CN104910804A - Latex particle toughened methyl silicone resin and preparation method thereof - Google Patents
Latex particle toughened methyl silicone resin and preparation method thereof Download PDFInfo
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Abstract
The invention relates to latex particle toughened methyl silicone resin and a preparation method thereof. The resin disclosed by the invention contains the ingredients in gram by weight: 2-50g of emulsion metered by latex particle content, 0-60g of deionized water, 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, 0-0.5g of leveling agent and 0-0.5g of antifoamer. The resin disclosed by the invention has the biggest advantage that a very good toughening effect can be realized by latex particles of a small volume of emulsion, and a film formed material is endowed with very good flexibility while high hardness for the methyl silicone 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 latex particle 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 coating 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) (US4368235) 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.CN103201318A 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 the methyl silicon resin that a kind of latex particle is toughness reinforcing; it is crisp that this resin overcomes existing methyl silicon resin matter, easily ftractures in the curing process, the coating 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 latex particle 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: with the emulsion 2 ~ 50 of latex particle content meter, deionized water 0 ~ 60, 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, defoamer 0 ~ 0.5,
Described emulsion is one or several in ACRYLIC EMULSION, epoxy emulsion, organic silicon emulsion, and the median size of its latex particle is that between 20nm ~ 3 μm, above-mentioned emulsion is anionic, cationic or non-ionic type;
Described silane coupling agent is γ-(2,3-propylene oxide) propyl trimethoxy silicane, γ-(2,3-propylene oxide) propyl-triethoxysilicane, gamma-amino propyl trimethoxy silicane, one in γ aminopropyltriethoxy silane;
Described solidifying agent is 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 methyl silicon resin that above-mentioned latex particle 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 latex particle is toughness reinforcing, acid catalyst described in it is hydrochloric acid, acetic acid or sulfuric acid.Preferred hydrochloric acid or acetic acid.
The methyl silicon resin that above-mentioned latex particle is toughness reinforcing, described in it, the filming condition of the methyl silicon resin that latex particle is toughness reinforcing is: at 60 DEG C after predrying 10min, more namely solidification 0.3 ~ 2h forms the toughness reinforcing methyl silicon resin film of latex particle 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 latex particle 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 latex particle is toughness reinforcing, and it is characterized in that, concrete steps are as follows:
1. each component is prepared according to formula according to claim 1;
2. in reaction vessel, add deionized water, an acidic catalyst, methyl trialkoxysilane, tetraalkoxysilane, phenyl trialkoxysilane, dimethyldialkylammonium TMOS and silane coupling agent successively, stirring reaction 1 ~ 12h completes hydrolysis prepolymerization, then adds emulsion stirring and mixes for 3 ~ 5 minutes;
Or, in reaction vessel, first add emulsion, then in emulsion, add deionized water, an acidic catalyst, methyl trialkoxysilane, tetraalkoxysilane, phenyl trialkoxysilane, dimethyldialkylammonium TMOS and silane coupling agent successively, stirring reaction completes hydrolysis prepolymerization in 1 ~ 12 hour;
3., in step 2. gained liquid material, after adding solidifying agent, ethanol or Virahol, flow agent, defoamer, stir to mix for 3 ~ 5 minutes and be the toughness reinforcing methyl silicon resin of latex particle.
The preparation method of the methyl silicon resin that above-mentioned latex particle is toughness reinforcing, step described in it 2. in stirring reaction be in room temperature, or to carry out at 30 ~ 50 DEG C.
The preparation method of the methyl silicon resin that above-mentioned latex particle 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 latex particle is toughness reinforcing, acid catalyst described in it is hydrochloric acid, acetic acid or sulfuric acid.Preferred hydrochloric acid or acetic acid.
Technique effect of the present invention is: principal character of the present invention utilizes latex particle to carry out plasticizing methyl silicone resin.The toughness reinforcing methyl silicon resin of the latex particle of technical solution of the present invention is compared with existing toughness reinforcing methyl silicon resin, and maximum advantage only needs emulsion particle for a small amount of emulsion can realize extraordinary toughening effect.While maintaining methyl silicon resin high rigidity, the material given after film forming has good snappiness.Why the film of the methyl silicon resin formation that latex particle is toughness reinforcing has so superior performance, is-combined structure because the organic and inorganic of its uniqueness is separated.The hard polysiloxane serving as external phase in the film ensures paint film high rigidity and scratch-resistant performance; The latex particle of emulsion is filled in the middle of polysiloxane network uniformly, 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 latex particle of emulsion can play again the effect of buffering, now coating produce deformation can be completed by the latex particle of the good emulsion of elasticity, the explosion of film can be avoided.Emulsion latex morphology of particles, size and addition can be determined according to the film performance expected.Such as: adopt the less microemulsion of latex particle size can provide the transparency of film; The emulsion that latex particle Tg is lower is adopted to be favourable to the shock resistance of raising paint film and bending resistance; Adopt the emulsion of latex particle good heat resistance such as polysiloxane emulsion can improve the resistance toheat of paint film.In addition; the preparation technology of the methyl silicon resin that emulsion 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.
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 emulsion used in embodiment comprises:
Anionic polyacrylate emulsion is the commercially available prod of environmental protection coating material company limited of CNOOC, product grade is CT-6910, and its latex particle content is 40wt%, pH=9, latex particle median size is 120nm, and glass transition temperature (Tg) is 10 DEG C;
Cationic polyacrylate emulsion is the commercially available prod of Ma'an Mountain nine and Chemical Co., Ltd., product grade is JH-1840, and its latex particle content is 30wt%, pH=4, latex particle median size is 39nm, and glass transition temperature (Tg) is-18 DEG C;
Cationic polysiloxane emulsion is the commercially available prod of Laiyang Sheng Bang organosilicon scientific & technical corporation, and its latex particle content is 30wt%, pH=4, and latex particle median size is 35nm;
Non-ionic type epoxy emulsion is the commercially available prod of environmental protection coating material company limited of CNOOC, and product grade is CT-6062, and its latex particle content is 50wt%, pH=7, and latex particle median size is 140nm;
Flow agent is the product of German BYK company, and product grade is BYK-331;
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; Thermotolerance is pressed GB/T 1735-1979 method and is measured;
Embodiment 1
1. each component is prepared by following formula
Deionization 50g; An acidic catalyst acetic acid 1g; Methyltrimethoxy silane 40g; Emulsion is anionic polyacrylate emulsion (CT-6910) 5g (with its latex particle content meter); Solidifying agent is Tetramethylammonium hydroxide 0.1g;
2. in the round-bottomed flask of 250mL, add deionized water, an acidic catalyst and methyl trialkoxysilane successively, at 25 DEG C, stirring reaction 2h completes hydrolysis prepolymerization, then adds emulsion and stirs and mix for 3 minutes;
3., in step 2. gained liquid material, after adding solidifying agent, stir to mix for 3 minutes and be the toughness reinforcing methyl silicon resin of latex particle.
The methyl silicon resin toughness reinforcing with embodiment 1 gained latex particle is coated on tinplate, is coated with film thickness monitoring < 50 μm, at 60 DEG C after predrying 10min, 1h is solidified again at 80 DEG C, measuring gained hardness of film is 6H, and sticking power is 0 grade, and paint film is without cracking.
Embodiment 2
1. each component is prepared by following formula
Deionization 50g; An acidic catalyst acetic acid 1g; Methyltrimethoxy silane 40g; Phenyltrimethoxysila,e 5g; Emulsion is anionic polyacrylate emulsion (CT-6910) 40g (with its latex particle content meter); Solidifying agent is Tetramethylammonium hydroxide 0.1g;
2. in the round-bottomed flask of 250mL, add deionized water, an acidic catalyst, methyltrimethoxy silane and phenyltrimethoxysila,e successively, at 25 DEG C, stirring reaction 2h completes hydrolysis prepolymerization, then adds emulsion and stirs and mix for 5 minutes;
3., in step 2. gained liquid material, after adding solidifying agent, stir to mix for 3 minutes and be the toughness reinforcing methyl silicon resin of latex particle.
The methyl silicon resin toughness reinforcing with embodiment 2 gained latex particle is coated on tinplate, be coated with film thickness monitoring < 50 μm, at 60 DEG C after predrying 10min, 1h is solidified again at 80 DEG C, measure gained hardness of film close to 6H, sticking power is 0 grade, and paint film is without cracking, and snappiness bends by 1mm.
Embodiment 3
1. each component is prepared by following formula
Deionization 20g; An acidic catalyst is acetic acid 0.5g; Methyltrimethoxy silane 50g; Phenyltrimethoxysila,e 5g; Emulsion is cationic polyacrylate emulsion (JH-1840) 2g (with its latex particle content meter); Solidifying agent is Tetramethylammonium hydroxide 0.1g, flow agent 0.2g;
2. in the round-bottomed flask of 250mL, first add emulsion, then in emulsion, add deionized water, an acidic catalyst, methyltrimethoxy silane and phenyltrimethoxysila,e successively, stirring at room temperature is reacted and is completed hydrolysis prepolymerization in 4 hours;
3., in step 2. gained liquid material, after adding solidifying agent and flow agent, stir to mix for 3 minutes and be the toughness reinforcing methyl silicon resin of latex particle.
The methyl silicon resin toughness reinforcing with embodiment 3 gained latex particle is coated on PMMA plate, is coated with film thickness monitoring < 50 μm, at 60 DEG C after predrying 10min, 1h is solidified again at 80 DEG C, measuring gained hardness of film is 6H, and sticking power is 0 grade, and paint film is without cracking.
Embodiment 4
1. each component is prepared by following formula
Deionization 20g; An acidic catalyst is acetic acid 0.5g; Methyltrimethoxy silane 50g; Tetramethoxy-silicane 5g, dimethyldimethoxysil,ne 2g; Emulsion is cationic polysiloxane emulsion 2g (with its latex particle content meter); Solidifying agent is Tetramethylammonium hydroxide 0.1g;
2. in the round-bottomed flask of 250mL, first add emulsion, then in emulsion, add deionized water, an acidic catalyst, methyltrimethoxy silane, tetramethoxy-silicane and dimethyldimethoxysil,ne successively, stirring at room temperature is reacted and is completed hydrolysis prepolymerization in 4 hours;
3., in step 2. gained liquid material, after adding solidifying agent, stir to mix for 3 minutes and be the toughness reinforcing methyl silicon resin of latex particle.
The methyl silicon resin toughness reinforcing with embodiment 4 gained latex particle is coated on tinplate, be coated with film thickness monitoring < 50 μm, at 60 DEG C after predrying 10min, 1h is solidified again at 80 DEG C, measuring gained hardness of film is 6H, and sticking power is 0 grade, and paint film is without cracking, snappiness bends by 1mm, and thermotolerance is place 5h film non yellowing at 180 DEG C.
Embodiment 5
1. each component is prepared by following formula
Deionization 20g; An acidic catalyst acetic acid 1.0g; Methyltrimethoxy silane 50g, tetramethoxy-silicane 5g, silane coupling agent gamma-amino propyl trimethoxy 2g; Emulsion is cationic epoxy emulsion (CT-6062) 10g (with its latex particle content meter); Solidifying agent is Tetramethylammonium hydroxide 0.1g;
2. in the round-bottomed flask of 250mL, first add emulsion, then in emulsion, add deionized water, an acidic catalyst, methyltrimethoxy silane, tetramethoxy-silicane and silane coupling agent successively, stirring at room temperature is reacted and is completed hydrolysis prepolymerization in 4 hours;
3., in step 2. gained liquid material, after adding solidifying agent, stir to mix for 5 minutes and be the toughness reinforcing methyl silicon resin of latex particle.
The methyl silicon resin toughness reinforcing with embodiment 5 gained latex particle is coated on tinplate, be coated with film thickness monitoring < 50 μm, at 60 DEG C after predrying 10min, 1h is solidified again at 80 DEG C, measuring gained hardness of film is 6H, sticking power is 0 grade, and paint film is without cracking, and snappiness bends by 1mm.
Claims (10)
1. the methyl silicon resin that a latex particle 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: with the emulsion 2 ~ 50 of latex particle content meter, deionized water 0 ~ 60, 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, defoamer 0 ~ 0.5;
Described emulsion is one or several in ACRYLIC EMULSION, epoxy emulsion, organic silicon emulsion, and the median size of its latex particle is that between 20nm ~ 3 μm, above-mentioned emulsion is anionic, cationic or non-ionic type;
Described silane coupling agent is γ-(2,3-propylene oxide) propyl trimethoxy silicane, γ-(2,3-propylene oxide) propyl-triethoxysilicane, gamma-amino propyl trimethoxy silicane, one in γ aminopropyltriethoxy silane;
Described solidifying agent is 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.
2. the methyl silicon resin that latex particle 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.
3. the methyl silicon resin that latex particle according to claim 1 is toughness reinforcing, is characterized in that, described acid catalyst is hydrochloric acid, acetic acid or sulfuric acid.
4. the methyl silicon resin that latex particle according to claim 3 is toughness reinforcing, is characterized in that, described acid catalyst is hydrochloric acid or acetic acid.
5. the methyl silicon resin that latex particle according to claim 1 is toughness reinforcing, it is characterized in that, the filming condition of the methyl silicon resin that described latex particle is toughness reinforcing is: at 60 DEG C after predrying 10min, more namely solidification 0.3 ~ 2h forms the toughness reinforcing methyl silicon resin film of latex particle at 80 ~ 140 DEG C.
6. a preparation method for the methyl silicon resin that latex particle according to claim 1 is toughness reinforcing, is characterized in that, concrete steps are as follows:
1. each component is prepared according to formula according to claim 1;
2. in reaction vessel, add deionized water, an acidic catalyst, methyl trialkoxysilane, tetraalkoxysilane, phenyl trialkoxysilane, dimethyldialkylammonium TMOS and silane coupling agent successively, stirring reaction 1 ~ 12h completes hydrolysis prepolymerization, then adds emulsion stirring and mixes for 3 ~ 5 minutes;
Or, in reaction vessel, first add emulsion, then in emulsion, add deionized water, an acidic catalyst, methyl trialkoxysilane, tetraalkoxysilane, phenyl trialkoxysilane, dimethyldialkylammonium TMOS and silane coupling agent successively, stirring reaction completes hydrolysis prepolymerization in 1 ~ 12 hour;
3., in step 2. gained liquid material, after adding solidifying agent, ethanol or Virahol, flow agent, defoamer, stir to mix for 3 ~ 5 minutes and be the toughness reinforcing methyl silicon resin of latex particle.
7. the preparation method of the methyl silicon resin that latex particle according to claim 6 is toughness reinforcing, is characterized in that, described step 2. in stirring reaction be in room temperature, or to carry out at 30 ~ 50 DEG C.
8. the preparation method of the methyl silicon resin that latex particle 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.
9. the preparation method of the methyl silicon resin that latex particle according to claim 6 is toughness reinforcing, is characterized in that, described acid catalyst is hydrochloric acid, acetic acid or sulfuric acid.
10. the preparation method of the methyl silicon resin that latex particle according to claim 9 is toughness reinforcing, is characterized in that, described acid catalyst is hydrochloric acid or acetic acid.
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| CN106957396A (en) * | 2017-04-10 | 2017-07-18 | 广东优科艾迪高分子材料有限公司 | A kind of automatically cleaning wear-resisting type organosilicon toughener and preparation method and application |
| CN108774334A (en) * | 2018-06-26 | 2018-11-09 | 常州穗时新材料有限公司 | ABS surface antifouling, wear-resisting organosilicon coating material and preparation method thereof |
| CN109486412A (en) * | 2018-09-19 | 2019-03-19 | 航天材料及工艺研究所 | Low transmitting thermal control coating of a kind of low absorption and preparation method thereof |
| CN109867991A (en) * | 2019-03-15 | 2019-06-11 | 常州穗时新材料有限公司 | One kind is exempted to cure high-performance ceramic sealing wax and preparation method thereof |
| CN111040166A (en) * | 2019-11-28 | 2020-04-21 | 湖北新四海化工股份有限公司 | Environment-friendly moisture-curing silicone resin and preparation method thereof |
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| CN111040166A (en) * | 2019-11-28 | 2020-04-21 | 湖北新四海化工股份有限公司 | Environment-friendly moisture-curing silicone resin and preparation method thereof |
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