CN105176482A - High-performance dealcoholized organosilicon adhesive and preparation technique thereof - Google Patents
High-performance dealcoholized organosilicon adhesive and preparation technique thereof Download PDFInfo
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- CN105176482A CN105176482A CN201510739169.3A CN201510739169A CN105176482A CN 105176482 A CN105176482 A CN 105176482A CN 201510739169 A CN201510739169 A CN 201510739169A CN 105176482 A CN105176482 A CN 105176482A
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Abstract
The invention provides a high-performance dealcoholized organosilicon adhesive which is a high-performance dealcoholized sealant prepared by compounding an alkoxy-terminated polydimethylsiloxane base adhesive with a coupling agent as a bonding assistant. The invention also provides a preparation method of the high-performance dealcoholized organosilicon adhesive. The high-performance dealcoholized organosilicon adhesive shortens the surface viscosity reduction time, obviously enhances the curing speed, and satisfies the requirements of most industries for enhancing production efficiency and shortening procedure time consumption. No viscosity peak exists in the production process, thereby greatly enhancing the production and lowering the production risk. The high-performance dealcoholized organosilicon adhesive has favorable bonding property, and can satisfy the bonding requirements of most substrates. Due to the enhancement of the storage stability, the allowed storage time of the product is up to 12 months or above, thereby reducing the loss caused by performance reduction due to transportation and storage.
Description
Technical field
The present invention relates to a kind of high-performance dealcoholizing-type organic silica gel and preparation technology thereof.
Background technology
Traditional single-component de-alcoholized room temperature vulcanized silicone rubber is glue based on hydroxy-end capped polydimethylsiloxane generally, and many organoalkoxysilanes are linking agent, organic titanate and inner complex thereof is catalyzer, then coordinates coupling agent, reinforced filling etc. to be prepared from.
This conventional art has the following disadvantages: 1, surperficial tack free time is long, and deeply-curing speed is slow; 2, when being applied to the adhering and sealing of some industry, not ideal enough to touched base material attachment cementability; 3, basic glue middle-end hydroxyl activity is too high, when being added with organic titanate class catalyzer in production process, can produce viscosity peak, causes sizing material sharply thickening, brings high energy consumption, the problems such as high-drag, affect subsequent production; 4, the existence of basic glue terminal hydroxy group, also causes the product stock stability produced bad, shows that product performance extend along with the shelf-time and decline, and after general three months, surperficial tack free time extends, and after sulfuration, mechanical property obviously declines.
Summary of the invention
Technical problem to be solved by this invention, proposes a kind of high-performance dealcoholizing-type organic silica gel exactly, its glue based on alkoxy end-capped polydimethylsiloxane, and composite coupling agent is that bonding auxiliary agent obtains.
The invention allows for the preparation technology of above-mentioned high-performance dealcoholizing-type organic silica gel
For solving the problems of the technologies described above, the present invention is achieved by the following technical solutions:
A kind of high-performance dealcoholizing-type organic silica gel, comprise the material of following parts by weight: 100 parts of alkoxy end-capped polydimethylsiloxanes, 5 ~ 30 parts of dimethyl silicone oils, 30 ~ 130 parts of fillers, 3 ~ 10 parts of linking agents, 1 ~ 10 part of catalyzer and 0.5 ~ 3 part of composite coupling agent, described alkoxy end-capped polydimethylsiloxane is by α, alpha, omega-dihydroxy polydimethyl siloxane, end-capping reagent and capping catalyst obtain in the ratio of 80 ~ 120:1 ~ 12:0.1 ~ 5, wherein α, the viscosity of alpha, omega-dihydroxy polydimethyl siloxane is 2000 ~ 100000cps, described composite coupling agent is obtained in the ratio of 1 ~ 10:1 ~ 10 is composite by amino-alkyl silicane coupling agent and epoxyhydrocarbyl silane coupling agent.
Two ends of the present invention adopt alkoxy end-capped, avoid the appearance on viscosity peak in production process, greatly reduce the risk factor produced and occur defective products; Have employed alkoxy end-capped technology, improve the stability in storage of product, make the quality guaranteed period of product extend to more than 12 months from three to six months, thus decrease product because of oversize the caused expired loss such as to scrap of transport, process of depositing.
As preferably, described filler is one or more in active nano-calcium carbonate, water-ground limestone, silicon powder, diatomite, talcum powder, gas-phase silica, precipitated silica.
As preferably, described filler is one or both in active nano-calcium carbonate, water-ground limestone.
As preferably, described end-capping reagent is one or more in tetramethoxy-silicane, tetraethoxysilane, methyltrimethoxy silane, vinyltrimethoxy silane, propyl trimethoxy silicane, phenyltrimethoxysila,e, phenyl triethoxysilane, Union carbide A-162, vinyltriethoxysilane, dimethyldimethoxysil,ne and dimethyldiethoxysilane.
As preferably, described end-capping reagent is one or more in tetramethoxy-silicane, methyltrimethoxy silane, vinyltrimethoxy silane, propyl trimethoxy silicane, phenyltrimethoxysila,e, dimethyldimethoxysil,ne.
As preferably, described capping catalyst is one or more in acetoxime, Diacetylmonoxime, diethyl ketoxime, cyclopentanone oxime, cyclohexanone-oxime, diphenyl-ketoxime, benzaldoxime.
As preferably, described capping catalyst is one or more in acetoxime, Diacetylmonoxime, diethyl ketoxime, cyclopentanone oxime, cyclohexanone-oxime.
As preferably, described linking agent is one or more in tetramethoxy-silicane, methyltrimethoxy silane, vinyltrimethoxy silane, tetraethoxysilane, vinyltriethoxysilane, dimethyldimethoxysil,ne, diethyldiethoxysilane, phenyltrimethoxysila,e, phenyl triethoxysilane.
As preferably, described catalyzer is titanium propanolate, butyl (tetra) titanate, the metatitanic acid tert-butyl ester, 2-ethyl hexyl oxy titanic acid ester, two (methyl aceto acetate base) titanium complex of diisopropoxy, two (methyl ethyl diketone) titanium complex, 1 of diisopropoxy, one or more in two (methyl ethyl diketone) complex compound of two (methyl aceto acetate) complex compound of 3-third dioxy base titanium, 1,3-third dioxy base titanium.
As preferably, described amino-alkyl silicane coupling agent is one or more in 3-aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, 3-urea propyl trimethoxy silicane, anilinomethyl trimethoxy silane, anilinomethyl triethoxysilane.
As preferably, described epoxyhydrocarbyl silane coupling agent is 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane, 3-(2,3-epoxy third oxygen) propyl-triethoxysilicane, 3-(2,3-epoxy third oxygen) hydroxypropyl methyl dimethoxysilane, one or more in 2-(3,4-epoxycyclohexyl) ethyl triethoxysilane.
A preparation technology for high-performance dealcoholizing-type organic silica gel, comprises the following steps: in the stirrer of band heating and cooling recirculated water, adds 100 parts of alkoxy end-capped polydimethylsiloxanes, 5 ~ 30 parts of dimethyl silicone oils, 30 ~ 130 parts of fillers, are warming up to 120 DEG C, decompression dehydration 2 hours, then room temperature is cooled to, 3 ~ 10 parts of linking agents are added, 1 ~ 10 part of catalyzer, 0.5 ~ 3 part of composite coupling agent in nitrogen atmosphere, half an hour is stirred in decompression, obtained product.
As preferably, described alkoxy end-capped polydimethylsiloxane is by α, alpha, omega-dihydroxy polydimethyl siloxane, end-capping reagent and capping catalyst obtain in the ratio of 80 ~ 120:1 ~ 12:0.1 ~ 5, wherein α, the viscosity of alpha, omega-dihydroxy polydimethyl siloxane is 2000 ~ 100000cps, concrete steps are: under nitrogen protection condition, α is added in proportion in reactor, alpha, omega-dihydroxy polydimethyl siloxane, end-capping reagent and capping catalyst, stirring reaction 3 hours at 90 DEG C, then 130 DEG C of underpressure distillation 1 hour is warming up to, obtained alkoxy end-capped polydimethylsiloxane.
As preferably; described composite coupling agent is obtained in the ratio of 1 ~ 10:1 ~ 10 by amino-alkyl silicane coupling agent and epoxyhydrocarbyl silane coupling agent; concrete steps are: under nitrogen protection condition; 1 ~ 10 part of amino-alkyl silicane coupling agent and 1 ~ 10 part of epoxyhydrocarbyl silane coupling agent is added in proportion in reactor; stirring reaction 3 hours at 90 DEG C; then room temperature is cooled to, obtained composite coupling agent.
Compared with prior art, the beneficial effect that the present invention has is: 1, reduce surperficial tack free time short, significantly improve curing speed, meets the requirement that most industries is consuming time to operation of enhancing productivity, reduce; 2, in production process without viscosity peak, substantially increase production safety coefficient, reduce production risk.3, cementability is good, can meet to feel the bonding requirements of most of base material.4, the raising of stability in storage, makes product allow the shelf-time to reach more than 12 months, decreases because of transport and deposits the loss that the degradation that causes brings.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of the alkoxy end-capped polydimethylsiloxane of the present invention;
Fig. 2 is preparation technology's schema of the composite coupling agent of the present invention;
Fig. 3 is preparation technology's schema of high-performance dealcoholizing-type organic silica gel of the present invention.
Embodiment
For the understanding the present invention making those skilled in the art more clear and intuitive, below in conjunction with accompanying drawing, the present invention is further illustrated.
Embodiment 1
The high-performance dealcoholizing-type organic silica gel of the present embodiment comprises the material of following parts by weight: 100 parts of alkoxy end-capped polydimethylsiloxanes, 20 parts of dimethyl silicone oils, 130 parts of active nano-calcium carbonates, 2 parts of linking agent methyltrimethoxy silanes, 2 parts of catalyzer diisopropoxies two (methyl aceto acetate base) titanium complex, 0.5 part of composite coupling agent;
Its preparation process is: (1) is under nitrogen protection condition, add the α of viscosity 5000cps in the ratio of 100:5:0.5 in reactor, alpha, omega-dihydroxy polydimethyl siloxane, tetramethoxy-silicane, diethyl ketoxime, stirring reaction 3 hours at 90 DEG C, then 130 DEG C of underpressure distillation 1 hour is warming up to, obtained alkoxy end-capped polydimethylsiloxane;
(2) under nitrogen protection condition, 3-aminopropyl triethoxysilane and 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane is added in the ratio of 1:1, stirring reaction 3 hours at 90 DEG C in reactor, then room temperature is cooled to, obtained composite coupling agent;
(3) in the stirrer of band heating and cooling recirculated water, add 100 parts of alkoxy end-capped polydimethylsiloxanes, 20 parts of dimethyl silicone oils, 130 parts of active nano-calcium carbonates, be warming up to 120 DEG C, decompression dehydration 2 hours, is then cooled to room temperature, adds 2 parts of linking agent methyltrimethoxy silanes in nitrogen atmosphere, 2 parts of two (methyl aceto acetate base) titanium complexs of catalyzer diisopropoxy, 0.5 part of composite coupling agent, half an hour is stirred in decompression, obtained product.
Embodiment 2
The high-performance dealcoholizing-type organic silica gel of the present embodiment comprises the material of following parts by weight: 100 parts of alkoxy end-capped polydimethylsiloxanes, 20 parts of dimethyl silicone oils, 90 parts of active nano-calcium carbonates, 40 parts of water-ground limestones, 3 parts of linking agent vinyltrimethoxy silanes, 1.5 parts of catalyzer 1,3-third dioxy base titaniums two (methyl ethyl diketone) complex compound, 1 part of composite coupling agent;
Its preparation process is: (1) is under nitrogen protection condition, add the α of 20000cps in the ratio of 100:2:5:1 in reactor, alpha, omega-dihydroxy polydimethyl siloxane, tetramethoxy-silicane, methyltrimethoxy silane, acetoxime, stirring reaction 3 hours at 90 DEG C, then 130 DEG C of underpressure distillation 1 hour is warming up to, obtained alkoxy end-capped polydimethylsiloxane;
(2) under nitrogen protection condition, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and 2-(3 is added in the ratio of 1:1.5 in reactor, 4-epoxycyclohexyl) ethyl triethoxysilane, stirring reaction 3 hours at 90 DEG C, then room temperature is cooled to, obtained composite coupling agent;
(3) in the stirrer of band heating and cooling recirculated water, 100 parts of alkoxy end-capped polydimethylsiloxanes are added, 20 parts of dimethyl silicone oils, 90 parts of active nano-calcium carbonates, 40 parts of water-ground limestones, are warming up to 120 DEG C, decompression dehydration 2 hours, then be cooled to room temperature, in nitrogen atmosphere, add 3 parts of linking agent vinyltrimethoxy silanes, 1.5 parts of catalyzer 1, two (methyl ethyl diketone) complex compound of 3-third dioxy base titanium, 1 part of composite coupling agent, half an hour is stirred in decompression, obtained product.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a high-performance dealcoholizing-type organic silica gel, it is characterized in that the material comprising following parts by weight: 100 parts of alkoxy end-capped polydimethylsiloxanes, 5 ~ 30 parts of dimethyl silicone oils, 30 ~ 130 parts of fillers, 3 ~ 10 parts of linking agents, 1 ~ 10 part of catalyzer and 0.5 ~ 3 part of composite coupling agent, described alkoxy end-capped polydimethylsiloxane is by α, alpha, omega-dihydroxy polydimethyl siloxane, end-capping reagent and capping catalyst obtain in the ratio of 80 ~ 120:1 ~ 12:0.1 ~ 5, wherein α, the viscosity of alpha, omega-dihydroxy polydimethyl siloxane is 2000 ~ 100000cps, described composite coupling agent is obtained in the ratio of 1 ~ 10:1 ~ 10 is composite by amino-alkyl silicane coupling agent and epoxyhydrocarbyl silane coupling agent.
2. high-performance dealcoholizing-type organic silica gel according to claim 1, is characterized in that: described filler is one or more in active nano-calcium carbonate, water-ground limestone, silicon powder, diatomite, talcum powder, gas-phase silica, precipitated silica.
3. high-performance dealcoholizing-type organic silica gel according to claim 1, is characterized in that: described end-capping reagent is one or more in tetramethoxy-silicane, tetraethoxysilane, methyltrimethoxy silane, vinyltrimethoxy silane, propyl trimethoxy silicane, phenyltrimethoxysila,e, phenyl triethoxysilane, Union carbide A-162, vinyltriethoxysilane, dimethyldimethoxysil,ne and dimethyldiethoxysilane.
4. high-performance dealcoholizing-type organic silica gel according to claim 1, is characterized in that: described capping catalyst is one or more in acetoxime, Diacetylmonoxime, diethyl ketoxime, cyclopentanone oxime, cyclohexanone-oxime, diphenyl-ketoxime, benzaldoxime.
5. high-performance dealcoholizing-type organic silica gel according to claim 1, is characterized in that: described linking agent is one or more in tetramethoxy-silicane, methyltrimethoxy silane, vinyltrimethoxy silane, tetraethoxysilane, vinyltriethoxysilane, dimethyldimethoxysil,ne, diethyldiethoxysilane, phenyltrimethoxysila,e, phenyl triethoxysilane.
6. high-performance dealcoholizing-type organic silica gel according to claim 1, it is characterized in that: described catalyzer is titanium propanolate, butyl (tetra) titanate, the metatitanic acid tert-butyl ester, 2-ethyl hexyl oxy titanic acid ester, two (methyl aceto acetate base) titanium complex of diisopropoxy, two (methyl ethyl diketone) titanium complex, 1 of diisopropoxy, one or more in two (methyl ethyl diketone) complex compound of two (methyl aceto acetate) complex compound of 3-third dioxy base titanium, 1,3-third dioxy base titanium.
7. high-performance dealcoholizing-type organic silica gel according to claim 1, is characterized in that: described amino-alkyl silicane coupling agent is one or more in 3-aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, 3-urea propyl trimethoxy silicane, anilinomethyl trimethoxy silane, anilinomethyl triethoxysilane.
8. high-performance dealcoholizing-type organic silica gel according to claim 1, it is characterized in that: described epoxyhydrocarbyl silane coupling agent is 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane, 3-(2,3-epoxy third oxygen) propyl-triethoxysilicane, 3-(2,3-epoxy third oxygen) hydroxypropyl methyl dimethoxysilane, one or more in 2-(3,4-epoxycyclohexyl) ethyl triethoxysilane.
9. the preparation technology of the high-performance dealcoholizing-type organic silica gel according to any one of claim 1 ~ 8, it is characterized in that comprising the following steps: in the stirrer of band heating and cooling recirculated water, add 100 parts of alkoxy end-capped polydimethylsiloxanes, 5 ~ 30 parts of dimethyl silicone oils, 30 ~ 130 parts of fillers, be warming up to 120 DEG C, decompression dehydration 2 hours, then room temperature is cooled to, 3 ~ 10 parts of linking agents are added, 1 ~ 10 part of catalyzer, 0.5 ~ 3 part of composite coupling agent in nitrogen atmosphere, half an hour is stirred in decompression, obtained product.
10. the preparation technology of high-performance dealcoholizing-type organic silica gel according to claim 9, it is characterized in that: described alkoxy end-capped polydimethylsiloxane is by α, alpha, omega-dihydroxy polydimethyl siloxane, end-capping reagent and capping catalyst obtain in the ratio of 80 ~ 120:1 ~ 12:0.1 ~ 5, wherein α, the viscosity of alpha, omega-dihydroxy polydimethyl siloxane is 2000 ~ 100000cps, concrete steps are: under nitrogen protection condition, α is added in proportion in reactor, alpha, omega-dihydroxy polydimethyl siloxane, end-capping reagent and capping catalyst, stirring reaction 3 hours at 90 DEG C, then 130 DEG C of underpressure distillation 1 hour is warming up to, obtained alkoxy end-capped polydimethylsiloxane,
Described composite coupling agent is obtained in the ratio of 1 ~ 10:1 ~ 10 by amino-alkyl silicane coupling agent and epoxyhydrocarbyl silane coupling agent; concrete steps are: under nitrogen protection condition; 1 ~ 10 part of amino-alkyl silicane coupling agent and 1 ~ 10 part of epoxyhydrocarbyl silane coupling agent is added in proportion in reactor; stirring reaction 3 hours at 90 DEG C; then room temperature is cooled to, obtained composite coupling agent.
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| CN105860861A (en) * | 2016-05-06 | 2016-08-17 | 烟台图文马克化工科技有限公司 | Silicone sealant for hanging wallboard |
| CN106147695A (en) * | 2016-06-29 | 2016-11-23 | 佛山市幸多新材料有限公司 | Quick cured silicone glue of one 1 to 1 double-component and preparation method thereof |
| CN107022337A (en) * | 2017-04-19 | 2017-08-08 | 常熟市恒信粘胶有限公司 | Spary coating type weather-resistance flame-retardant silicone structure sealant and preparation method thereof |
| CN107936570A (en) * | 2017-11-06 | 2018-04-20 | 浙江衢州硅宝化工有限公司 | The de-oxime type room curing silicon rubber and preparation method of a kind of low smell |
| CN108485595A (en) * | 2018-04-19 | 2018-09-04 | 薛向东 | A kind of long-acting mould-proof silicone sealant |
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| CN110878142A (en) * | 2019-11-29 | 2020-03-13 | 湖北新蓝天新材料股份有限公司 | Synthesis method of alkoxy-terminated polysiloxane and alkoxy-terminated polysiloxane |
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| CN112898947A (en) * | 2021-02-08 | 2021-06-04 | 佛山市元通胶粘实业有限公司 | Dealcoholized organosilicon sealant by gas phase method and preparation method thereof |
| CN114045150A (en) * | 2021-11-12 | 2022-02-15 | 湖北回天新材料股份有限公司 | Multifunctional silica gel for indoor decoration and preparation method thereof |
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| WO2024040689A1 (en) * | 2022-08-25 | 2024-02-29 | 江西天永诚高分子材料有限公司 | Dealcoholization-type room temperature vulcanized silicone rubber and preparation method therefor |
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| CN105860861A (en) * | 2016-05-06 | 2016-08-17 | 烟台图文马克化工科技有限公司 | Silicone sealant for hanging wallboard |
| CN106147695A (en) * | 2016-06-29 | 2016-11-23 | 佛山市幸多新材料有限公司 | Quick cured silicone glue of one 1 to 1 double-component and preparation method thereof |
| CN107022337A (en) * | 2017-04-19 | 2017-08-08 | 常熟市恒信粘胶有限公司 | Spary coating type weather-resistance flame-retardant silicone structure sealant and preparation method thereof |
| CN107936570A (en) * | 2017-11-06 | 2018-04-20 | 浙江衢州硅宝化工有限公司 | The de-oxime type room curing silicon rubber and preparation method of a kind of low smell |
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| CN108485595A (en) * | 2018-04-19 | 2018-09-04 | 薛向东 | A kind of long-acting mould-proof silicone sealant |
| CN108822553A (en) * | 2018-07-10 | 2018-11-16 | 合肥工业大学 | A kind of the self-reinforcing heat-conducting insulating silicon rubber material and preparation method of filling crosslinking function conduction powder |
| CN111704864A (en) * | 2019-07-19 | 2020-09-25 | 广州市高士实业有限公司 | Silane modified polyether sealant and preparation method and application thereof |
| CN111704864B (en) * | 2019-07-19 | 2021-06-15 | 广州市高士实业有限公司 | Silane modified polyether sealant and preparation method and application thereof |
| CN110591557A (en) * | 2019-09-26 | 2019-12-20 | 杭州之江新材料有限公司 | Organic silicon coating adhesive and preparation method thereof |
| CN110878142A (en) * | 2019-11-29 | 2020-03-13 | 湖北新蓝天新材料股份有限公司 | Synthesis method of alkoxy-terminated polysiloxane and alkoxy-terminated polysiloxane |
| CN112898947A (en) * | 2021-02-08 | 2021-06-04 | 佛山市元通胶粘实业有限公司 | Dealcoholized organosilicon sealant by gas phase method and preparation method thereof |
| CN114045150A (en) * | 2021-11-12 | 2022-02-15 | 湖北回天新材料股份有限公司 | Multifunctional silica gel for indoor decoration and preparation method thereof |
| WO2024040689A1 (en) * | 2022-08-25 | 2024-02-29 | 江西天永诚高分子材料有限公司 | Dealcoholization-type room temperature vulcanized silicone rubber and preparation method therefor |
| CN115785527A (en) * | 2022-12-28 | 2023-03-14 | 佛山市普力达科技有限公司 | Coupling agent for accelerating deep curing, preparation method and transparent RTV (room temperature vulcanized) applied by coupling agent |
| CN115785527B (en) * | 2022-12-28 | 2023-09-12 | 佛山市普力达科技有限公司 | Accelerated deep curing coupling agent, preparation method and transparent RTV (real time kinematic) applied to same |
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Application publication date: 20151223 |
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