CN108003347A - A kind of preparation method for high-power encapsulation MDT silicones - Google Patents
A kind of preparation method for high-power encapsulation MDT silicones Download PDFInfo
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- CN108003347A CN108003347A CN201711179671.9A CN201711179671A CN108003347A CN 108003347 A CN108003347 A CN 108003347A CN 201711179671 A CN201711179671 A CN 201711179671A CN 108003347 A CN108003347 A CN 108003347A
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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
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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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
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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
- C08G77/70—Siloxanes defined by use of the MDTQ nomenclature
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
Abstract
The present invention relates to a kind of preparation method for high-power encapsulation MDT silicones, including：Acid is added in four-hole bottle, dimethyldialkylammonium oxysilane, methyl phenyl di-alkoxy silane, phenyl trialkoxysilane, alcohol and water, stirring, be heated to 25 DEG C reaction 12 it is small when, remaining total water and vinyl double seal head is added dropwise at the same time at room temperature after the completion of reaction, hexamethyldisiloxane, temperature in control system is between 30 40 DEG C, when reaction 12 is small at 70 DEG C after being added dropwise, then the alcohol in system is steamed, then the pH=9 10 of the toluene and alkali regulation system more than theoretical amount of resin is added, when 90 DEG C of reactions 1 are small, then heating steams remaining alcohol and water in system, finally cool down again, neutralized with acid, it is washed to the pH=6 7 of system, toluene is evaporated off up to silicones in 120 DEG C of backspins；The MDT silicones of preparation is mainly used for the reinforcing agent of packaging plastic, organosilicon adhesive and silicone molding compound.
Description
Technical field
The present invention relates to a kind of preparation method for high-power encapsulation MDT silicones, belong to the synthesis skill of silicones
Art field.
Technical background
In recent years, with the development of semiconductor light emitting technology, semiconductor lighting substitute high energy consumption, low light efficiency incandescent lamp
As inexorable trend, cause global extensive concern.Organosilicon material is due to its good resistant of high or low temperature and recyclability, especially
It is the silicon rubber or silicones vulcanized by hydrosilylation mode, is that high power LED device is most preferable so far
Encapsulating material, the silicones of MDT types is one kind in organic siliconresin, it by single functionality silica chain link (R3SiO1/2,
M chain links), the organosilicon of two degree of functionality silica chain links (R2SiO, D chain link) and three-functionality-degree silica chain link (RSiO3/2, T chain link)
Monomer is formed through cohydrolysis-polycondensation reaction.
In existing technology, in relation to existing for the general refractive index control of MDT silicones used in LED packaging silicon rubbers
Between 1.50-1.55, belong to high refractive index silicone；But as LED is encapsulated towards high-power, large-sized development, simple
High refractive index resins have been unable to meet the requirement of higher.A kind of MDT resins of the present invention preferably meet LED packaging silicon rubbers to resistant to sulfur
Change, the requirement of thermal shock performance and high-power, large scale for light decay under higher high temperature.
The content of the invention
For the deficiency of existing MDT silicones, the present invention provides a kind of by methyl M links, vinyl M links, methylbenzene
The synthetic method for the MDT resins that base D links, methyl ethylene D links, phenyl T links form.
Technical scheme is as follows：
A kind of preparation method for high-power encapsulation MDT silicones, it is characterised in that in four-hole bottle add acid,
Dimethyldialkylammonium oxysilane, methyl phenyl di-alkoxy silane, phenyl trialkoxysilane, alcohol and suitable water, stirring, add
When hot to 25 DEG C reaction 1-2 are small, remaining total water and vinyl double seal head, pregnancy is added dropwise at the same time at room temperature after the completion of reaction
Base disiloxane, the temperature in control system reacted between 30-40 DEG C, after being added dropwise at 70 DEG C 1-2 it is small when, then steam
Alcohol in system, then adds the pH=9-10 of the toluene and alkali regulation system more than theoretical amount of resin, when 90 DEG C of reactions 1 are small,
Then heating steams remaining alcohol and water in system, finally cools down again, is neutralized with acid, is washed to the pH=6-7 of system；120℃
Toluene is evaporated off up to silicones in backspin；
The acid, vinyl double seal head, hexamethyldisiloxane, dimethyldimethoxysil,ne, alcohol, water, aminomethyl phenyl
Dialkoxy silicane, the mass ratio of phenyl trialkoxysilane are (1.18-1.99)：(5.58-38.50)：(30.46-
113.24)：(60.11-240.44)：(11.80-19.95)：(50.20-120.80)：(182.29-210.35)：(198.26-
240.37)。
Preferable according to the present invention, the dimethyldialkylammonium oxysilane is dimethyldimethoxysil,ne, dimethyl two
Ethoxysilane；
It is preferable according to the present invention, play the compatibility of increase system using alcohol is added and suppress to react too fast；
Preferable according to the present invention, the phenyl methyl dialkoxy silicane is aminomethyl phenyl dimethoxysilane, methyl
Diethylamino phenyl oxysilane；
Preferable according to the present invention, the phenyl trialkoxysilane is phenyltrimethoxysila,e, phenyl triethoxy
Silane；
Preferable according to the present invention, the acid is hydrochloric acid, sulfuric acid, phosphoric acid, Emathlite, trifluoromethane sulfonic acid and acidity sun
Ion exchange resin；
Preferable according to the present invention, the dosage of water is phenyl trialkoxysilane, methyl phenyl di-alkoxy silane and two
1.4-2.7 times of methyl dioxane oxysilane total moles quality；
Preferable according to the present invention, the alcohol is ethanol, methanol；The alkali is Na2CO3、NaHCO3、K2CO3、KHCO3、
NaOH、KOH；
Preferable according to the present invention, speed of agitator is 200-450 revs/min；
Preferable according to the present invention, vinyl mass percent is 1.5%-6%；
Preferable according to the present invention, the value of R/Si is 1.1-1.8；
Preferable according to the present invention, the MDT silicones of synthesis accurately can control alkoxy by deviating from the amount of alcohol
Surplus；
Preferable according to the present invention, the reactor is equipped with thermometer, constant pressure funnel, spherical condensation tube, tetrafluoro
The four round flask of stirring rod.
MDT silicones prepared by invention is mainly used for the reinforcing agent of packaging plastic, organosilicon adhesive and silicone molding compound.
Embodiment
Embodiment 1
1.77g concentrated hydrochloric acids, 30.46g dimethyldimethoxysil,nes, 182.29g aminomethyl phenyls two are added in four-hole bottle
Methoxy silane, 198.26g phenyltrimethoxysila,es, 15.10g ethanol and 5g water, stir, be heated to 25 DEG C reaction 2 it is small when, instead
57.40g water and 15.13g vinyl double seal heads, 67.70g hexamethyldisiloxane is added dropwise at the same time at room temperature after the completion of answering, controls
Temperature in system processed when reaction 2 is small at 70 DEG C after being added dropwise, then steams the alcohol in system, then between 30-40 DEG C
300g toluene and the pH=10 of suitable Na2CO3 regulation systems are added, when 90 DEG C of reactions 1 are small, 120 DEG C then heated to and steams
Remaining alcohol and water in system, finally cools down, the pH=6-7 of system is neutralized, be washed to acetic acid again；120 DEG C of backspins are evaporated off
Toluene is up to silicones；Its yield is 95%.
Embodiment 2
1.77g concentrated hydrochloric acids, 30.46g dimethyl diethoxysilanes, 210.35g aminomethyl phenyls two are added in four-hole bottle
Ethoxy silane, 240.37g phenyl triethoxysilanes, 15.10g ethanol and 5g water, stir, be heated to 25 DEG C reaction 2 it is small when, instead
57.40g water and 15.13g vinyl double seal heads, 67.70g hexamethyldisiloxane is added dropwise at the same time at room temperature after the completion of answering, controls
Temperature in system processed when reaction 2 is small at 70 DEG C after being added dropwise, then steams the alcohol in system, then between 30-40 DEG C
300g toluene and the pH=10 of suitable NaHCO3 regulation systems are added, when 90 DEG C of reactions 1 are small, 120 DEG C then heated to and steams
Remaining alcohol and water in system, finally cools down, the pH=6-7 of system is neutralized, be washed to acetic acid again；120 DEG C of backspins are evaporated off
For toluene up to silicones, its yield is 94%.
Embodiment 3
The 1.60g concentrated sulfuric acids, 30.46g dimethyldimethoxysil,nes, 182.29g aminomethyl phenyls two are added in four-hole bottle
Methoxy silane, 198.26g phenyltrimethoxysila,es, 15.10g alcohol and 5g water, stir, be heated to 25 DEG C reaction 2 it is small when, reaction
After the completion of at room temperature at the same time 57.40g water and 15.13g vinyl double seal heads, 67.70g hexamethyldisiloxane is added dropwise, control
Temperature in system when reaction 2 is small at 70 DEG C after being added dropwise, then steams the alcohol in system, Ran Houjia between 30-40 DEG C
Enter 300g toluene and the pH=10 of suitable NaOH regulation systems, when 90 DEG C of reactions 1 are small, then heat to 120 DEG C and steam system
Interior remaining alcohol and water, finally cools down, the pH=6-7 of system is neutralized, be washed to acetic acid again；Toluene is evaporated off in 120 DEG C of backspins
Up to silicones；Its yield is 90%.
Embodiment 4
1.50g trifluoromethane sulfonic acids, 30.46g dimethyldimethoxysil,nes, 182.29g methyl are added in four-hole bottle
Phenyl dimethoxy silane, 198.26g phenyltrimethoxysila,es, 15.10g methanol and 5g water, stir, are heated to 25 DEG C of reactions 2
Hour, 57.40g water and 15.13g vinyl double seal heads, two silicon of 67.70g hexamethyls is added dropwise at the same time at room temperature after the completion of reaction
Oxygen alkane, the temperature in control system when reaction 2 is small at 70 DEG C after being added dropwise, are then steamed in system between 30-40 DEG C
Alcohol, then adds 300g toluene and the pH=10 of suitable KOH regulation systems, when 90 DEG C of reactions 1 are small, then heats to 120 DEG C
Remaining alcohol and water in system is steamed, finally cools down again, the pH=6-7 of system is neutralized, be washed to acetic acid；Rotated at 120 DEG C
Toluene is removed up to silicones；Its yield is 93%.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention scope, every in the present invention
Spirit and principle within, any modification, equivalent substitution, improvement and etc. done, should be included in protection scope of the present invention
Within.
Claims (2)
1. a kind of preparation method for high-power encapsulation MDT silicones, it is characterised in that acid, two are added in four-hole bottle
Methyl dioxane oxysilane, methyl phenyl di-alkoxy silane, phenyl trialkoxysilane, alcohol and water, stir, are heated to 25 DEG C
When reaction 1-2 is small, remaining total water and vinyl double seal head, two silica of hexamethyl is added dropwise at the same time at room temperature after the completion of reaction
Alkane, the temperature in control system reacted between 30-40 DEG C, after being added dropwise at 70 DEG C 1-2 it is small when, then steam in system
Alcohol, then adds the pH=9-10 of the toluene and alkali regulation system more than theoretical amount of resin, when 90 DEG C of reactions 1 are small, then heats up
Remaining alcohol and water in system is steamed, is finally cooled down again, is neutralized with acid, is washed to the pH=6-7 of system；120 DEG C of backspins are evaporated off
Toluene is removed up to silicones；
The acid, vinyl double seal head, hexamethyldisiloxane, dimethyldimethoxysil,ne, alcohol, water, aminomethyl phenyl dioxane
Oxysilane, the mass ratio of phenyl trialkoxysilane are (1.18-1.99)：(5.58-38.50)：(30.46-113.24)：
(60.11-240.44)：(11.80-19.95)：(50.20-120.80)：(182.29-210.35)：(198.26-240.37).
2. preparation method according to claim 1, it is characterised in that the dimethyldialkylammonium oxysilane is dimethyl two
Methoxy silane or dimethyl diethoxysilane；The phenyl methyl dialkoxy silicane is aminomethyl phenyl dimethoxysilane
Or aminomethyl phenyl diethoxy silane；The acid be hydrochloric acid, sulfuric acid, phosphoric acid, Emathlite, trifluoromethane sulfonic acid and acid sun from
One kind in sub-exchange resin；The alcohol is one kind in ethanol, methanol；The alkali is Na2CO3、NaHCO3、K2CO3、KHCO3、
One kind in NaOH, KOH.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711179671.9A CN108003347A (en) | 2017-11-23 | 2017-11-23 | A kind of preparation method for high-power encapsulation MDT silicones |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711179671.9A CN108003347A (en) | 2017-11-23 | 2017-11-23 | A kind of preparation method for high-power encapsulation MDT silicones |
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| CN108003347A true CN108003347A (en) | 2018-05-08 |
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| CN201711179671.9A Withdrawn CN108003347A (en) | 2017-11-23 | 2017-11-23 | A kind of preparation method for high-power encapsulation MDT silicones |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109438710A (en) * | 2018-11-06 | 2019-03-08 | 烟台德邦科技有限公司 | Preparation method of MDT resin for Molding silica gel |
| CN116178724A (en) * | 2022-11-07 | 2023-05-30 | 湖北兴瑞硅材料有限公司 | Synthesis method of methyl phenyl silicone oil |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56151731A (en) * | 1980-04-25 | 1981-11-24 | Japan Synthetic Rubber Co Ltd | Preparation of silicone resin |
| CN103232601A (en) * | 2013-04-28 | 2013-08-07 | 成都硅宝科技股份有限公司 | Phenyl MDT silicon resin and preparation method thereof |
| CN103450481A (en) * | 2013-09-17 | 2013-12-18 | 深圳市鑫东邦科技有限公司 | Preparation method of methyl phenyl vinyl silicone |
-
2017
- 2017-11-23 CN CN201711179671.9A patent/CN108003347A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56151731A (en) * | 1980-04-25 | 1981-11-24 | Japan Synthetic Rubber Co Ltd | Preparation of silicone resin |
| CN103232601A (en) * | 2013-04-28 | 2013-08-07 | 成都硅宝科技股份有限公司 | Phenyl MDT silicon resin and preparation method thereof |
| CN103450481A (en) * | 2013-09-17 | 2013-12-18 | 深圳市鑫东邦科技有限公司 | Preparation method of methyl phenyl vinyl silicone |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109438710A (en) * | 2018-11-06 | 2019-03-08 | 烟台德邦科技有限公司 | Preparation method of MDT resin for Molding silica gel |
| CN116178724A (en) * | 2022-11-07 | 2023-05-30 | 湖北兴瑞硅材料有限公司 | Synthesis method of methyl phenyl silicone oil |
| CN116178724B (en) * | 2022-11-07 | 2024-05-17 | 湖北兴瑞硅材料有限公司 | Synthesis method of methyl phenyl silicone oil |
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Effective date of registration: 20190225 Address after: 264006 No. 3-24 Kaifeng Road Renewable Resource Processing Demonstration Zone, Yantai Development Zone, Shandong Province Applicant after: Yantai Darbond Technology Co., Ltd. Address before: 264006 Kaifeng Road 3-3 Resource Regeneration and Processing Demonstration Zone, Yantai Development Zone, Shandong Province Applicant before: Yantai Debang Advanced Silicon Materials Co.,Ltd. |
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Application publication date: 20180508 |