CN103172866A - Method for preparing controllable viscosity hydroxyl-terminated polydimethylsiloxane - Google Patents
Method for preparing controllable viscosity hydroxyl-terminated polydimethylsiloxane Download PDFInfo
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- CN103172866A CN103172866A CN2013100830281A CN201310083028A CN103172866A CN 103172866 A CN103172866 A CN 103172866A CN 2013100830281 A CN2013100830281 A CN 2013100830281A CN 201310083028 A CN201310083028 A CN 201310083028A CN 103172866 A CN103172866 A CN 103172866A
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Abstract
The invention relates to the field of organosilicone, and in particular relates to a method for preparing controllable viscosity hydroxyl-terminated polydimethylsiloxan. The method comprises the steps of: mixing hydrolysate with water, adding a reagent A and a reagent B to remove impurities under proper temperature, then standing and separating so as to obtain the required hydrolysate; polymerizing the hydrolysate under the catalysis of a KOH alkaline glue at 100-140 DEG C, adding a phosphoric acid aqueous solution to neutralize when a reaction system reaches the required viscosity, and heating to remove low molecular weight substances so as to obtain the 107 silicon rubber. By utilizing hydrolysate pretreatment, the influences of impurities such as chloride ions and chain links with three functional degrees to the system are greatly reduced; and the viscosity of the system can be slowly and uniformly increased through controlling a catalyst, and the reaction is easy to control.
Description
Technical field
The present invention relates to field of organic silicon, be specifically related to a kind of method of producing the controlled hydroxyl endblocked polydimethylsiloxane of viscosity.
Background technology
Hydroxyl endblocked polydimethylsiloxane (107 silicon rubber) is with hydroxy-end capped straight chain type reactive polysiloxanes, can make line style or the cross-linking type polysiloxane of high molecular weight.It is the basic material of preparation room temperature vulcanized silicone rubber etc.Having been widely used aspect being bonded and sealed of electronic devices and components and Macintosh, moistureproof shockproof and insulating material, along with rolling up of Highrise buildings, 107 silicon rubber also increase greatly as the raw materials requirement amount of building sealant.
The 107 modal synthetic methods of silicon rubber are to utilize the dimethyl siloxane of ring-type, carry out ring-opening polymerization as D4 (octamethylcyclotetrasiloxane), D5 (decamethyl five siloxanes) or DMC (D3～D7 mixture) and obtain.The general KOH that adopts is as catalyzer.
Increasingly competitive along with raw material and price, many producers study synthetic 107 silicon rubber take the organosilane monomer hydrolyzate as raw material one after another, and the employing hydrolyzate is raw material, has reduced the link that its cracking rectifying is become DMC, reduces costs and energy consumption.Therefore, 107 silicon rubber become a kind of trend take hydrolyzate as raw material system.But contain the impurity such as chlorion and three-functionality-degree chain link in the organosilane monomer hydrolyzate, wherein chlorion meeting and catalyst reaction, spent catalyst, and the Repone K inorganic salt that generate are very large on the product appearance impact; And the easy generation in reaction system of three-functionality-degree chain link is crosslinked, makes reaction system produce elastomerics and forms waste product.Therefore, the chlorion and the three-functionality-degree chain link that reduce as much as possible in reaction system are the prerequisites that obtains high quality 107 silicon rubber.And in 107 silicon rubber building-up processes, polymerization is risen, and when gluing, viscosity is difficult to control, and the laboratory repetition rate is low.
Announced a kind of method with synthetic 107 silicon rubber of hydrolyzate in patent publication No. CN 101338034A.Adopting the KOH aqueous solution is catalyzer, and phosphate aqueous solution is neutralizing agent, adds a certain amount of distilled water when hydrolyzate dewaters, to reduce chlorion and the three-functionality-degree impurity in reaction system.
Patent publication No. CN 101173044A discloses a kind of method that organosilicon hydrolyzation thing loop wire separates preparation 107 silicon rubber that fully utilizes.Separate by hydrolyzation material first being carried out loop wire, recycle isolated linear body and obtain 107 silicon rubber through dehydration, base catalyzed polymerization, organophosphorus ester neutralization.
Summary of the invention
The present invention relates to a kind of method of producing the controlled hydroxyl endblocked polydimethylsiloxane of viscosity.Concrete grammar comprises: the hydrolyzate and a certain amount of water that add organosilane monomer to produce in the there-necked flask of 500mL, stir 30min at 50～160 ℃ of temperature, and add reagent A, add reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.To carry out hydrolyzate after pre-treatment and take off lowly, and add catalyzer to carry out polyreaction, question response neutralizes with phosphoric acid during to required viscosity, and the reaction system after neutralization removes low molecule to flowing out without cut, namely gets 107 silicon rubber.
Described reagent A is one or more in anionite-exchange resin, calcium sulfite, gac, Silver Nitrate etc., and the input amount of its sorbent material is 5 ~ 150ppm of hydrolyzate, and further preferred input amount is 20 ~ 30ppm of hydrolyzate.
Described reagent B is ammoniacal liquor, and the ammoniacal liquor input amount is 5 ~ 150ppm of hydrolyzate, and further preferred add-on is 20 ~ 30ppm.
Described catalyzer is KOH alkali glue, and add-on is 5～150ppm of reaction system, and further add-on is 30 ~ 55ppm of reaction system.
Described phosphoric acid is phosphate aqueous solution, and mass concentration is 5～50%, and further the mass concentration of preferably phosphoric acid is 30%; Add-on is 5～150ppm of reaction system, and further add-on is 70 ~ 80ppm of reaction system.
Described hydrolyzate is 100 ~ 140 ℃ with the polymerization temperature of catalyzer KOH alkali glue under vacuum.
The viscosity of described hydroxyl endblocked polydimethylsiloxane can be controlled in 20000 ~ 80000mPa.s.
The impact that present method is brought to solve the impurity such as chlorion and three-functionality-degree chain link by hydrolyzate being carried out pre-treatment is controlled catalyzer to control viscosity.Hydrolyzate is mixed under proper temperature with a certain amount of water, add chlorion sorbent material and ammoniacal liquor to carry out standing separation after removal of impurities.Can remove preferably the impurity such as chlorion in hydrolyzate and three-functionality-degree chain link.And the control of catalyzer makes reaction system viscosity evenly to increase gently, and neutralization gets final product when system arrives required viscosity.Make viscosity controlled, the laboratory can be repeated.
Advantage of the present invention: 1) reduced the temperature of hydrolyzate pre-treatment, the present invention is controlled at 50 ~ 75 ℃; 2) adopt one or more of anionite-exchange resin in the chlorion sorbent material, calcium sulfite, gac, Silver Nitrate, can better remove chlorion and and reduce the crosslinked of three-functionality-degree chain link; 3) the synthetic viscosity that can rationally control hydroxyl endblocked polydimethylsiloxane of catalyzer KOH alkali glue, product homogeneous transparent simultaneously.
Specific embodiment
Below by specific embodiment, the preparation method of the hydroxyl endblocked polydimethylsiloxane that viscosity is controlled is described, the present embodiment is not limited to following examples.
Embodiment 1
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of ℃ of temperature, add 20ppm reagent A (reagent A is anionite-exchange resin and gac), add 20ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 0.5gKOH after 50～120 ℃ of dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 55ppmKOH alkali glue after material dewatering, the polymerization that heats up under 100 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes low molecule and extremely flows out without cut under suitable temperature and vacuum tightness, namely get transparent well, viscosity is 74000～80000 107 silicon rubber.
Embodiment 2
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of ℃ of temperature, add 20ppm reagent A (reagent A is anionite-exchange resin), add 30ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 0.5gKOH after 50 ℃～120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 55ppmKOH alkali glue after material dewatering, the polymerization that heats up under 100 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 70000～75000 107 silicon rubber.
Embodiment 3
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of ℃ of temperature, add 20ppm reagent A (reagent A is Silver Nitrate), add 20ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 0.5gKOH after 50 ℃～120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 55ppmKOH alkali glue after material dewatering, the polymerization that heats up under 120 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 66000～73000 107 silicon rubber.
Embodiment 4
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of ℃ of temperature, add 30ppm reagent A (reagent A is calcium sulfite), add 30ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 0.5gKOH after 50 ℃～120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 55ppmKOH alkali glue after material dewatering, the polymerization that heats up under 120 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 55000～68000 107 silicon rubber.
Embodiment 5
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 30ppm reagent A (reagent A is gac), add 20ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 0.5gKOH after 50 ℃～120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 55ppmKOH alkali glue after material dewatering, the polymerization that heats up under 120 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 47000～56000 107 silicon rubber.
Embodiment 6
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 20ppm reagent A (reagent A is anionite-exchange resin and gac), add 20ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 0.5gKOH after 50 ℃～120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 30ppmKOH alkali glue after material dewatering, the polymerization that heats up under 140 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 42000～50000 107 silicon rubber.
Embodiment 7
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 20ppm reagent A (reagent A is anionite-exchange resin), add 30ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 5.5gKOH after 50 ℃～120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 30ppmKOH alkali glue after material dewatering, the polymerization that heats up under 140 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 39000～46000 107 silicon rubber.
Embodiment 8
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 20ppm reagent A (reagent A is Silver Nitrate), add 30ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 5.5gKOH after 50 ℃～120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 30ppmKOH alkali glue after material dewatering, the polymerization that heats up under 140 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 37000～42000 107 silicon rubber.
Embodiment 9
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 30ppm reagent A (reagent A is calcium sulfite), add 30ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 5.5gKOH after 50 ℃～120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 30ppmKOH alkali glue after material dewatering, the polymerization that heats up under 130 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 35000～39000 107 silicon rubber.
Embodiment 10
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 30ppm reagent A (reagent A is gac), add 20ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 5.5gKOH after 50 ℃～120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 30ppmKOH alkali glue after material dewatering, the polymerization that heats up under 140 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 32000～36000 107 silicon rubber.
Embodiment 11
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 20ppm reagent A (reagent A is calcium sulfite and gac), add 20ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 5.5gKOH after 50 ℃～120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 55ppmKOH alkali glue after material dewatering, the polymerization that heats up under 120 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 20000～29000 107 silicon rubber.
Embodiment 12
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 30ppm reagent A (reagent A is calcium sulfite and gac), add 30ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 5.5gKOH after 50 ℃～120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 30ppmKOH alkali glue after material dewatering, the polymerization that heats up under 140 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 20000～25000 107 silicon rubber.
Claims (9)
1. the preparation method of the controlled hydroxyl endblocked polydimethylsiloxane of a viscosity comprises the following steps:
1): the pre-treatment of organosilane monomer hydrolyzate, organosilane monomer hydrolyzate and water are fed intake as 15:4 ~ 5 take the mass ratio that feeds intake, under 50 ℃ of conditions, stirring velocity with 60r/min fully mixes, add reagent A, add reagent B after stirring 30min, regulate pH to 7.1, standing, separate;
2): catalyzer KOH alkali glue synthetic, with the mixture of DMC(hexam ethylcyclotrisiloxane ~ ten tetramethyl-seven silane) carry out polymerization with KOH at 80 ~ 180 ℃ after dehydration, further preferably temperature is 130 ~ 150 ℃;
3): with the hydrolyzate of pre-treatment after dehydration under vacuum, add the polymerization that heats up of catalyzer KOH alkali glue, add with the phosphoric acid neutralization after reaching required viscosity, the reaction system after neutralization removes low molecule to flowing out without cut under vacuum, be hydroxyl endblocked polydimethylsiloxane.
2. the controlled hydroxyl endblocked polydimethylsiloxane of viscosity according to claim 1, is characterized in that, the viscosity of hydroxyl endblocked polydimethylsiloxane can be controlled in 20000 ~ 80000mPa.s.
3. the controlled hydroxyl endblocked polydimethylsiloxane of viscosity according to claim 1, it is characterized in that, in the pretreatment process of hydrolyzate, reagent A is one or more in anionite-exchange resin, calcium sulfite, gac, Silver Nitrate etc., the input quality of its Synergist S-421 95 is 5 ~ 150ppm of hydrolyzate, and further preferred input quality is 20 ~ 30ppm of hydrolyzate.
4. the controlled hydroxyl endblocked polydimethylsiloxane of viscosity according to claim 1, it is characterized in that, in the pretreatment process of hydrolyzate, reagent B is ammoniacal liquor, and it is 5 ~ 150ppm of hydrolyzate that ammoniacal liquor drops into quality, and further preferred input quality is 20 ~ 30ppm of hydrolyzate.
5. the controlled hydroxyl endblocked polydimethylsiloxane of viscosity according to claim 1, is characterized in that, in synthetic KOH alkali glue, the mass ratio that feeds intake of DMC and KOH is 30:1 ~ 1.1.
6. the controlled hydroxyl endblocked polydimethylsiloxane of viscosity according to claim 1, is characterized in that, the input quality of catalyzer KOH alkali glue is 5 ~ 150ppm of total reaction system, and further preferred input quality is 30 ~ 55ppm of total reaction system.
7. the controlled hydroxyl endblocked polydimethylsiloxane of viscosity according to claim 1, is characterized in that, the mass concentration of phosphate aqueous solution is 5～50%, and further the mass concentration of preferably phosphoric acid is 30%; It drops into quality is 5～150ppm of reaction system, and it drops into quality is 70 ~ 80ppm of reaction system.
8. the controlled hydroxyl endblocked polydimethylsiloxane of viscosity according to claim 1, is characterized in that, hydrolyzate is 100 ~ 140 ℃ with the polymerization temperature of catalyzer KOH alkali glue under vacuum.
9. the controlled hydroxyl endblocked polydimethylsiloxane of viscosity according to claim 1, is characterized in that, taking off low molecule temperature is 200 ~ 220 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204995A (en) * | 2013-03-04 | 2013-07-17 | 东莞新东方科技有限公司 | Method for preparing 107 glue |
| CN103435807A (en) * | 2013-08-01 | 2013-12-11 | 广东信翼新材料股份有限公司 | Method for preparing odorless and transparent 107 glue at ordinary pressure |
| CN108912331A (en) * | 2018-07-23 | 2018-11-30 | 湖北兴瑞硅材料有限公司 | A kind of synthetic method of low viscosity methyl silicone rubber at room temperature cure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101928399A (en) * | 2010-08-20 | 2010-12-29 | 浙江中天氟硅材料有限公司 | Preparation method for 107 silicon rubber with controllable viscosity |
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2013
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101928399A (en) * | 2010-08-20 | 2010-12-29 | 浙江中天氟硅材料有限公司 | Preparation method for 107 silicon rubber with controllable viscosity |
Non-Patent Citations (1)
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| 苗刚；陈海平: "甲基氯硅烷水解物合成107硅橡胶工艺的改进", 《有机硅材料》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204995A (en) * | 2013-03-04 | 2013-07-17 | 东莞新东方科技有限公司 | Method for preparing 107 glue |
| CN103435807A (en) * | 2013-08-01 | 2013-12-11 | 广东信翼新材料股份有限公司 | Method for preparing odorless and transparent 107 glue at ordinary pressure |
| CN108912331A (en) * | 2018-07-23 | 2018-11-30 | 湖北兴瑞硅材料有限公司 | A kind of synthetic method of low viscosity methyl silicone rubber at room temperature cure |
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