule optical initiator and preparation method thereof |
-
2009
- 2009-06-23 CN CN2009101155954A patent/CN101591503B/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103146304A (en) * | 2013-03-20 | 2013-06-12 | 苏州太湖电工新材料股份有限公司 | Solventless insulating paint |
| CN103146304B (en) * | 2013-03-20 | 2015-06-03 | 苏州太湖电工新材料股份有限公司 | Solventless insulating paint |
| CN109013567A (en) * | 2018-07-18 | 2018-12-18 | 中车兰州机车有限公司 | Method for cleaning insulating paint sample |
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| Publication number | Publication date |
|---|---|
| CN101591503B (en) | 2011-08-10 |
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Owner name: WUJIANG TAIHU INSULATING MATERIAL CO., LTD. Free format text: FORMER NAME: WUJIANG TAIHU INSULATING MATERIAL FACTORY Owner name: SUZHOU TAIHU ELECTRIC NEW MATERIAL CO. LTD. Free format text: FORMER NAME: WUJIANG TAIHU INSULATING MATERIAL CO., LTD. |
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Address after: Yu Cai Lu Beishe town 215214 Wujiang City, Jiangsu province FENHU Economic Development Zone No. 36 Patentee after: SUZHOU TAIHU ELECTRIC ADVANCED MATERIAL Co.,Ltd. Address before: Yu Cai Lu Beishe town 215214 Wujiang City, Jiangsu province FENHU Economic Development Zone No. 36 Patentee before: Wujiang Taihu Insulation Materials Co.,Ltd. Address after: Yu Cai Lu Beishe town 215214 Wujiang City, Jiangsu province FENHU Economic Development Zone No. 36 Patentee after: Wujiang Taihu Insulation Materials Co.,Ltd. Address before: Yu Cai Lu Beishe town 215214 Wujiang City, Jiangsu province FENHU Economic Development Zone No. 36 Patentee before: Wujiang Taihu Insulating Material Factory |