CN106478951A - A kind of preparation method of LED packaging plastic methyl and phenyl hydrogen-containing silicon oil - Google Patents
A kind of preparation method of LED packaging plastic methyl and phenyl hydrogen-containing silicon oil Download PDFInfo
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- CN106478951A CN106478951A CN201610906890.1A CN201610906890A CN106478951A CN 106478951 A CN106478951 A CN 106478951A CN 201610906890 A CN201610906890 A CN 201610906890A CN 106478951 A CN106478951 A CN 106478951A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
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Abstract
The invention discloses a kind of preparation method of LED packaging plastic methyl and phenyl hydrogen-containing silicon oil.With aminomethyl phenyl dimethoxysilane as raw material, hydrochloric acid or acidic cationic resin are catalyst to the method, and Hydrolysis condensation reaction under condition of heating and stirring prepares aminomethyl phenyl end hydroxyl silicone oil；With the aminomethyl phenyl end hydroxyl silicone oil of above-mentioned preparation and tetramethyl tetrahydrochysene basic ring tetrasiloxane (D4 H) it is raw material, hexamethyl disiloxane (MM) or hydrogeneous double-seal head (MMH) it is end-capping reagent, acidic cationic resin is catalyst, reacts under condition of heating and stirring, and reaction terminates rear sucking filtration and removes catalyst, distills product at reduced pressure afterwards and methyl and phenyl hydrogen-containing silicon oil is obtained after removing low-boiling-point substance.Prepared containing hydrogen silicone oil is colorless transparent viscous liquid, and light transmittance, refractive index and active hydrogen content are high, and heat stability is good, can serve as LED packaging plastic material.
Description
Technical field
The present invention relates to LED packaging plastic technical field, specifically refer to a kind of LED packaging plastic methyl and phenyl hydrogen-containing silicon oil
Preparation method.
Background technology
Light-Emitting Diode (LED) has the series of advantages such as stable performance, efficient energy-saving, safety and environmental protection, normal lighting,
Be used widely in the fields such as car bulb, mobile phone and TV, it has also become the trend of following lighting engineering and trend.Encapsulating material
Select impact to LED performance most important, organosilicon material relies on its excellent heat stability, resistance to ag(e)ing, mechanicalness
Energy, optical property and moisture-proof, become the primary study direction of domestic and international LED encapsulation material.Therefore, develop excellent performance
Organosilicon encapsulating material significant for the lifting of China's LED encapsulation technology and the development of LED industry.
One of organosilicon encapsulating material research and development key link is exactly to synthesize that light transmittance and refractive index be high, heat stability is good
Containing hydrogen silicone oil, it requires even structure, highly transparent and refractive index more than 1.5.The LED packaging plastic reported both at home and abroad at present
With methyl and phenyl hydrogen-containing silicon oil mostly by forming containing silicane hydroxide and non-hydrogeneous hydrolyzing chlorosilane polycondensation.This preparation process needs
Using organic solvent, repeatability and controllability are poor, therefore there is the drawbacks of synthesis technique is complicated to pollute power consumption with production process.
Chinese patent CN104672455A discloses one kind strong acid catalyst cyclosiloxane ring-opening polymerisation and prepares aminomethyl phenyl
The method of containing hydrogen silicone oil, but the raw material (methyl phenyl ring siloxane) used in the method is condensed by hydrolyzing chlorosilane mostly
It is obtained, this preparation technology complex operation, the Pintsch process process that it is comprised and separating-purifying process considerably increase production
Difficulty and cost.
Therefore provide that a kind of synthesis technique is simple, preparation method that production process environmental protection and energy saving and raw materials for production are easy to get is system
Key for the good methyl and phenyl hydrogen-containing silicon oil of light transmittance and refractive index height, heat stability.
Content of the invention
The invention provides a kind of preparation method of LED packaging plastic methyl and phenyl hydrogen-containing silicon oil.The method prepares
Containing hydrogen silicone oil be colorless transparent viscous liquid, light transmittance, refractive index and active hydrogen content are high, and heat stability is good, Ke Yiyong
Make LED packaging plastic material.
The present invention is achieved through the following technical solutions：
A kind of preparation method of LED packaging plastic methyl and phenyl hydrogen-containing silicon oil it is characterised in that：
(1) with aminomethyl phenyl dimethoxysilane as raw material, hydrochloric acid or acidic cationic resin are catalyst, stir in heating
Hydrolysis condensation reaction under the conditions of mixing, prepares aminomethyl phenyl end hydroxyl silicone oil；Reaction mechanism formula is as follows：
(2) with the aminomethyl phenyl end hydroxyl silicone oil of above-mentioned preparation and tetramethyl tetrahydrochysene basic ring tetrasiloxane (D4 H) it is raw material,
Hexamethyl disiloxane (MM) or hydrogeneous double-seal head (MMH) it is end-capping reagent, acidic cationic resin is catalyst, in heated and stirred
Under the conditions of react, reaction terminates rear sucking filtration and removes catalyst, distills product at reduced pressure afterwards and methyl is obtained after removing low-boiling-point substance
Phenyl hydrogen-containing silicon oil.
Described in step (1) with hydrochloric acid for the reaction condition of catalyst preparation aminomethyl phenyl end hydroxyl silicone oil it is：Methylbenzene
Base dimethoxysilane is 1 with the mass ratio of hydrochloric acid:0.8-1:2；The concentration of hydrochloric acid is 1.5%-2.5% (mass fraction)；Instead
Temperature is answered to be 50-70 DEG C；Response time is 2-4 hour.
The reaction with hydrochloric acid for catalyst preparation aminomethyl phenyl end hydroxyl silicone oil described in step (1) is also located after following
Reason：By product with distilled water wash 3-4 time to neutral, then again by product removing system under the conditions of the 80 DEG C/- 0.096MPa
Moisture, thus be obtained water white aminomethyl phenyl end hydroxyl silicone oil.
The optimum response with acidic cationic resin for catalyst preparation aminomethyl phenyl end hydroxyl silicone oil described in step (1)
Condition is：Aminomethyl phenyl dimethoxysilane is 1 with the mass ratio of distilled water:0.8-1:2；The consumption of acidic cationic resin is
The 0.6%-1.2% of reactant gross weight；Reaction temperature is 60-80 DEG C；Response time is 2-4 hour.
The reaction also warp with acidic cationic resin for catalyst preparation aminomethyl phenyl end hydroxyl silicone oil described in step (1)
Following post processing：Product sucking filtration is removed acidic cationic resin, then again that product is de- under the conditions of 80 DEG C/- 0.096MPa
Except the moisture in system, thus water white aminomethyl phenyl end hydroxyl silicone oil is obtained.
The optimum reaction condition preparing methyl and phenyl hydrogen-containing silicon oil described in step (2) is：Aminomethyl phenyl end hydroxyl silicone oil
With D4 HMass ratio be 30:0-4:3；End-capping reagent consumption is the 1%-3% of total weight of monomer；Acidic cationic resin consumption is monomer
The 1%-2% of gross weight；Reaction temperature is 60-80 DEG C；Response time is 4-6 hour.
The described acidic cationic resin of step (1) (2) is CH-01 type acidic cationic resin.
The condition of the described vacuum distillation of step (2) is 200 DEG C/- 0.096MPa.
With respect to prior art, beneficial effects of the present invention are as follows：
(1) preparation process, from aminomethyl phenyl dimethoxysilane, first passes through hydrolysis-condensation reaction synthesis of methyl phenyl
End hydroxyl silicone oil.This hydrolytic condensation process single easy to control, impurity content is low, last handling process is simple, it is to avoid existing conjunction
Become the complicated technology of methyl phenyl ring siloxane.
(2) technological operation preparing methyl and phenyl hydrogen-containing silicon oil is simple, repeatability and controllability are good, without using organic molten
Agent energy-conserving and environment-protective.
(3) methyl and phenyl hydrogen-containing silicon oil prepared is colorless transparent viscous liquid, and light transmittance is high, heat stability is good, folding
Between 1.48-1.54, reactive hydrogen (mass percent) content, between 0.02%-0.7%, can serve as LED encapsulation to rate of penetrating
Glue material.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described, but scope of the present invention is not
It is confined to the involved scope of embodiment.
Embodiment 1
(1) hydrochloric acid that 40g mass fraction is 2.0% is taken to be added to the four-hole boiling flask equipped with mechanical agitation and temperature controller
In be preheated to 60 DEG C, be subsequently adding 50g aminomethyl phenyl dimethoxysilane and react 2 hours under the conditions of 60 DEG C.Question response terminates
Afterwards, by product with distilled water wash 3-4 time to neutral, then by product be transferred in round bottom distilling flask in 80 DEG C/-
Moisture in removing system under the conditions of 0.096MPa, thus be obtained water white aminomethyl phenyl end hydroxyl silicone oil.
(2) the aminomethyl phenyl end hydroxyl silicone oil taking the above-mentioned preparation of 30g is added to equipped with mechanical agitation and temperature controller
It is preheated to 60 DEG C in there-necked flask, be subsequently adding 0.89gMMHEnd-capping reagent and 0.31gCH-01 type acidic cationic resin are in 60 DEG C
Under the conditions of react 4 hours.After question response terminates, sucking filtration removes CH-01 type acidic cationic resin catalyst, then turns product
Move in round bottom distilling flask vacuum distillation removing low-boiling-point substance under the conditions of 200 DEG C/- 0.096MPa, thus water white transparency is obtained
Thick methyl and phenyl hydrogen-containing silicon oil.N after testingD 25=1.5425, H% (mass percent)=0.02%.
Embodiment 2
(1) hydrochloric acid that 40g mass fraction is 2.0% is taken to be added to the four-hole boiling flask equipped with mechanical agitation and temperature controller
In be preheated to 60 DEG C, be subsequently adding 50g aminomethyl phenyl dimethoxysilane and react 2 hours under the conditions of 60 DEG C.Question response terminates
Afterwards, by product with distilled water wash 3-4 time to neutral, then by product be transferred in round bottom distilling flask in 80 DEG C/-
Moisture in removing system under the conditions of 0.096MPa, thus be obtained water white aminomethyl phenyl end hydroxyl silicone oil.
(2) aminomethyl phenyl end hydroxyl silicone oil and the 15gD of the above-mentioned preparation of 30g are taken4 HIt is added to equipped with mechanical agitation and temperature control
It is preheated to 60 DEG C in the there-necked flask of device processed, be subsequently adding 1gMM end-capping reagent and 0.46gCH-01 type acidic cationic resin in 60
React 4 hours under the conditions of DEG C.After question response terminates, sucking filtration removes CH-01 type acidic cationic resin catalyst, then by product
It is transferred in round bottom distilling flask vacuum distillation removing low-boiling-point substance under the conditions of 200 DEG C/- 0.096MPa, thus being obtained colourless
Bright thick methyl and phenyl hydrogen-containing silicon oil.N after testingD 25=1.4970, H% (mass percent)=0.50%.
Embodiment 3
(1) hydrochloric acid that 40g mass fraction is 2.0% is taken to be added to the four-hole boiling flask equipped with mechanical agitation and temperature controller
In be preheated to 60 DEG C, be subsequently adding 50g aminomethyl phenyl dimethoxysilane and react 2 hours under the conditions of 60 DEG C.Question response terminates
Afterwards, by product with distilled water wash 3-4 time to neutral, then by product be transferred in round bottom distilling flask in 80 DEG C/-
Moisture in removing system under the conditions of 0.096MPa, thus be obtained water white aminomethyl phenyl end hydroxyl silicone oil.
(2) aminomethyl phenyl end hydroxyl silicone oil and the 15gD of the above-mentioned preparation of 30g are taken4 HIt is added to equipped with mechanical agitation and temperature control
It is preheated to 60 DEG C in the there-necked flask of device processed, be subsequently adding 1gMMHEnd-capping reagent and 0.46gCH-01 type acidic cationic resin in
React 4 hours under the conditions of 60 DEG C.After question response terminates, sucking filtration removes CH-01 type acidic cationic resin catalyst, then will produce
Thing is transferred in round bottom distilling flask vacuum distillation removing low-boiling-point substance under the conditions of 200 DEG C/- 0.096MPa, thus being obtained colourless
The methyl and phenyl hydrogen-containing silicon oil of clear viscous shape.N after testingD 25=1.4970, H% (mass percent)=0.53%.
Embodiment 4
(1) 50g aminomethyl phenyl dimethoxysilane and 40g distilled water is taken to be added to equipped with mechanical agitation and temperature controller
Four-hole boiling flask in be preheated to 60 DEG C, being subsequently adding 0.9gCH-01 type acidic cationic resin, to react 2 under the conditions of 60 DEG C little
When.After question response terminates, product sucking filtration is removed CH-01 type acidic cationic resin, then product is transferred to round bottom distillation
Moisture in removing system under the conditions of the 80 DEG C/- 0.096MPa in flask, thus be obtained water white aminomethyl phenyl terminal hydroxy group
Silicone oil.
(2) aminomethyl phenyl end hydroxyl silicone oil and the 15gD of the above-mentioned preparation of 30g are taken4 HIt is added to equipped with mechanical agitation and temperature control
It is preheated to 60 DEG C in the there-necked flask of device processed, be subsequently adding 1gMMHEnd-capping reagent and 0.46gCH-01 type acidic cationic resin in
React 4 hours under the conditions of 60 DEG C.After question response terminates, sucking filtration removes CH-01 type acidic cationic resin catalyst, then will produce
Thing is transferred in round bottom distilling flask vacuum distillation removing low-boiling-point substance under the conditions of 200 DEG C/- 0.096MPa, thus being obtained colourless
The methyl and phenyl hydrogen-containing silicon oil of clear viscous shape.N after testingD 25=1.4950, H% (mass percent)=0.50%.
Embodiment 5
(1) 50g aminomethyl phenyl dimethoxysilane and 40g distilled water is taken to be added to equipped with mechanical agitation and temperature controller
Four-hole boiling flask in be preheated to 60 DEG C, being subsequently adding 0.9gCH-01 type acidic cationic resin, to react 2 under the conditions of 60 DEG C little
When.After question response terminates, product sucking filtration is removed CH-01 type acidic cationic resin, then product is transferred to round bottom distillation
Moisture in removing system under the conditions of the 80 DEG C/- 0.096MPa in flask, thus be obtained water white aminomethyl phenyl terminal hydroxy group
Silicone oil.
(2) aminomethyl phenyl end hydroxyl silicone oil and the 15gD of the above-mentioned preparation of 20g are taken4 HIt is added to equipped with mechanical agitation and temperature control
It is preheated to 60 DEG C in the there-necked flask of device processed, be subsequently adding 1gMMHEnd-capping reagent and 0.36gCH-01 type acidic cationic resin in
React 4 hours under the conditions of 60 DEG C.After question response terminates, sucking filtration removes CH-01 type acidic cationic resin catalyst, then will produce
Thing is transferred in round bottom distilling flask vacuum distillation removing low-boiling-point substance under the conditions of 200 DEG C/- 0.096MPa, thus being obtained colourless
The methyl and phenyl hydrogen-containing silicon oil of clear viscous shape.N after testingD 25=1.4880, H% (mass percent)=0.7%.
Embodiment 6
(1) 100g aminomethyl phenyl dimethoxysilane and 80g distilled water is taken to be added to equipped with mechanical agitation and temperature control
It is preheated to 60 DEG C, being subsequently adding 1.8gCH-01 type acidic cationic resin, to react 2 under the conditions of 60 DEG C little in the four-hole boiling flask of device
When.After question response terminates, product sucking filtration is removed CH-01 type acidic cationic resin, then product is transferred to round bottom distillation
Moisture in removing system under the conditions of the 80 DEG C/- 0.096MPa in flask, thus be obtained water white aminomethyl phenyl terminal hydroxy group
Silicone oil.
(2) aminomethyl phenyl end hydroxyl silicone oil and the 15gD of the above-mentioned preparation of 40g are taken4 HIt is added to equipped with mechanical agitation and temperature control
It is preheated to 60 DEG C in the there-necked flask of device processed, be subsequently adding 1gMMHEnd-capping reagent and 0.56gCH-01 type acidic cationic resin in
React 4 hours under the conditions of 60 DEG C.After question response terminates, sucking filtration removes CH-01 type acidic cationic resin catalyst, then will produce
Thing is transferred in round bottom distilling flask vacuum distillation removing low-boiling-point substance under the conditions of 200 DEG C/- 0.096MPa, thus being obtained colourless
The methyl and phenyl hydrogen-containing silicon oil of clear viscous shape.N after testingD 25=1.5075, H% (mass percent)=0.41%.
Claims (10)
1. a kind of preparation method of LED packaging plastic methyl and phenyl hydrogen-containing silicon oil it is characterised in that
(1) with aminomethyl phenyl dimethoxysilane as raw material, hydrochloric acid or acidic cationic resin are catalyst, in heated and stirred bar
Hydrolysis condensation reaction under part, prepares aminomethyl phenyl end hydroxyl silicone oil；
(2) with the aminomethyl phenyl end hydroxyl silicone oil of above-mentioned preparation and tetramethyl tetrahydrochysene basic ring tetrasiloxane as raw material, hexamethyl two
Siloxanes or hydrogeneous double-seal head are end-capping reagent, and acidic cationic resin is catalyst, reacts under condition of heating and stirring, reaction knot
After bundle, sucking filtration removes catalyst, distills product at reduced pressure afterwards and methyl and phenyl hydrogen-containing silicon oil is obtained after removing low-boiling-point substance.
2. preparation method according to claim 1 it is characterised in that described in step (1) with hydrochloric acid as catalyst preparation
The reaction condition of aminomethyl phenyl end hydroxyl silicone oil is：Aminomethyl phenyl dimethoxysilane is 1 with the mass ratio of hydrochloric acid:0.8-1:2；
The concentration of hydrochloric acid is 1.5%-2.5% mass fraction；Reaction temperature is 50-70 DEG C；Response time is 2-4 hour.
3. preparation method according to claim 2 it is characterised in that described in step (1) with hydrochloric acid as catalyst preparation
The reaction of aminomethyl phenyl end hydroxyl silicone oil is also through following post processing：By product with distilled water wash 3-4 time to neutral, then again will
Moisture in product removing system under the conditions of the 80 DEG C/- 0.096MPa, thus be obtained water white aminomethyl phenyl terminal hydroxy group silicon
Oil.
4. preparation method according to claim 1 is it is characterised in that described in step (1) with acidic cationic resin be
The reaction condition of catalyst preparation aminomethyl phenyl end hydroxyl silicone oil is：Aminomethyl phenyl dimethoxysilane and the mass ratio of distilled water
For 1:0.8-1:2；The consumption of acidic cationic resin is the 0.6%-1.2% of reactant gross weight；Reaction temperature is 60-80 DEG C；
Response time is 2-4 hour.
5. preparation method according to claim 4 is it is characterised in that described in step (1) with acidic cationic resin be
The reaction of catalyst preparation aminomethyl phenyl end hydroxyl silicone oil is also through following post processing：Product sucking filtration is removed acid cation tree
Fat, then again by the moisture in product removing system under the conditions of the 80 DEG C/- 0.096MPa, thus be obtained water white methyl
Phenyl end hydroxyl silicone oil.
6. the preparation method according to claim 1 or 2 or 3 or 4 or 5 is it is characterised in that the described aminomethyl phenyl of step (2)
End hydroxyl silicone oil and mass ratio >=4 of tetramethyl tetrahydrochysene basic ring tetrasiloxane:3；End-capping reagent consumption is the 1%- of total weight of monomer
3%；Acidic cationic resin consumption is the 1%-2% of total weight of monomer.
7. preparation method according to claim 6 it is characterised in that the described aminomethyl phenyl end hydroxyl silicone oil of step (2) with
The mass ratio of tetramethyl tetrahydrochysene basic ring tetrasiloxane is 5:1-4:3.
8. preparation method according to claim 6 is it is characterised in that the described reaction temperature of step (2) is 60-80 DEG C；Instead
It is 4-6 hour between seasonable.
9. preparation method according to claim 8 is it is characterised in that the condition of the described vacuum distillation of step (2) is 200
℃/-0.096MPa.
10. the preparation method according to claim 1 or 2 or 3 or 4 or 5 is it is characterised in that the described acidity of step (1) (2)
Cationic resin is CH-01 type acidic cationic resin.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107189068A (en) * | 2017-05-27 | 2017-09-22 | 华南理工大学 | A kind of preparation method of dimethyl end hydroxyl silicone oil |
| CN108586747A (en) * | 2018-04-11 | 2018-09-28 | 杭州师范大学 | A kind of preparation method of middle high phenyl content methyl phenyl silicone oil |
| CN109485852A (en) * | 2018-10-13 | 2019-03-19 | 周群邦 | A kind of preparation method and applications of the ring-like structural hydroxyl polysiloxanes of band |
| CN111234228A (en) * | 2020-02-26 | 2020-06-05 | 华南理工大学 | Hydrogen-containing methyl phenyl silicone resin for LED packaging adhesive and preparation method and application thereof |
| CN111378135A (en) * | 2020-04-30 | 2020-07-07 | 新纳奇材料科技江苏有限公司 | Preparation method of low-viscosity alkoxy-terminated polydimethylsiloxane |
| CN113307974A (en) * | 2021-06-21 | 2021-08-27 | 江西蓝星星火有机硅有限公司 | Method for rapidly recovering hydrogen-containing silicone oil in acid |
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| CN115010929A (en) * | 2022-06-24 | 2022-09-06 | 江西蓝星星火有机硅有限公司 | Preparation method of hydroxyl-terminated vinyl silane prepolymer |
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| CN107189068B (en) * | 2017-05-27 | 2020-05-22 | 华南理工大学 | Preparation method of dimethyl-terminated hydroxyl silicone oil |
| CN107189068A (en) * | 2017-05-27 | 2017-09-22 | 华南理工大学 | A kind of preparation method of dimethyl end hydroxyl silicone oil |
| CN108586747A (en) * | 2018-04-11 | 2018-09-28 | 杭州师范大学 | A kind of preparation method of middle high phenyl content methyl phenyl silicone oil |
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| CN109485852B (en) * | 2018-10-13 | 2021-09-14 | 周群邦 | Preparation method and application of hydroxyl polysiloxane with ring-shaped structure |
| CN109485852A (en) * | 2018-10-13 | 2019-03-19 | 周群邦 | A kind of preparation method and applications of the ring-like structural hydroxyl polysiloxanes of band |
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| CN111234228B (en) * | 2020-02-26 | 2021-02-19 | 华南理工大学 | Hydrogen-containing methyl phenyl silicone resin for LED packaging adhesive and preparation method and application thereof |
| CN111378135A (en) * | 2020-04-30 | 2020-07-07 | 新纳奇材料科技江苏有限公司 | Preparation method of low-viscosity alkoxy-terminated polydimethylsiloxane |
| CN113307974A (en) * | 2021-06-21 | 2021-08-27 | 江西蓝星星火有机硅有限公司 | Method for rapidly recovering hydrogen-containing silicone oil in acid |
| CN113881239A (en) * | 2021-11-16 | 2022-01-04 | 深圳市华源宏新材料有限公司 | Methyl hydrogen-containing silicone rubber and preparation method thereof |
| CN114874442A (en) * | 2022-06-24 | 2022-08-09 | 惠州普赛达新材料有限公司 | Si-H polymer, heat-conducting silica gel composition, and preparation method and application thereof |
| CN115010929A (en) * | 2022-06-24 | 2022-09-06 | 江西蓝星星火有机硅有限公司 | Preparation method of hydroxyl-terminated vinyl silane prepolymer |
| CN115340822A (en) * | 2022-09-24 | 2022-11-15 | 中京新材料科技(河北)有限公司 | Ultra-smooth self-cleaning coating and preparation method thereof |
| CN115340822B (en) * | 2022-09-24 | 2023-11-07 | 中京新材料科技(河北)有限公司 | Super-smooth self-cleaning coating and preparation method thereof |
| CN117467142A (en) * | 2023-11-23 | 2024-01-30 | 广东鼎立森新材料有限公司 | Preparation method of methyl phenyl silicone resin block copolymer |
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Application publication date: 20170308 |