CN105254893A - Low-viscosity 107 silicone rubber and preparation method thereof - Google Patents
Low-viscosity 107 silicone rubber and preparation method thereof Download PDFInfo
- Publication number
- CN105254893A CN105254893A CN201510830441.9A CN201510830441A CN105254893A CN 105254893 A CN105254893 A CN 105254893A CN 201510830441 A CN201510830441 A CN 201510830441A CN 105254893 A CN105254893 A CN 105254893A
- Authority
- CN
- China
- Prior art keywords
- preparation
- reaction
- viscosity
- silicon rubber
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Silicon Polymers (AREA)
Abstract
The invention relates to the field of adhesives, in particular to low-viscosity 107 silicone rubber and a preparation method thereof, and aims at providing the low-viscosity 107 silicone rubber preparation method which is simple in reaction process control and stable in product viscosity. The method specifically comprises the steps of 1 dewatering, wherein in a non-vacuum state, decompression dewatering are performed on dimethyl siloxane mixed ring bodies at the temperature of 80 DEG C-100 DEG C for 0.5-1.5 hours; 2 catalyzing, wherein a basic catalyst is added when the temperature is increased to 100 DEG C-115 DEG C, the temperature is increased continuously, the reaction temperature is controlled at 130 DEG C-160 DEG C, and the balanced reaction time is controlled for 0.5-1.5 hours; 3 degrading, wherein degrading is performed by adding water; 4 neutralizing, wherein a neutralization reaction is performed by adding a neutralizing agent; 5 fraction collecting, wherein vacuum is started after the neutralization reaction, the materials are heated to reach the temperature of 120 DEG C-195 DEG C, the vacuum degree is controlled and kept at negative 0.08 MPa-negative 0.098 MPa, and fractions are collected until no fraction is dropped. The preparation method is high in yield, and the obtained low-viscosity 107 silicone rubber can be widely applied to electronic industry and aviation and military industry.
Description
Technical field
The present invention relates to glue paste field, be specifically related to a kind of low viscosity 107 silicon rubber and preparation method thereof.
Background technology
In organosilicon series product, α, alpha, omega-dihydroxy polydimethyl siloxane (being called for short 107 silicon rubber) is one of staple product in silicon rubber, in many aspects as the fields such as building, coating, industrial art all have a wide range of applications.Particularly in recent years along with a large amount of employings of the industrialization of Building Trade in China, seriation, high level and superelevation stratification, lighting and full field of view system and large-scale framework cladding panel structure, more and more higher to the requirement of sealing material.
The concrete technology that prior art prepares 107 silicon rubber is: dimethyl siloxane mixes ring body (being called for short DMC) and first dewaters at certain temperature and vacuum degree condition, after being warming up to certain temperature, add basic catalyst, ring-opening polymerization is to certain viscosity, rear intensification destroys basic catalyst, then product is carried out de-reduction process.The more difficult control of this technique pilot process, there is unstable in control process.
Summary of the invention
It is simple that the object of the invention is to provide a kind of reaction process to control, the preparation method of low viscosity 107 silicon rubber that product viscosity is stable, and be adopt alkali to make catalyzer in the method, distilled water does end-capping reagent.The viscosity of the present invention 107 silicon rubber is 2000mPas ~ 3000mPas.
Concrete, the preparation method of low viscosity 107 silicon rubber of the present invention, comprises the steps:
A, dehydration: under non-vacuum, dimethyl siloxane mixes ring body under the condition of 80 DEG C ~ 100 DEG C, decompression dehydration 0.5 ~ 1.5 hour;
B, catalysis: add basic catalyst when being warming up to 100 ~ 115 DEG C, continue to heat up, and controls temperature of reaction at 130 ~ 160 DEG C, by balanced reaction time controling at 0.5 ~ 1.5 hour;
C, degraded: add water degraded;
D, neutralization: add neutralizing agent and carry out neutralization reaction;
E, collection cut: after neutralization reaction, open vacuum, and heated material temperature reaches 120 ~ 195 DEG C (preferably 190 DEG C), control and maintain vacuum tightness be-0.08MPa ~-0.098MPa (preferably-0.095MPa ~-0.098MPa), collect cut, till oozing without cut.
In technique scheme, the weight proportion of each material is: dimethyl siloxane mixes ring body 3500 parts, basic catalyst 0.01 ~ 0.07 part, distilled water 3.4 ~ 17 parts, and the number of neutralizing agent is 0.015 ~ 0.105 part;
Further preferably, the weight proportion of each material is: dimethyl siloxane mix ring body 3500 parts, basic catalyst 0.01 ~ 0.07 part, distilled water 7 parts, neutralizing agent at least with the molar mass such as basic catalyst.
In technique scheme, basic catalyst comprises: at least one in the saline and alkaline glue of silanol of the saline and alkaline glue of silanol of potassium hydroxide, Tetramethylammonium hydroxide, tetrabutylammonium hydroxide phosphorus or potassium hydroxide, the saline and alkaline glue of silanol of Tetramethylammonium hydroxide, tetrabutylammonium hydroxide phosphorus.
In technique scheme, described neutralizing agent comprises: at least one in carbonic acid gas, silica-based phosphoric acid ester, phosphoric acid.
In technique scheme, reaction carries out in the conversion unit with whipping appts and condensing works.
In technique scheme, balanced reaction time during step B catalysis preferably controls at 0.5 ~ 1h.
In technique scheme, temperature of reaction during step B catalysis is preferably 140 ~ 160 DEG C.
In technique scheme, during steps A dehydration, logical rare gas element (preferred nitrogen) enters in conversion unit in advance, and ensures that whole reaction process is carried out under nitrogen protection.
In technique scheme, step e is collected in cut, and de-low temperature 120 ~ 190 DEG C, vacuum tightness is-0.08MPa ~-0.098MPa, and preferred vacuum tightness is-0.095MPa ~-0.098MPa.Contriver finds through test, when 120 DEG C, has small molecules and therefrom evaporates, and along with the rising of temperature, it is more and more that small molecules is deviate from, and when temperature reaches 190 DEG C, nearly all small molecules can therefrom be deviate from, therefore select de-low temperature to be 120 ~ 195 DEG C.
Key improvements point of the present invention is, 107 silicon rubber preparation methods in the past control reaction to be in vacuum state in whole technical process.But the present invention reacts under the non-vacuum in steps A dehydration, step B catalysis, step C degraded, step D with all at atmosphere, and only heat up in a steamer Time-sharing control reaction system in collection and be in vacuum state, such benefit is controlled by above-mentioned steps, and 107 silicone rubber products transparencies of preparation are higher, even molecular weight distribution.
The viscosity of 107 silicon rubber prepared by the inventive method is lower, and be generally 2000 ~ 3000mPas, transparency is higher, and molecular weight distribution is comparatively even, molecular weight ranges 36000 ~ 40000.Low viscosity 107 silicon rubber mostly in the market be from organosilicon hydrolyzation material be raw material, the product transparency of preparation is lower, and turbidity scope is 7 ~ 9, and molecular weight distribution is wider, molecular weight ranges is 18000 ~ 58000, can not be used for the preparation of high transparency silicone adhesive.The present invention is from DMC, and the low viscosity 107 silicone rubber products transparency of preparation is higher, even molecular weight distribution, may be used for the production of high-end silicone adhesive.
The invention has the beneficial effects as follows: by effectively controlling above-mentioned reaction conditions, low viscosity 107 silicone rubber products can be obtained, low viscosity 107 silicone rubber products tool in current electronic industry and aviation and war industry has been widely used and higher marketable value, this invention is from the raw material DMC that is easy to get, adopt base catalysis composition principle, for the preparation of low viscosity 107 silicon rubber provides a kind of new Controlling Technology and method, preparation technology is simple, product viscosity is stablized, yield is high, can meet the needs of actual production.
Embodiment
Shaker test is below adopted to show the beneficial effect of preparation method of the present invention.
In the four-hole boiling flask of 5000ml, add 3500g dimethyl siloxane mixed methylcyclosiloxane, heating, stirs, decompression dehydration 0.5 hour when about 80 DEG C simultaneously.Continue to heat up, when temperature is increased to 100 ~ 115 DEG C, add catalyzer potassium hydroxide, continue to heat up, control temperature of reaction at 130 ~ 160 DEG C, material viscosity increases gradually, to control in reaction times at 0.5 ~ 1.5 hour, and then add distilled water and degrade, add phosphoric acid after degraded terminates and carry out neutralization reaction, neutralization terminates rear unlatching vacuum, be heated to temperature of charge and reach 190 DEG C, vacuum tightness >-0.095MPa, maintain this vacuum tightness, till oozing without cut.
1. temperature of reaction is on the impact of product
Siloxane bond in ring body will be fragmented into macromolecular compound by strong alkaline substance in theory more than 120 DEG C, and speed of reaction also can present the trend of rise along with the rising of temperature of reaction, but too high temperature also can cause the difficulty of reaction controlling to strengthen, therefore the temperature of reaction that this experiment adopts controls at 130 ~ 160 DEG C, choose 130 DEG C, 135 DEG C, 140 DEG C, 145 DEG C, 150 DEG C, 155 DEG C, 160 DEG C of seven points carry out simultaneous test, catalyzer is KOH, consumption is 0.05g, polymerization time is 55min, amount of water is 7g, degradation time is 1h, phosphoric acid add-on is 0.058g, in and the time be 40min, then underpressure distillation is carried out, deviate from low molecule.The data obtained are as table 1:
Table 1 temperature of reaction is on the impact of product
As can be seen from Table 1, the rising of temperature can improve speed of reaction effectively, and then improves the viscosity of product, and the transformation efficiency of reaction also improves thereupon.But in an experiment, if temperature is too high, then the viscosity of product will become uncontrolled, stir and also become more difficult, so select 155 DEG C as temperature of reaction.
2, the add-on of catalyzer is on the impact of product
The add-on of catalyzer has considerable influence to product.It is very few that catalyzer adds, and catalytic effect is not obvious, if add too many, then affect outward appearance and the viscosity of product.Raw material add-on 3500g, dewatering time 30min, catalyst levels is 0.01g ~ 0.07g, and polymerization time is 55min, and amount of water is 7g, and degradation time is 1h, investigates the consumption of catalyzer to the impact of product.
The impact of table 2 catalyst levels and low viscosity 107 silicon rubber viscosity
As can be seen from Table 2, the viscosity of product increases along with the increase of catalyzer, but when the add-on of catalyzer is too much, has considerable influence to the outward appearance of product.Because the product produced must meet Standard, namely product is required to be colourless transparent liquid, and the catalyst charge therefore selected is 0.05g.
3, the add-on of water is on the impact of product
Dimethyl siloxane mixed methylcyclosiloxane polymerization reaction take place in the presence of a catalyst, after polymerization reaches certain hour, need add the viscosity of water to product and degrade, the addition of water directly has influence on the final viscosity of product.7 kinds of different additions are selected to observe the impact of water on product viscosity, as shown in table 3:
The add-on of table 3 water is on the impact of product
As can be seen from Table 3, the addition of water and the slightly inversely proportional function of the viscosity of 107 silicon rubber, the addition of water is more, and the viscosity of 107 silicon rubber is lower.This is because a water molecules disconnects a silica silicon key, generate two hydroxyls.But under the condition of degraded, hydroxyl is also very easy to be condensed into water, so this is a running balance, finally can generates the condition how many hydroxyls depend on reaction, when the water yield is many, easily generate hydroxyl, so will ensure there is enough water in liquid phase as far as possible.But along with the addition of water constantly increases, though the once downtrending of the viscosity of product, but system occurs muddy, and the turbidity of product also declines thereupon.Therefore the addition of the water of this experimental selection is 7g.This experiment 6 and 7 sample that does, viscosity is respectively 1700mPas and 1050mPas, but product appearance but some muddiness, non-leuco clear viscous liquids, does not meet index request.
4, the reaction times is on the impact of product
The scope in reaction times is at 30 ~ 60min, every 5 minutes as an experimental study point, experiment condition: raw material add-on 3500g, dewatering time 30min, catalyst levels is 0.05g, amount of water is 7g, degradation time is 1h, and phosphoric acid add-on is 0.058g, in and the time be 40min, then carry out underpressure distillation, deviate from low molecule.Obtain result as table 4:
Table 4 reaction times is on the impact of product viscosity
As can be seen from Table 4, along with the prolongation of time, the viscosity of product can increase thereupon, but when viscosity is excessive, the degraded after product can go wrong thereupon, therefore selects the polymerization time of product to be 55min.
The present invention have studied the preparation process of 107 silicon rubber of 2000mPas ~ 3000mPas viscosity, and emphasis have studied the impact of each reaction conditions on product.By investigating each reaction conditions and adjustment preparation technology, preparing low viscous 107 silicon rubber, having drawn to draw a conclusion:
1) investigate different temperature of reaction to the impact of product viscosity by simultaneous test, determine that preferably temperature of reaction is 155 DEG C.
2) investigate the different reaction times to the impact of product viscosity by simultaneous test, to determine polymerization reaction time be 55min.
3) investigate different catalyst charge to the impact of product viscosity by simultaneous test, the add-on determining catalyzer is 0.05g.
4) add-on being investigated different water by simultaneous test, on the impact of product viscosity and turbidity, determines the add-on of water.
5) 2500mPas and the 3000mPas107 silicon rubber index property utilizing this test method to prepare is more stable, and has supplied client's use.
Example of preparing of the present invention is below adopted to show beneficial effect of the present invention.
Embodiment 1
By following raw material weight proportioning: 3500g dimethyl siloxane mixed methylcyclosiloxane joins in the vessel with whipping appts and condensing works, and heating, opens stirring simultaneously, decompression dehydration 0.5 hour when being warming up to 95 DEG C.Continue to heat up, 0.05g potassium hydroxide basic catalyzer is added when temperature is increased to 115 DEG C, continue to heat up, control temperature of reaction at 155 DEG C, material viscosity increases gradually, by balanced reaction time controling at 50min, then add 7g distilled water to degrade, the phosphoric acid adding etc. molar mass after degraded terminates carries out neutralization reaction, neutralization terminates rear slow unlatching vacuum, be heated to temperature of charge and reach 190 DEG C, vacuum tightness >-0.095MPa, maintain this vacuum tightness, till oozing without cut.Obtain water white 107 silicone rubber products that 2981g (25 DEG C) viscosity is 2000mPas.Yield is 85%.
Embodiment 2
By following raw material weight proportioning: 3500g dimethyl siloxane mixed methylcyclosiloxane joins in the vessel with whipping appts and condensing works, and heating, opens stirring simultaneously, decompression dehydration 0.5 hour when being warming up to 95 DEG C.Continue to heat up, 0.05g potassium hydroxide basic catalyzer is added when temperature is increased to 115 DEG C, continue to heat up, control temperature of reaction at 160 DEG C, material viscosity increases gradually, by balanced reaction time controling at 55min, then add 7g distilled water to degrade, the phosphoric acid adding etc. molar mass after degraded terminates carries out neutralization reaction, neutralization terminates rear slow unlatching vacuum, be heated to temperature of charge and reach 190 DEG C, vacuum tightness >-0.095MPa, maintain this vacuum tightness, till oozing without cut.Obtain water white 107 silicone rubber products that 3086.2g (25 DEG C) viscosity is 2600mPas.Yield is 88%.
Embodiment 3
By following raw material weight proportioning: 3500g dimethyl siloxane mixed methylcyclosiloxane joins in the vessel with whipping appts and condensing works, and heating, opens stirring simultaneously, decompression dehydration 0.5 hour when being warming up to 95 DEG C.Continue to heat up, 0.05g potassium hydroxide basic catalyzer is added when temperature is increased to 115 DEG C, continue to heat up, control temperature of reaction at 155 DEG C, material viscosity increases gradually, by balanced reaction time controling at 58min, then add 7g distilled water to degrade, the phosphoric acid adding 0.075g after degraded terminates carries out neutralization reaction, neutralization terminates rear slow unlatching vacuum, be heated to temperature of charge and reach 175 DEG C, vacuum tightness >-0.095MPa, maintain this vacuum tightness, till oozing without cut.Obtain water white 107 silicone rubber products that 3325g (25 DEG C) viscosity is 2550mPas.Yield is 95%.
Embodiment 4
By following raw material weight proportioning: 3500g dimethyl siloxane mixed methylcyclosiloxane joins in the vessel with whipping appts and condensing works, and heating, opens stirring simultaneously, decompression dehydration 0.5 hour when being warming up to 95 DEG C.Continue to heat up, 0.05g potassium hydroxide basic catalyzer is added when temperature is increased to 115 DEG C, continue to heat up, control temperature of reaction at 155 DEG C, material viscosity increases gradually, by balanced reaction time controling at 50min, then add 7g distilled water to degrade, the phosphoric acid adding 0.075g after degraded terminates carries out neutralization reaction, neutralization terminates rear slow unlatching vacuum, be heated to temperature of charge and reach 190 DEG C, vacuum tightness >-0.095MPa, maintain this vacuum tightness, till oozing without cut.Obtain water white 107 silicone rubber products that 3080g (25 DEG C) viscosity is 2500mPas.Yield is 88%.
Embodiment 5
By following raw material weight proportioning: 3500g dimethyl siloxane mixed methylcyclosiloxane joins in the vessel with whipping appts and condensing works, and heating, opens stirring simultaneously, decompression dehydration 0.5 hour when being warming up to 95 DEG C.Continue to heat up, 0.05g potassium hydroxide basic catalyzer is added when temperature is increased to 115 DEG C, continue to heat up, control temperature of reaction at 155 DEG C, material viscosity increases gradually, by balanced reaction time controling at 60min, then add 7g distilled water to degrade, the phosphoric acid adding etc. molar mass after degraded terminates carries out neutralization reaction, neutralization terminates rear slow unlatching vacuum, be heated to temperature of charge and reach 180 DEG C, vacuum tightness >-0.095MPa, maintain this vacuum tightness, till oozing without cut.Obtain water white 107 silicone rubber products that 3290g (25 DEG C) viscosity is 2550mPas.Yield is 94%.
Embodiment 6
By following raw material weight proportioning: 3500g dimethyl siloxane mixed methylcyclosiloxane joins in the vessel with whipping appts and condensing works, and heating, opens stirring simultaneously, decompression dehydration 0.5 hour when being warming up to 95 DEG C.Continue to heat up, 0.05g potassium hydroxide basic catalyzer is added when temperature is increased to 115 DEG C, continue to heat up, control temperature of reaction at 155 DEG C, material viscosity increases gradually, by balanced reaction time controling at 55min, then add 7g distilled water to degrade, the phosphoric acid adding etc. molar mass after degraded terminates carries out neutralization reaction, neutralization terminates rear slow unlatching vacuum, be heated to temperature of charge and reach 190 DEG C, vacuum tightness >-0.095MPa, maintain this vacuum tightness, till oozing without cut.Obtain water white 107 silicone rubber products that 3226.5g (25 DEG C) viscosity is 2500mPas.Yield is 92%.
The product analysis of embodiment 1-6 the results are shown in Table 6:
Table 6: product analysis result
Note: industry standard: turbidity≤3 are acceptable end products; ≤ 7 is salable product.
As seen from the experiment, 107 silicone rubber products prepared by the present invention, viscosity is all at 2000 ~ 2600mPas, and viscosity is lower, the higher and stable processing technique of transparency, circulation ratio and operability better.
Claims (10)
1. low viscosity 107 silicon rubber preparation method, it is characterized in that: comprise the steps:
A, dehydration: under non-vacuum, dimethyl siloxane mixes ring body under the condition of 80 DEG C ~ 100 DEG C, decompression dehydration 0.5 ~ 1.5 hour;
B, catalysis: add basic catalyst when being warming up to 100 ~ 115 DEG C, continue to heat up, and controls temperature of reaction at 130 ~ 160 DEG C, by balanced reaction time controling at 0.5 ~ 1.5 hour;
C, degraded: add water degraded;
D, neutralization: add neutralizing agent and carry out neutralization reaction;
E, collection cut: open vacuum after neutralization reaction, and heated material temperature reaches 120 ~ 195 DEG C, control and maintain vacuum tightness-0.08MPa ~-0.098MPa, collect cut, till oozing without cut;
Preferably, step e heated material temperature reaches 190 DEG C;
Preferably, step e maintains vacuum tightness-0.095MPa ~-0.098MPa.
2. low viscosity 107 silicon rubber according to claim 1 preparation method, it is characterized in that: the weight proportion of each material is: dimethyl siloxane mixes ring body 3500 parts, basic catalyst 0.01 ~ 0.07 part, distilled water 3.4 ~ 17 parts, the number of neutralizing agent is 0.015 ~ 0.105 part;
Preferably, the weight proportion of each material is: dimethyl siloxane mix ring body 3500 parts, basic catalyst 0.01 ~ 0.07 part, distilled water 7 parts, neutralizing agent at least with the molar masss such as basic catalyst.
3. low viscosity 107 silicon rubber according to claim 1 and 2 preparation method, it is characterized in that: described basic catalyst comprises: at least one in the saline and alkaline glue of silanol of the saline and alkaline glue of silanol of potassium hydroxide, Tetramethylammonium hydroxide, tetrabutylammonium hydroxide phosphorus or potassium hydroxide, the saline and alkaline glue of silanol of Tetramethylammonium hydroxide, tetrabutylammonium hydroxide phosphorus.
4. low viscosity 107 silicon rubber according to claim 1 and 2 preparation method, it is characterized in that: described neutralizing agent comprises: at least one in carbonic acid gas, silica-based phosphoric acid ester, phosphoric acid.
5. low viscosity 107 silicon rubber according to claim 1 preparation method, it is characterized in that: reaction carries out in the conversion unit with whipping appts and condensing works.
6. low viscosity 107 silicon rubber according to claim 1 preparation method, it is characterized in that: during steps A dehydration, logical nitrogen enters conversion unit in advance, and whole reaction process is carried out under protection of inert gas;
Preferably, described rare gas element is nitrogen.
7. low viscosity 107 silicon rubber according to claim 1 preparation method, it is characterized in that: balanced reaction time controling during step B catalysis is at 0.5 ~ 1h.
8. low viscosity 107 silicon rubber according to claim 1 preparation method, it is characterized in that: temperature of reaction during step B catalysis is preferably 140 ~ 160 DEG C.
9. low viscosity 107 silicon rubber according to claim 1 preparation method, it is characterized in that: step e is collected in cut, de-low temperature 120 ~ 190 DEG C.
10. the preparation method described in any one of claim 1-9 prepares low viscosity 107 silicon rubber of gained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510830441.9A CN105254893B (en) | 2015-11-25 | 2015-11-25 | A kind of silicon rubber of low viscosity 107 and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510830441.9A CN105254893B (en) | 2015-11-25 | 2015-11-25 | A kind of silicon rubber of low viscosity 107 and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105254893A true CN105254893A (en) | 2016-01-20 |
| CN105254893B CN105254893B (en) | 2018-02-16 |
Family
ID=55094861
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510830441.9A Expired - Fee Related CN105254893B (en) | 2015-11-25 | 2015-11-25 | A kind of silicon rubber of low viscosity 107 and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105254893B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105801863A (en) * | 2016-05-10 | 2016-07-27 | 山东大学 | Preparation method of hydroxyl-terminated poly(diethyldimethyl)siloxane |
| CN106279696A (en) * | 2016-09-27 | 2017-01-04 | 枣阳市华威硅氟材料有限公司 | A kind of production system of 107 silicone rubber |
| 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 |
| CN111087620A (en) * | 2019-12-31 | 2020-05-01 | 枣阳市金鹏化工有限公司 | Method for synthesizing 201 methyl silicone oil from waste silicone rubber |
| CN111154106A (en) * | 2019-12-30 | 2020-05-15 | 枣阳市金鹏化工有限公司 | Novel high-viscosity 107 glue and preparation method thereof |
| CN114561014A (en) * | 2022-03-21 | 2022-05-31 | 内蒙古恒星化学有限公司 | Method for synthesizing glue 107 and glue 107 |
| CN114573813A (en) * | 2022-03-07 | 2022-06-03 | 新疆西部合盛硅业有限公司 | Catalyst and process for preparing 107 glue |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101173044A (en) * | 2007-10-30 | 2008-05-07 | 江苏宏达新材料股份有限公司 | Method for producing 107 adhesive by comprehensive utilization of organosilicon hydrolyzation material loop separation |
| CN102604103A (en) * | 2012-04-11 | 2012-07-25 | 唐山三友硅业有限责任公司 | Preparation method of low volatile matter room temperature vulcanization methyl silicone rubber |
| 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 |
-
2015
- 2015-11-25 CN CN201510830441.9A patent/CN105254893B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101173044A (en) * | 2007-10-30 | 2008-05-07 | 江苏宏达新材料股份有限公司 | Method for producing 107 adhesive by comprehensive utilization of organosilicon hydrolyzation material loop separation |
| CN102604103A (en) * | 2012-04-11 | 2012-07-25 | 唐山三友硅业有限责任公司 | Preparation method of low volatile matter room temperature vulcanization methyl silicone rubber |
| 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 |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105801863A (en) * | 2016-05-10 | 2016-07-27 | 山东大学 | Preparation method of hydroxyl-terminated poly(diethyldimethyl)siloxane |
| CN105801863B (en) * | 2016-05-10 | 2021-04-02 | 山东大学 | Preparation method of hydroxyl-terminated polymethylethylsiloxane |
| CN106279696A (en) * | 2016-09-27 | 2017-01-04 | 枣阳市华威硅氟材料有限公司 | A kind of production system of 107 silicone rubber |
| 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 |
| CN111154106A (en) * | 2019-12-30 | 2020-05-15 | 枣阳市金鹏化工有限公司 | Novel high-viscosity 107 glue and preparation method thereof |
| CN111087620A (en) * | 2019-12-31 | 2020-05-01 | 枣阳市金鹏化工有限公司 | Method for synthesizing 201 methyl silicone oil from waste silicone rubber |
| CN114573813A (en) * | 2022-03-07 | 2022-06-03 | 新疆西部合盛硅业有限公司 | Catalyst and process for preparing 107 glue |
| CN114561014A (en) * | 2022-03-21 | 2022-05-31 | 内蒙古恒星化学有限公司 | Method for synthesizing glue 107 and glue 107 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105254893B (en) | 2018-02-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105254893A (en) | Low-viscosity 107 silicone rubber and preparation method thereof | |
| CN101509196B (en) | Method of preparing epoxy modified amino-silicone oil softening agent | |
| CN102690387B (en) | Resin used for serum separating gel, serum separating gel and preparation methods of resin used for serum separating gel | |
| US20220056209A1 (en) | Method for preparing reactive sealant resin | |
| CN104829838A (en) | Preparation method of hydroxyl terminated polyfluorosiloxane | |
| CN105175730A (en) | Method for preparing silicone rubber from organosilicon hydrolysate | |
| CN105801868A (en) | Preparing method of bifunctionality epoxy resin emulsifier and emulsion | |
| CN105238085B (en) | A kind of epoxy terminated SBS modified pitch and preparation method thereof that heat-storage is stablized | |
| CN103044636A (en) | Preparation method of enzymatically hydrolyzed sericin protein composite absorbent material | |
| CN111072969A (en) | Preparation method of viscosity-controllable hydroxyl-terminated polymethylphenylsiloxane | |
| CN105131296B (en) | A kind of self-cross linking type LED encapsulation gum resin and preparation method thereof | |
| CN111560119A (en) | Preparation method of dimethyl diphenyl polysiloxane | |
| CN107522807A (en) | Preparation method of catalyst for preparing rare earth butadiene rubber | |
| CN105131297A (en) | Phenyl vinyl MQ resin and preparation method thereof | |
| CN105153480B (en) | A kind of method and application preparing its liquid crystalline phase by regulating and controlling sodium alginate molecular weight distribution | |
| CN114437020A (en) | Preparation method of glycolide | |
| Kalinina et al. | Hydrolytic polycondensation of methylalkoxysilanes under pressure | |
| CN103755864B (en) | A kind of preparation method of fluorescence lucite | |
| CN1807437A (en) | Organophosphorus ester preparation method | |
| CN104831364A (en) | Method for surface modification of calcium sulfate whiskers | |
| CN109776801A (en) | A kind of preparation method of phenyl silicone oil | |
| CN106349277A (en) | Method for preparing alkoxy-terminated polymethyltrifluoropropyl siloxane oligomers | |
| CN112442174A (en) | Radiation-resistant phenyl silicone rubber and preparation method and application thereof | |
| CN105086988A (en) | Low-carbon-hydrocarbon anhydrous fracturing fluid gelling agent and preparation method thereof | |
| CN103965384A (en) | Preparation method of polymethyl methacrylate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180216 Termination date: 20191125 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |