CN104910807A - Organosilicon ingredient toughened methyl silicone resin and preparation method thereof - Google Patents
Organosilicon ingredient toughened methyl silicone resin and preparation method thereof Download PDFInfo
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Abstract
The invention relates to organosilicon component toughened methyl silicone resin and a preparation method thereof. The resin contains the ingredients in gram by weight: 2-30g of organosilicon component, 20-40g of deionized water or acidic silica sol, 30-80g of methyl trialkoxysilane, 0-30g of tetra-alkoxysilane, 0-15g of phenyl trialkoxysilane, 0-10g of dimethyl dialkoxysilane, 0-10g of silane coupling agent, 0-10g of acidic catalyst, 0.02-0.5g of curing agent, 0-15g of ethanol or isopropanol and 0-0.5g of leveling agent, wherein the organosilicon component is synthesized from terminal-hydrogen silicone oil and vinyl siloxane in the presence of a catalyst. The resin disclosed by the invention has the biggest advantage that a film formed material is endowed with very good flexibility, wet-heat resistance and high-temperature resistance while high hardness for the methylsilicone resin is maintained. The preparation method is simple, is good in environmental friendliness and facilitates large-scale production. The surface protection effect for hard or flexible transparent and opaque plastic parts is good.
Description
Technical field
The present invention relates to toughness reinforcing methyl silicon resin of a kind of organosilicon composition and preparation method thereof.Be specially adapted to hard or flexible and transparent, opaque plastics part surfacecti proteon and for metallic surface, the protection of stone material efflorescence prevention.
Background technology
Methyl silicon resin is a kind of by MeSiO
1.5, Me
2siO, Me
3siO
0.5and SiO
2link set is combined into the silicone product of main body.The advantages such as this product has hard, clear, and high temperature weightlessness is few, extensively should in wear-resisting Hardening coating, high temperature resistant mica-bond agent and resistance coating etc.But because methyl silicon resin matter is crisp, easily ftracture in the curing process, the film formed, when external environment constantly changes, also usually there will be crackle, even peels off from base material.These shortcomings greatly limit the application of methyl silicon resin, and therefore, plasticizing methyl silicone resin just seems particularly important.Li Buchun (organosilicon material and application, 1999,3,4-7) carry out plasticizing methyl silicone resin with short-chain hydroxyl silicone oil and dimethyldichlorosilane(DMCS), United States Patent (USP) (US 4368235) it is also proposed similar way and improves the anti-cracking performance of methyl silicon resin when solidifying.But the toughening effect that this method can reach is extremely limited.When strong cured system such as use Tetramethylammonium hydroxide, TBAH etc., paint film still easily produces crazing in the curing process, and paint film bends or when being subject to clashing into, also easily bursts.CN 103201318A discloses a kind of method preparing resin-linear organosilicon oxygen alkane segmented copolymer, can be used for improving the elongation at break of methyl silicon resin and fracture toughness property.But when improving the toughness of methyl silicon resin in this way, the pencil hardness of paint film also greatly reduces, and the transparency of paint film also receives impact thereupon.
Summary of the invention
First object of the present invention is: provide a kind of and take into account the methyl silicon resin that hardness is high, snappiness good, resistant to elevated temperatures organosilicon composition is toughness reinforcing; it is crisp that this resin overcomes existing methyl silicon resin matter; easily ftracture in the curing process; the film formed; when external environment constantly changes, also usually there will be the shortcoming of crackle.
The technical scheme realizing the present invention's first object is: the methyl silicon resin that a kind of organosilicon composition is toughness reinforcing, it is characterized in that, it is made up of following component, gram meter by weight, each amounts of components is as follows: organosilicon composition 2 ~ 30, deionized water or acidic silicasol 20 ~ 40, methyl trialkoxysilane 30 ~ 80, tetraalkoxysilane 0 ~ 30, phenyl trialkoxysilane 0 ~ 15, dimethyldialkylammonium TMOS 0 ~ 10, silane coupling agent 0 ~ 10, an acidic catalyst 0 ~ 10, solidifying agent 0.02 ~ 0.5, ethanol or Virahol 0 ~ 15, flow agent 0 ~ 0.5;
The synthesis under platinum catalyst exists by end hydrogen silicone oil and vinylsiloxane of described organosilicon composition, wherein, the hydrogen content of end hydrogen silicone oil used is at 0.1wt% ~ 1.5wt%; Vinylsiloxane is one or more in vinyltriethoxysilane, vinyltrimethoxy silane, vinyl methyl diethoxy silane, vinyl methyl dimethoxysilane;
Described silane coupling agent is the one in γ-(2,3-propylene oxide) propyl trimethoxy silicane, γ-(2,3-propylene oxide) propyl-triethoxysilicane, gamma-amino propyl trimethoxy, γ aminopropyltriethoxy silane;
Described solidifying agent is aluminium acetylacetonate, dibutyltin dilaurate, Tetramethylammonium hydroxide, TBAH, Guanidinium hydrochloride, 1, one or more in 8-diazabicylo 11 carbon-7-alkene, or be the hydrochloride, 1 of the hydrochloride of Tetramethylammonium hydroxide, TBAH, one or more in the hydrochloride of 8-diazabicylo 11 carbon-7-alkene, or be one or more in the acetate of the acetate of Tetramethylammonium hydroxide, the acetate of TBAH, 1,8-diazabicylo 11 carbon-7-alkene;
The particle diameter of described acidic silicasol is 5 ~ 100nm.
The methyl silicon resin that above-mentioned organosilicon composition is toughness reinforcing, described in it, the concrete synthetic method of organosilicon composition is as follows:
Reaction vessel is placed in water-bath, add vinylsiloxane monomer and platinum catalyst successively, be uniformly mixed, then being added drop-wise to hydrogen content is in the end hydrogen silicone oil of 0.1wt% ~ 1.5wt%, controls temperature≤80 DEG C of reaction solution, dropwises, continue reaction at 80 DEG C and namely obtain organosilicon composition in 2 hours, save backup, wherein, the add-on of vinylsiloxane is 1 ~ 1.05 with the mol ratio of SiH group in end hydrogen silicone oil; Platinum catalyst consumption is 0.02% ~ 0.06% of vinylsiloxane consumption.
The methyl silicon resin that above-mentioned organosilicon composition is toughness reinforcing, methyl trialkoxysilane described in it is methyltrimethoxy silane or Union carbide A-162; Tetraalkoxysilane is tetramethoxy-silicane or tetraethoxysilane; Phenyl trialkoxysilane is phenyltrimethoxysila,e or phenyl triethoxysilane; Dimethyldialkylammonium TMOS is dimethyldimethoxysil,ne or dimethyldiethoxysilane.
The methyl silicon resin that above-mentioned organosilicon composition is toughness reinforcing, acid catalyst described in it is hydrochloric acid, acetic acid or sulfuric acid.
The methyl silicon resin that above-mentioned organosilicon composition is toughness reinforcing, the filming condition of the methyl silicon resin that organosilicon composition described in it is toughness reinforcing is: at 40 DEG C after predrying 10min, more namely solidification 0.3 ~ 2h forms organosilicon composition plasticizing methyl silicone resin film at 80 ~ 140 DEG C.
Second object of the present invention is: provide a kind of simple to operate and be easy to the toughness reinforcing methyl silicon resin preparation method of the organosilicon composition of large-scale production.
The technical scheme realizing the present invention's second object is: the preparation method of the methyl silicon resin that a kind of above-mentioned organosilicon composition is toughness reinforcing, is characterized in that,
Method one is that organosilicon composition and siloxanyl monomers are hydrolyzed prepolymerization in same reaction vessel, and the hydrolysis prepolymerization product obtained mixes with solidifying agent, ethanol or Virahol, flow agent and namely obtains the toughness reinforcing methyl silicon resin of organosilicon composition;
Method two is that organosilicon composition and siloxanyl monomers are hydrolyzed respectively prepolymerization in two reaction vessels, namely two kinds that obtain respectively be hydrolyzed prepolymerization product: the hydrolysis prepolymerization product of organosilicon composition and the hydrolysis prepolymerization product of siloxanyl monomers, mix with solidifying agent, ethanol or Virahol, flow agent and namely obtain the toughness reinforcing methyl silicon resin of organosilicon composition.
The preparation method of the methyl silicon resin that above-mentioned organosilicon composition is toughness reinforcing, described in it, the concrete operation step of method one is as follows:
1. prepare each component according to the formula of claim 1, save backup;
2. prepare organosilicon composition according to method described in claim 2, save backup;
3. in reaction vessel, add deionized water or acidic silicasol that 1. step prepare successively, an acidic catalyst, methyl trialkoxysilane, tetraalkoxysilane, phenyl trialkoxysilane, dimethyldialkylammonium TMOS, silane coupling agent, stirred at ambient temperature mixing 1 ~ 4h, then the organosilicon composition 2 ~ 30 grams that 2. step obtains is added, again at the hydrolysis prepolymerization product that 60 ~ 80 DEG C of stirring reaction 1 ~ 12h obtain, add the solidifying agent that 1. step prepares wherein, ethanol or Virahol, after flow agent, stir to mix for 3 ~ 5 minutes and be the toughness reinforcing methyl silicon resin of organosilicon composition.
The preparation method of the methyl silicon resin that above-mentioned organosilicon composition is toughness reinforcing, described in it, the concrete operation step of method two is as follows:
1. each component is prepared according to the formula of claim 1;
2. prepare organosilicon composition according to method described in claim 5, save backup;
3. in reaction vessel, first adding 0 ~ 30 gram of ethanol or Virahol and 2 ~ 6 grams of pH value is the aqueous acetic acid of 4 ~ 5, then the organosilicon composition 2 ~ 30 grams that 2. step obtains is added, at room temperature stir after 2 hours, reaction 2h is continued, the hydrolysis prepolymerization product of obtained organosilicon composition at 80 DEG C; In another reaction vessel, add deionized water or acidic silicasol, an acidic catalyst, methyl trialkoxysilane, tetraalkoxysilane, phenyl trialkoxysilane, dimethyldialkylammonium TMOS, silane coupling agent that 1. step prepare successively, stirred at ambient temperature 1 ~ 4h, obtains the hydrolysis prepolymerization product of siloxanyl monomers at 60 ~ 80 DEG C of stirring reaction 1 ~ 12h;
4. in mixing vessel, add the hydrolysis prepolymerization product of the siloxanyl monomers that 3. the hydrolysis prepolymerization product of the organosilicon composition that 3. step obtains and step obtain, stir 3 ~ 5 minutes, the solidifying agent then 1. prepared with step, flow agent stir to mix for 3 ~ 5 minutes and namely obtain the toughness reinforcing methyl silicon resin of organosilicon composition.
The preparation method of the methyl silicon resin that above-mentioned organosilicon composition is toughness reinforcing, methyl trialkoxysilane described in it is methyltrimethoxy silane or Union carbide A-162; Tetraalkoxysilane is tetramethoxy-silicane or tetraethoxysilane; Phenyl trialkoxysilane is phenyltrimethoxysila,e or phenyl triethoxysilane; Dimethyldialkylammonium TMOS is dimethyldimethoxysil,ne or dimethyldiethoxysilane.
The preparation method of the methyl silicon resin that above-mentioned organosilicon composition is toughness reinforcing, acid catalyst described in it is hydrochloric acid, acetic acid or sulfuric acid.
Technique effect of the present invention is: the toughness reinforcing methyl silicon resin of the organosilicon composition of technical solution of the present invention is compared with existing toughness reinforcing methyl silicon resin, maximum advantage is because introduce special organosilicon composition in resin of the present invention, make resin of the present invention while maintenance methyl silicon resin high rigidity and heatproof, the material given after film forming has good snappiness.Why the film of the methyl silicon resin formation that organosilicon composition is toughness reinforcing has so superior performance is because the coating formed has the combined feature of soft or hard on microcosmic level.Hard polysiloxane ensure that high rigidity and the scratch-resistant performance of paint film in the coating, and organosilicon component wherein effectively can absorb the string stress that methyl silicon resin produces when solidifying, thus avoid the cracking behaviors of methyl silicon resin when fast setting.Film when cured impacted or bending time, the effect that these toughness reinforcing points can play again buffering can avoid the explosion of film.In addition, because organosilicon composition is to hold hydrogen silicone oil and vinylsiloxane for Material synthesis, therefore ensure that the film of resin formation of the present invention has good wet-heat resisting, resistance to elevated temperatures.Special organosilicon composition and matrix resin have good consistency, and ensure that the coating formed has high transparent, this makes this resin have special advantage in the process of Transparent Parts stiffened; In addition; the preparation technology of the methyl silicon resin that organosilicon composition of the present invention is toughness reinforcing is simple; substantially not with an organic solvent; therefore; VOC content is low, good environmental protection, easy scale operation; in the surfacecti proteon of hard or flexible and transparent, opaque plastics part, and for metallic surface, stone material efflorescence prevention protection aspect, there is very high using value.
Table 1 provides the character difference of methyl silicon resin of the present invention and existing methyl silicon resin.
Embodiment
Below in conjunction with embodiment, the present invention is described further, but is not limited to this.
Embodiment raw materials is unless otherwise indicated commercially available industrial goods, buys by commercial channel.
The platinum catalyst used in embodiment is Speier catalyzer, its H
2ptCl
6.6H
2o content is 0.5wt%, also can adopt Karstedt catalyzer etc.; The acidic silicasol that the acidic silicasol used is produced for Suzhou Nano Dispersions Co., Ltd., its solids content is 30wt%, and silicon sol particle diameter is 12nm, also can adopt the Ludox series acidic silicasol of U.S.'s Grace chemical production; The BYK-331 that the flow agent used is German BYK company;
The pH value used in embodiment be 4 ~ 5 aqueous acetic acid be by acetic acid and deionized water according to make its pH value be 4 ~ 5 ratio mix, stir or vibration 5 ~ 10 minutes;
The method detecting film performance employing is as follows:
Hardness is pressed GB/T1730-1993 method and is measured; Sticking power is pressed GB/T9286-1998 method and is measured; Snappiness is pressed GB/T1731-1993 method and is measured;
Embodiment 1 prepares the toughness reinforcing methyl silicon resin of organosilicon composition
1. prepare each component following: 15g deionization, 1g an acidic catalyst acetic acid, 40g methyltrimethoxy silane, 5g phenyltrimethoxysila,e, 0.1g solidifying agent Tetramethylammonium hydroxide, 0.1g flow agent, saves backup;
2. the round-bottomed flask of 250mL is placed in water-bath, add 24 grams of vinyl three ethoxy siloxanes and 1.44 grams of Speier catalyzer successively, stir in room-temperature water bath, then drip the end hydrogen silicone oil that 80 grams of hydrogen contents are 0.1wt%, control temperature≤80 DEG C of reaction solution, dropwise, continue again to stir 2h, then continue reaction at 80 DEG C and namely obtain organosilicon composition in 2 hours, save backup, wherein, the add-on of vinylsiloxane is 1:1 with the mol ratio of SiH group in end hydrogen silicone oil; Platinum catalyst consumption is the 0.03wt% of vinylsiloxane consumption,
The 2. involved chemical equation of step is as follows:
3. in the round-bottomed flask of 100ml, add deionization, an acidic catalyst acetic acid, methyltrimethoxy silane, phenyltrimethoxysila,e that 1. step prepares successively, after being uniformly mixed 4h at 25 DEG C, add the organosilicon composition that 2. 2g step obtains, obtain being hydrolyzed prepolymerization product at 80 DEG C of stirring reaction 2h again, after adding solidifying agent Tetramethylammonium hydroxide that 1. step prepare, flow agent wherein, stir to mix for 5 minutes and be the toughness reinforcing methyl silicon resin of organosilicon composition.
Methyl silicon resin toughness reinforcing for organosilicon composition obtained for embodiment 1 is coated on tinplate, film thickness monitoring is < 50 μm, at 40 DEG C after predrying 10min, solidify 1 hour at 120 DEG C again, the hardness 5H of gained film, sticking power 0 grade, paint film, without cracking, bends by 1mm.
Embodiment 2 prepares the toughness reinforcing methyl silicon resin of organosilicon composition
1. each component following is prepared: 14.8g acidic silicasol silicon, 1.2g an acidic catalyst acetic acid, 46g Union carbide A-162,5g phenyltrimethoxysila,e, 1.2g silane coupling agent γ-(2,3-propylene oxide) propyl trimethoxy silicane, 0.1g solidifying agent Tetramethylammonium hydroxide, 0.1g flow agent, saves backup;
2. obtain organosilicon composition by embodiment 1 same procedure, save backup;
3. in the round-bottomed flask of 100ml, add acidic silicasol silicon, an acidic catalyst acetic acid, Union carbide A-162, phenyltrimethoxysila,e, silane coupling agent that 1. step prepares successively, after being at room temperature uniformly mixed 4h, add the organosilicon composition that 2. 4g step obtains, obtain being hydrolyzed prepolymerization product at 80 DEG C of stirring reaction 2h again, after adding solidifying agent Tetramethylammonium hydroxide that 1. step prepare, flow agent wherein, stir to mix for 3 minutes and be the toughness reinforcing methyl silicon resin of organosilicon composition.
Methyl silicon resin toughness reinforcing for organosilicon composition obtained for embodiment 2 is coated on polycarbonate plate, film thickness monitoring is < 10 μm, at 40 DEG C after predrying 10min, solidify 1 hour at 120 DEG C again, the hardness 3H of gained film, sticking power 0 grade, has certain anti-micro-curved ability.
Embodiment 3 prepares the toughness reinforcing methyl silicon resin of organosilicon composition
1. each component is prepared: 14.8g acidic silicasol silicon, median size is 12nm, 1.2g an acidic catalyst acetic acid, 46g Union carbide A-162,5g phenyltrimethoxysila,e, 1.2g coupling agent γ-(2,3-propylene oxide) propyl trimethoxy silicane, 40mg solidifying agent aluminium acetylacetonate, 0.1g flow agent, saves backup;
2. obtain organosilicon composition by embodiment 1 same procedure, save backup;
3. in the round-bottomed flask of 100ml, first add 20g ethanol and 2gpH value is the aqueous acetic acid of 4 ~ 5, then add the organosilicon composition that 2. 2g step obtains, at room temperature stir after 2 hours, reaction 2h is continued, the hydrolysis prepolymerization product of obtained organosilicon composition at 80 DEG C; In the round-bottomed flask of another 100ml, add acidic silicasol, an acidic catalyst, Union carbide A-162, phenyltrimethoxysila,e and silane coupling agent that 1. step prepares successively, after stirred at ambient temperature 4h, obtain the hydrolysis prepolymerization product of siloxanyl monomers at 80 DEG C of stirring reaction 2h;
4. in mixing vessel, add the hydrolysis prepolymerization product of the siloxanyl monomers that 3. the hydrolysis prepolymerization product of the organosilicon composition that 3. step obtains and step obtain, stir 5 minutes, the solidifying agent then 1. prepared with step, flow agent stir to mix for 5 minutes and namely obtain the toughness reinforcing methyl silicon resin of organosilicon composition.
Be coated on tinplate by methyl silicon resin toughness reinforcing for organosilicon composition obtained for embodiment 3, film thickness monitoring is < 10 μm, at 40 DEG C after predrying 10min, solidify 1 hour at 120 DEG C again, the hardness 5H of gained film, film, without cracking, has certain anti-micro-curved ability.
Claims (10)
1. the methyl silicon resin that organosilicon composition is toughness reinforcing, is characterized in that, it is made up of following component, gram meter by weight, each amounts of components is as follows: organosilicon composition 2 ~ 30, deionized water or acidic silicasol 20 ~ 40, methyl trialkoxysilane 30 ~ 80, tetraalkoxysilane 0 ~ 30, phenyl trialkoxysilane 0 ~ 15, dimethyldialkylammonium TMOS 0 ~ 10, silane coupling agent 0 ~ 10, an acidic catalyst 0 ~ 10, solidifying agent 0.02 ~ 0.5, ethanol or Virahol 0 ~ 15, flow agent 0 ~ 0.5;
The synthesis under platinum catalyst exists by end hydrogen silicone oil and vinylsiloxane of described organosilicon composition, wherein, the hydrogen content of end hydrogen silicone oil used is at 0.1wt% ~ 1.5wt%; Vinylsiloxane is one or more in vinyltriethoxysilane, vinyltrimethoxy silane, vinyl methyl diethoxy silane, vinyl methyl dimethoxysilane;
Described silane coupling agent is the one in γ-(2,3-propylene oxide) propyl trimethoxy silicane, γ-(2,3-propylene oxide) propyl-triethoxysilicane, gamma-amino propyl trimethoxy, γ aminopropyltriethoxy silane;
Described solidifying agent is aluminium acetylacetonate, dibutyltin dilaurate, Tetramethylammonium hydroxide, TBAH, Guanidinium hydrochloride, 1, one or more in 8-diazabicylo 11 carbon-7-alkene, or be the hydrochloride, 1 of the hydrochloride of Tetramethylammonium hydroxide, TBAH, one or more in the hydrochloride of 8-diazabicylo 11 carbon-7-alkene, or be one or more in the acetate of the acetate of Tetramethylammonium hydroxide, the acetate of TBAH, 1,8-diazabicylo 11 carbon-7-alkene;
The particle diameter of described acidic silicasol is 5 ~ 100nm.
2. the methyl silicon resin that organosilicon composition according to claim 1 is toughness reinforcing, is characterized in that, the concrete synthetic method of described organosilicon composition is as follows:
Reaction vessel is placed in water-bath, add vinylsiloxane monomer and platinum catalyst successively, be uniformly mixed, then being added drop-wise to hydrogen content is in the end hydrogen silicone oil of 0.1wt% ~ 1.5wt%, controls temperature≤80 DEG C of reaction solution, dropwises, continue reaction at 80 DEG C and namely obtain organosilicon composition in 2 hours, save backup, wherein, the add-on of vinylsiloxane is 1 ~ 1.05 with the mol ratio of SiH group in end hydrogen silicone oil; Platinum catalyst consumption is 0.02% ~ 0.06% of vinylsiloxane consumption.
3. the methyl silicon resin that organosilicon composition according to claim 1 is toughness reinforcing, is characterized in that, described methyl trialkoxysilane is methyltrimethoxy silane or Union carbide A-162; Tetraalkoxysilane is tetramethoxy-silicane or tetraethoxysilane; Phenyl trialkoxysilane is phenyltrimethoxysila,e or phenyl triethoxysilane; Dimethyldialkylammonium TMOS is dimethyldimethoxysil,ne or dimethyldiethoxysilane.
4. the methyl silicon resin that organosilicon composition according to claim 1 is toughness reinforcing, is characterized in that, described acid catalyst is hydrochloric acid, acetic acid or sulfuric acid.
5. the methyl silicon resin that organosilicon composition according to claim 1 is toughness reinforcing, it is characterized in that, the filming condition of the methyl silicon resin that described organosilicon composition is toughness reinforcing is: at 40 DEG C after predrying 10min, more namely solidification 0.3 ~ 2h forms organosilicon composition plasticizing methyl silicone resin film at 80 ~ 140 DEG C.
6. a preparation method for the methyl silicon resin that the organosilicon composition that one of Claims 1 to 5 is described is toughness reinforcing, is characterized in that,
Method one is that organosilicon composition and siloxanyl monomers are hydrolyzed prepolymerization in same reaction vessel, and the hydrolysis prepolymerization product obtained mixes with solidifying agent, ethanol or Virahol, flow agent and namely obtains the toughness reinforcing methyl silicon resin of organosilicon composition;
Method two is that organosilicon composition and siloxanyl monomers are hydrolyzed respectively prepolymerization in two reaction vessels, namely two kinds that obtain respectively be hydrolyzed prepolymerization product: the hydrolysis prepolymerization product of organosilicon composition and the hydrolysis prepolymerization product of siloxanyl monomers, mix with solidifying agent, ethanol or Virahol, flow agent and namely obtain the toughness reinforcing methyl silicon resin of organosilicon composition.
7. the preparation method of the methyl silicon resin that organosilicon composition according to claim 6 is toughness reinforcing, is characterized in that, the concrete operation step of described method one is as follows:
1. prepare each component according to the formula of claim 1, save backup;
2. prepare organosilicon composition according to method described in claim 2, save backup;
3. in reaction vessel, add deionized water or acidic silicasol that 1. step prepare successively, an acidic catalyst, methyl trialkoxysilane, tetraalkoxysilane, phenyl trialkoxysilane, dimethyldialkylammonium TMOS, silane coupling agent, stirred at ambient temperature mixing 1 ~ 4h, then the organosilicon composition 2 ~ 30 grams that 2. step obtains is added, again at the hydrolysis prepolymerization product that 60 ~ 80 DEG C of stirring reaction 1 ~ 12h obtain, add the solidifying agent that 1. step prepares wherein, ethanol or Virahol, after flow agent, stir and within 3 ~ 5 minutes, be the toughness reinforcing methyl silicon resin of organosilicon composition.
8. the preparation method of the methyl silicon resin that organosilicon composition according to claim 6 is toughness reinforcing, is characterized in that, the concrete operation step of described method two is as follows:
1. each component is prepared according to the formula of claim 1;
2. prepare organosilicon composition according to method described in claim 5, save backup;
3. in reaction vessel, first adding 0 ~ 30 gram of ethanol or Virahol and 2 ~ 6 grams of pH value is the aqueous acetic acid of 4 ~ 5, then the organosilicon composition 2 ~ 30 grams that 2. step obtains is added, at room temperature stir after 2 hours, reaction 2h is continued, the hydrolysis prepolymerization product of obtained organosilicon composition at 80 DEG C; In another reaction vessel, add deionized water or acidic silicasol, an acidic catalyst, methyl trialkoxysilane, tetraalkoxysilane, phenyl trialkoxysilane, dimethyldialkylammonium TMOS, silane coupling agent that 1. step prepare successively, stirred at ambient temperature 1 ~ 4h, obtains the hydrolysis prepolymerization product of siloxanyl monomers at 60 ~ 80 DEG C of stirring reaction 1 ~ 12h;
4. in mixing vessel, add the hydrolysis prepolymerization product of the siloxanyl monomers that 3. the hydrolysis prepolymerization product of the organosilicon composition that 3. step obtains and step obtain, stir 3 ~ 5 minutes, the solidifying agent then 1. prepared with step, flow agent stir to mix for 3 ~ 5 minutes and namely obtain the toughness reinforcing methyl silicon resin of organosilicon composition.
9. the preparation method of the methyl silicon resin that organosilicon composition according to claim 6 is toughness reinforcing, is characterized in that, described methyl trialkoxysilane is methyltrimethoxy silane or Union carbide A-162; Tetraalkoxysilane is tetramethoxy-silicane or tetraethoxysilane; Phenyl trialkoxysilane is phenyltrimethoxysila,e or phenyl triethoxysilane; Dimethyldialkylammonium TMOS is dimethyldimethoxysil,ne or dimethyldiethoxysilane.
10. the preparation method of the methyl silicon resin that organosilicon composition according to claim 6 is toughness reinforcing, is characterized in that, described acid catalyst is hydrochloric acid, acetic acid or sulfuric acid.
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| CN105274851A (en) * | 2015-11-06 | 2016-01-27 | 辽宁恒星精细化工有限公司 | Durable, antistatic and dustproof finishing agent for flocking fabrics and preparation method thereof |
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| CN108774334B (en) * | 2018-06-26 | 2021-09-28 | 常州穗时新材料有限公司 | Antifouling and wear-resistant organic silicon coating material for ABS surface and preparation method thereof |
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| CN109880466A (en) * | 2019-02-20 | 2019-06-14 | 太仓佩琦涂料有限公司 | Novel flexible nanometer water low-temperature setting Lacquer finish glaze and preparation method thereof |
| CN111073506A (en) * | 2019-12-30 | 2020-04-28 | 华电郑州机械设计研究院有限公司 | Inorganic silicon-organic silicon copolymerized temperature-resistant heat-insulating coating and preparation and use method thereof |
| CN111286268A (en) * | 2020-03-26 | 2020-06-16 | 郭芳敏 | Toughening and hardening coating composition, preparation method and plastic treatment method |
| CN111621228A (en) * | 2020-07-01 | 2020-09-04 | 广东威凯表面技术有限公司 | Easy-to-clean coating with high hardness and high toughness |
| CN111978859A (en) * | 2020-08-07 | 2020-11-24 | 上海虹涂新材料科技有限公司 | Easily-cleaned high-hardness antibacterial water-based ceramic paint and preparation process thereof |
| CN112175422A (en) * | 2020-08-25 | 2021-01-05 | 浙江巨化技术中心有限公司 | Coating composition for automobile glass |
| CN112175422B (en) * | 2020-08-25 | 2021-10-22 | 浙江巨化技术中心有限公司 | Coating composition for automobile glass |
| CN115521645A (en) * | 2022-11-10 | 2022-12-27 | 贵州云天科贸有限公司 | Single-component inorganic zinc-rich antirust anti-slip coating |
| CN115521645B (en) * | 2022-11-10 | 2023-09-12 | 贵州云天科贸有限公司 | Single-component inorganic zinc-rich antirust anti-slip coating |
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