CN105315468B - A kind of epoxy polysiloxane and epoxidation preparation method - Google Patents
A kind of epoxy polysiloxane and epoxidation preparation method Download PDFInfo
- Publication number
- CN105315468B CN105315468B CN201510836626.0A CN201510836626A CN105315468B CN 105315468 B CN105315468 B CN 105315468B CN 201510836626 A CN201510836626 A CN 201510836626A CN 105315468 B CN105315468 B CN 105315468B
- Authority
- CN
- China
- Prior art keywords
- preparation
- temperature
- vinyl
- compound
- polysiloxanes
- 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.)
- Active
Links
- 0 CN(**(*)N)N*N Chemical compound CN(**(*)N)N*N 0.000 description 1
Landscapes
- Silicon Polymers (AREA)
Abstract
The invention discloses a kind of epoxy polysiloxane and its epoxidation preparation method.The present invention by using octamethylcy-clotetrasiloxane first, and base is made in anion open loop in the basic conditions for t etram-ethyltetravinylcyclotetrasiloxane and vinyl double seal head, then in the presence of ethyl acetate, with tetracarboxylic metal phthalocyanine complex compound and H2O2The mixture being mixed to get obtains epoxy polysiloxane compound as catalyst.Preparation method of the present invention is simple, avoids interface compatibility problem caused by blending and modifying, and modification by copolymerization side reaction is more, and difficult compound the shortcomings of removing, being prepared of catalyst can be used in LED illumination lamp technical field.
Description
Technical field
The present invention relates to macromolecule synthesising technology field, and in particular to a kind of epoxy polysiloxane and epoxidation preparation side
Method.
Background technology
Light emitting diode (LED) has been widely used in picture and text showing, traffic signals, detector system, electronic equipment, the back of the body
The fields such as light source.In recent years, as power-type LED is popularized, it is based especially on the development of ultraviolet white light LEDs, it is desirable to package material
Expect there is ultraviolet light that it can be kept while higher absorption in visible region high transparency；In addition, the continuous hair of LED technology
Exhibition, diversified needs are generated to brightness, purposes, packaged type etc., mutually modified using epoxy resin and polysiloxanes, by
Contain organosilicon composition and epoxy component simultaneously in structure, the good mechanical performance of epoxy resin, bonding can be given full play to
Performance and excellent electrical insulation capability and organic siliconresin high-low temperature resistant, protection against the tide, excellent weatherability and electrical insulation capability it is excellent
Gesture.
Traditional modifying epoxy resin by organosilicon typically uses blending and modifying or modification by copolymerization.Blending and modifying is that will first have
Machine silicon and epoxy resin are mixed, then the solidification such as curing agent, curing accelerator and other additives is added into mixed system
Shaping.But the two solubility parameters difference is larger, is easily separated.And the performance of blend and the morphosis of blend have
Close, morphosis is determined by co-mixing system each component compatibility, therefore the consistency problem for solving the two is crucial.Modification by copolymerization
It is to utilize the hydroxyl of the active group and epoxy resin on organosilicon to improve the compatibility of organosilicon material and epoxy resin
Base and epoxy reaction, because introduced in the structure of cured product more stable and there is flexible Si-O-Si segments, but
Reaction is whard to control and difficult remove of catalyst influences product property.
The content of the invention
For overcome the deficiencies in the prior art, the present invention provides a kind of epoxy polysiloxane and epoxidation preparation method.
In the inventive method, by carrying out epoxidation to the carbon-carbon double bond on polysiloxanes, so as to obtain modifying epoxy resin by organosilicon,
The method reaction is gentle, and used catalyst is metal complex solid powder and H2O2, easily separated and removal.Blending is avoided to change
Property caused by interface compatibility problem, and modification by copolymerization side reaction is more, catalyst difficult the shortcomings of removing.
Technical scheme is specifically described as follows.
The present invention provides a kind of epoxy polysiloxane compound, and the light transmittance of the compound is between 90~95%, room temperature
Viscosity at 25 DEG C is between 4000~7000mPas；Its structural formula is as follows：
Wherein, x represents the degree of polymerization, span 20-30.
The present invention also provides a kind of epoxidation preparation method of above-mentioned epoxy polysiloxane compound, comprises the following steps that：
(1) preparation of more vinyl polysiloxanes
By octamethylcy-clotetrasiloxane, t etram-ethyltetravinylcyclotetrasiloxane and vinyl double seal head, (chemical name is
The tetramethyl disiloxane of 1,3 one divinyl one 1,1,3,3 one) according to 30:(5-15):The mass ratio of (0.2-0.8), depressurizing
Under conditions of, 0.5h~1h is removed water at a temperature of 40 DEG C~80 DEG C；Catalyst tetramethylammonium hydroxide aqueous solution is added afterwards,
4h~8h is reacted at a temperature of 90 DEG C~110 DEG C, reaction terminates rear decomposition catalyst and removes low-boiling-point substance, obtains the poly- silicon of more vinyl
Oxygen alkane；Wherein, the addition of TMAH accounts for the 0.03%~0.05% of mix monomer gross mass；More vinyl
The structural formula of polysiloxanes is as follows：
(2) preparation of epoxy polysiloxane compound
More vinyl polysiloxanes that step (1) is prepared are added drop-wise in the solution containing epoxidation reagent, 30
DEG C~70 DEG C at a temperature of, react 3h~6h, afterwards purifies and separates obtain epoxy polysiloxane；Wherein：Epoxidation reagent is tetracarboxylic acid
Sour metal phthalocyanine complex and 30wt%H2O2Mixture；Tetracarboxylic metal phthalocyanine complex compound and 30wt%H2O2Mass ratio
For 1：3-1：10；The mass ratio of more vinyl polysiloxanes and tetracarboxylic metal phthalocyanine complex compound is 10：2-10：6, the epoxy
The structural formula of polysiloxanes is as follows：
In above-mentioned steps (1), octamethylcy-clotetrasiloxane and t etram-ethyltetravinylcyclotetrasiloxane, vinyl double seal head
Mass ratio be 30：(8-12)：(0.3-0.6).
In above-mentioned steps (1), removed water at a temperature of 50 DEG C~70 DEG C.
In above-mentioned steps (2), temperature is 40 DEG C~60 DEG C, more vinyl polysiloxanes and tetracarboxylic metal phthalocyanine complex compound
Mass ratio be 10：4.
In above-mentioned steps (2), in the solution containing epoxidation reagent, solvent is ethyl acetate or dimethyl sulfoxide.
In above-mentioned steps (2), in the solution containing epoxidation reagent, the mass volume ratio of epoxidation reagent and solvent
For 1：4-1：10mg/mL.
In above-mentioned steps (2), the purifying of epoxy polysiloxane is that the mode being then evaporated under reduced pressure is realized by first filtering
's.The condition of vacuum distillation is 40 DEG C~70 DEG C under -0.095MPa.
The NDJ-1 that the viscosity of the epoxy polysiloxane of gained of the invention is provided using the sharp bearing device Manufacturing Co., Ltd in Shanghai
Rotation viscometer, by GB/T2794-2013,《The measure list cylinder rotary viscosimeter method of adhesive viscosity》, in 25 DEG C of room temperature
Under conditions of detected, its viscosity is 4000~7000mPas.Using the UV- of UNICO(Shanghai) Instruments Co., Ltd.
2102PC ultra-violet and visible spectrophotometers, epoxy polysiloxane sample prepared by the present invention is placed in 1mm × 1mm × 10mm's
In quartz colorimetric utensil；Scanning wave band is 200-900nm, and test sample light transmittance, its light transmittance is up to 90~95%.
The beneficial effects of the present invention are：
1st, because the hydrogen atom In frared spectra on long-chain polysiloxanes end group and the carbon-carbon double bond of side base is weak, only ortho position
Silicon atom on contain methyl electron donating group, therefore the cloud density in double bond is relatively low, traditional Peracetic acid, between peroxide
The electrophilic oxidising agent such as chlorobenzoic acid, peroxy trifluoroacetic acid is difficult to its epoxidation, and the epoxidation reagent used in the present invention is gold
Belong to complex compound and 30%H2O2Composition nucleophilic oxidant, the carbon-carbon double bond weaker to supplied for electronic have well selectivity.
2nd, the end group on polysiloxanes and side base double bond epoxidation are directly prepared epoxy silicone resin by the present invention, are kept away
Interface compatibility problem caused by blending and modifying is exempted from, performance is unstable；And modification by copolymerization reaction is difficult to control and catalyst
The shortcomings of hardly possible removes, the method reaction is gentle, and used catalyst is solid powder and hydrogen peroxide, and easily separated and removal, is epoxy
The preparation of organic siliconresin provides a new path.
3rd, the preparing raw material octamethylcy-clotetrasiloxane of more vinyl polysiloxanes can change octaphenylcyclotetrasiloxane into,
The reagent containing phenyl such as aminomethyl phenyl cyclotetrasiloxane, because phenyl has higher refractive index and rigidity, sealed using it as LED
Package material can increase light extraction efficiency, make it have preferable resistance to elevated temperatures and UV resistance, and improve chip to external
The resistance of impact, slows down mechanical oscillation, ensures its normal work.
Brief description of the drawings
Fig. 1 is that the liquid epoxy polysiloxanes of the embodiment of the present invention 1 detects figure through infrared spectrum.
Embodiment
In raw material used in various embodiments of the present invention in addition to the special producer shown and model, other raw materials be it is commercially available,
Specification is that chemistry is pure.
The model of various equipment used in the present invention and the information of manufacturer are as follows：
NDJ-1 rotation viscometers, the sharp bearing device Manufacturing Co., Ltd in Shanghai；
UV-2102PC ultra-violet and visible spectrophotometers, UNICO(Shanghai) Instruments Co., Ltd..
Embodiment 1
Thermometer is loaded onto on reaction vessel, connects and vacuumizes de-watering apparatus, in order in terms of parts by weight, adds eight first
30 parts of basic ring tetrasiloxane, 8 parts of t etram-ethyltetravinylcyclotetrasiloxane, 0.4 part of vinyl double seal head, vacuum-
Below 0.090MPa, heating and magnetic stirring apparatus are opened, be warming up to 50 DEG C of the initial temperature of setting, remove water 0.5h；Afterwards plus
Entering catalyst tetramethylammonium hydroxide aqueous solution, the addition of TMAH accounts for the 0.03% of mix monomer gross mass,
Reflux condensing tube is changed, material in bottle is warming up to 100 DEG C of design temperature, polymerisation 5h (is indicated at a set temperature：Now
Vaccum dewatering device is not needed).Temperature is raised to more than 140 DEG C decomposition catalysts by reaction rapidly after terminating, and is examined when with pH test paper
When surveying pH=7 of tail gas or so, you can continue to heat up；Vacuum is warming up to more than 200 DEG C below -0.090MPa, takes off low boiling
Thing, time 10-20min, it can stop heating when observing that flowing out without cut goes out, be cooled to room temperature and can obtain water white transparency
Ethenyl blocking polysiloxanes.Yield 87.9%.
Mechanical agitation, thermometer, dropping funel are loaded onto on reaction vessel, in terms of parts by weight, adds vinyl more than 10 parts
Polysiloxanes, 50 parts of ethyl acetate, 2 parts of tetracarboxylic metal phthalocyanine complex compounds, mechanical agitation are warming up to 40 DEG C；30% dioxygen is added dropwise
10 parts of water, is added dropwise, dropping funel is removed, and changes reflux condensing tube, and react 5h at this temperature；Mistake after reaction terminates
Faint yellow solid is filtered out, gained clear liquid is washed with 10% sodium hydrogensulfite, to the not aobvious blueness of starch potassium iodide paper, then with
50 parts of deionized water is washed 2 times, with anhydrous sodium sulfate drying；Drier is filtered to remove, is concentrated to give colourless liquid epoxy organosilicon
Resin, yield 52%, light transmittance 93%, viscosity 4000mPas.
The epoxy silicone resin of above-mentioned gained is red by infrared chromatograph (type of Nicolet companies of the U.S. 380) progress
External spectrum is analyzed, and the infrared spectrogram of gained is as shown in figure 1, from figure 1 it appears that IR (KBr):829 (epoxide groups), card
Actually contain epoxy radicals.
Embodiment 2
Thermometer is loaded onto on reaction vessel, connects and vacuumizes de-watering apparatus, in order in terms of parts by weight, adds eight first
30 parts of basic ring tetrasiloxane, 12 parts of t etram-ethyltetravinylcyclotetrasiloxane, 0.6 part of vinyl double seal head, vacuum-
Below 0.090MPa, heating and magnetic stirring apparatus are opened, be warming up to 70 DEG C of the initial temperature of setting, remove water 1h；Add afterwards
Catalyst tetramethylammonium hydroxide aqueous solution, the addition of TMAH account for the 0.05% of mix monomer gross mass, changed
Upper reflux condensing tube, material in bottle is warming up to 100 DEG C of design temperature, polymerisation 5h (is indicated at a set temperature：Now not
Need vaccum dewatering device).Temperature is raised to more than 140 DEG C decomposition catalysts by reaction rapidly after terminating, and is detected when with pH test paper
During pH=7 of tail gas or so, you can continue to heat up；Vacuum is warming up to more than 200 DEG C below -0.090MPa, takes off low boiling
Thing, time 10-20min, it can stop heating when observing that flowing out without cut goes out, be cooled to room temperature and can obtain water white transparency
Ethenyl blocking polysiloxanes.Yield 85.2%.
Mechanical agitation, thermometer, dropping funel are loaded onto on reaction vessel, in terms of parts by weight, adds vinyl more than 10 parts
Polysiloxanes, 50 parts of ethyl acetate, 6 parts of tetracarboxylic metal phthalocyanine complex compounds, mechanical agitation are warming up to 60 DEG C；30% dioxygen is added dropwise
20 parts of water, is added dropwise, dropping funel is removed, and changes reflux condensing tube, and react 5h at this temperature；Mistake after reaction terminates
Faint yellow solid is filtered out, gained clear liquid is washed with 10% sodium hydrogensulfite, to the not aobvious blueness of starch potassium iodide paper, then with
50 parts of deionized water is washed 2 times, with anhydrous sodium sulfate drying；Drier is filtered to remove, is concentrated to give colourless liquid epoxy organosilicon
Resin, yield 64%, light transmittance 93%, viscosity 7000mPas.
Embodiment 3
Thermometer is loaded onto on reaction vessel, connects and vacuumizes de-watering apparatus, is sequentially added into octamethylcy-clotetrasiloxane
30 parts, 10 parts of t etram-ethyltetravinylcyclotetrasiloxane, 0.5 part of vinyl double seal head, vacuum is opened below -0.090MPa
Heating and magnetic stirring apparatus are opened, is warming up to 60 DEG C of the initial temperature of setting, removes water 0.5h；Catalyst tetramethyl hydrogen is added afterwards
Aqueous ammonium is aoxidized, the addition of TMAH accounts for the 0.04% of mix monomer gross mass, changes reflux condensing tube, will
Material is warming up to 110 DEG C of design temperature in bottle, and polymerisation 6h (is indicated at a set temperature：Vaccum dewatering dress is not needed now
Put).Temperature is raised to more than 140 DEG C decomposition catalysts by reaction rapidly after terminating, as pH=7 that tail gas is detected with pH test paper or so
When, you can continue to heat up；Vacuum is warming up to more than 200 DEG C below -0.090MPa, takes off low-boiling-point substance, time 10-
It 20min, can stop heating when observing that flowing out without cut goes out, be cooled to the ethenyl blocking that room temperature can obtain water white transparency
Polysiloxanes.Yield 86.4%.
Load onto mechanical agitation, thermometer, dropping funel on reaction vessel, add vinyl polysiloxane more than 10 parts, 60 parts
Ethyl acetate, 4 parts of tetracarboxylic metal phthalocyanine complex compounds, mechanical agitation are warming up to 50 DEG C；40 parts of 30% hydrogen peroxide is added dropwise, drips
Finish, dropping funel is removed, changes reflux condensing tube, and react 6h at this temperature；Reaction is filtered to remove faint yellow after terminating
Solid, gained clear liquid are washed with 10% sodium hydrogensulfite, to the not aobvious blueness of starch potassium iodide paper, then with 50 parts of deionized water
Washing 2 times, with anhydrous sodium sulfate drying；Drier is filtered to remove, is concentrated to give colourless liquid epoxy silicone resin, yield
56%, light transmittance 92%, viscosity 5200mPas.
Claims (9)
1. a kind of epoxy polysiloxane compound, it is characterised in that the light transmittance of the compound is between 90~95%, room temperature 25
Viscosity at DEG C is between 4000~7000mPas；Its structural formula is as follows：
Wherein, x represents the degree of polymerization, span 20-30.
2. a kind of epoxidation preparation method of epoxy polysiloxane compound as claimed in claim 1, it is characterised in that specific
Step is as follows：
(1) preparation of more vinyl polysiloxanes
First by octamethylcy-clotetrasiloxane, t etram-ethyltetravinylcyclotetrasiloxane and vinyl double seal head according to 30:(5-
15):The mass ratio of (0.2-0.8) at reduced pressure, removes water 0.5h~1h at a temperature of 40 DEG C~80 DEG C；Add and urge afterwards
Agent tetramethylammonium hydroxide aqueous solution, reacts 4h~8h at a temperature of 90 DEG C~110 DEG C, and reaction terminates rear decomposition catalyst simultaneously
Low-boiling-point substance is removed, obtains more vinyl polysiloxanes；Wherein, the addition of TMAH accounts for mix monomer gross mass
0.03%~0.05%；The structural formula of more vinyl polysiloxanes is as follows：
Wherein, x represents the degree of polymerization, span 20-30；
(2) preparation of epoxy polysiloxane compound
More vinyl polysiloxanes that step (1) is prepared are added drop-wise in the solution containing epoxidation reagent, 30 DEG C~
At a temperature of 70 DEG C, 3h~6h is reacted, purifies and separates obtain epoxy polysiloxane afterwards；Wherein：Epoxidation reagent is tetrabasic carboxylic acid gold
Belong to phthalocyanine complex and 30wt%H2O2Mixture；Tetracarboxylic metal phthalocyanine complex compound and 30wt%H2O2Mass ratio be 1：
3-1：10；The mass ratio of more vinyl polysiloxanes and tetracarboxylic metal phthalocyanine complex compound is 10：2-10：6, the poly- silicon of epoxy
The structural formula of oxygen alkane is as follows：
Wherein, x represents the degree of polymerization, span 20-30.
3. preparation method according to claim 2, it is characterised in that in step (1), octamethylcy-clotetrasiloxane and tetramethyl
Base tetravinyl cyclotetrasiloxane, the mass ratio of vinyl double seal head are 30：(8-12)：(0.3-0.6).
4. preparation method according to claim 2, it is characterised in that in step (1), removed at a temperature of 50 DEG C~70 DEG C
Water.
5. preparation method according to claim 2, it is characterised in that in step (2), temperature is 40 DEG C~60 DEG C, more second
The mass ratio of alkenyl polysiloxanes and tetracarboxylic metal phthalocyanine complex compound is 10：4.
6. preparation method according to claim 2, it is characterised in that described to contain the molten of epoxidation reagent in step (2)
In liquid, solvent is ethyl acetate or dimethyl sulfoxide.
7. preparation method according to claim 2, it is characterised in that described to contain the molten of epoxidation reagent in step (2)
In liquid, the mass volume ratio of epoxidation reagent and solvent is 1：4-1：10mg/mL.
8. preparation method according to claim 2, it is characterised in that in step (2), the purifying of epoxy polysiloxane is logical
Filtered after first, what the mode being then evaporated under reduced pressure was realized.
9. preparation method according to claim 8, it is characterised in that in step (2), the condition of vacuum distillation is：Pressure
For -0.095MPa, temperature is 40 DEG C~70 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510836626.0A CN105315468B (en) | 2015-11-26 | 2015-11-26 | A kind of epoxy polysiloxane and epoxidation preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510836626.0A CN105315468B (en) | 2015-11-26 | 2015-11-26 | A kind of epoxy polysiloxane and epoxidation preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105315468A CN105315468A (en) | 2016-02-10 |
| CN105315468B true CN105315468B (en) | 2017-12-05 |
Family
ID=55243846
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510836626.0A Active CN105315468B (en) | 2015-11-26 | 2015-11-26 | A kind of epoxy polysiloxane and epoxidation preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105315468B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109400880B (en) * | 2017-08-18 | 2020-09-04 | 北京化工大学 | Methyl vinyl phenyl silicone rubber with high phenyl content and high vinyl content and preparation method thereof |
| CN111410745A (en) * | 2019-01-07 | 2020-07-14 | 北京化工大学 | Ultra-low temperature-resistant epoxidized silicone rubber and preparation method thereof |
| CN113004524B (en) * | 2019-12-20 | 2023-01-13 | 万华化学集团股份有限公司 | Epoxy-organic silicon resin and preparation method and application thereof |
| CN113004523B (en) * | 2019-12-20 | 2022-08-05 | 万华化学集团股份有限公司 | Epoxy-organic silicon resin and preparation method and application thereof |
| CN111040168A (en) * | 2019-12-26 | 2020-04-21 | 广东盈骅新材料科技有限公司 | Epoxy modified organic silicon resin and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103319692A (en) * | 2012-03-22 | 2013-09-25 | 中科院广州化学有限公司 | High performance organosilicon epoxy material, preparation method and applications thereof |
| CN103805128A (en) * | 2012-11-15 | 2014-05-21 | 烟台德邦先进硅材料有限公司 | Adhesive for high-refractive index LED (Light Emitting Diode) package glue and adhesive synthesizing method |
| CN104672459A (en) * | 2015-02-05 | 2015-06-03 | 上海应用技术学院 | Vinyl phenyl silicon resin with side chain containing epoxy group and preparation method of vinyl phenyl silicon resin |
-
2015
- 2015-11-26 CN CN201510836626.0A patent/CN105315468B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103319692A (en) * | 2012-03-22 | 2013-09-25 | 中科院广州化学有限公司 | High performance organosilicon epoxy material, preparation method and applications thereof |
| CN103805128A (en) * | 2012-11-15 | 2014-05-21 | 烟台德邦先进硅材料有限公司 | Adhesive for high-refractive index LED (Light Emitting Diode) package glue and adhesive synthesizing method |
| CN104672459A (en) * | 2015-02-05 | 2015-06-03 | 上海应用技术学院 | Vinyl phenyl silicon resin with side chain containing epoxy group and preparation method of vinyl phenyl silicon resin |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105315468A (en) | 2016-02-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105315468B (en) | A kind of epoxy polysiloxane and epoxidation preparation method | |
| CN103627178B (en) | A kind of LED encapsulation liquid silicon rubber composition and preparation method thereof | |
| CN104672459B (en) | The Vinylphenyl silicon resin of a kind of side chain containing epoxide group and preparation method thereof | |
| CN103865389B (en) | A kind of using method of add-on type solvent-free organic silicon interleaving agent | |
| CN103012797A (en) | Preparation method of methyl phenyl vinyl silicone oil | |
| CN102898650B (en) | MTQ silicon resin with T-chain unit containing phenyl and preparation method thereof | |
| CN101891893A (en) | Preparation method of phenyl-based hydrogen-based silicone resin for encapsulating LED | |
| CN103805128A (en) | Adhesive for high-refractive index LED (Light Emitting Diode) package glue and adhesive synthesizing method | |
| CN104098905B (en) | A kind of LED lens strong elasticity phenyl organic siliconresin and preparation method thereof | |
| CN106700036B (en) | A kind of macromolecule and preparation method thereof with aggregation-induced emission effect | |
| CN104788488B (en) | A kind of preparation method of naphthyl alkoxy silane | |
| CN103409103A (en) | Environment-friendly high-temperature-resistant organic silicon pressure-sensitive adhesive and preparation method thereof | |
| CN106397771A (en) | Preparation method of tackifier used for organosilicone LED packaging colloidal system | |
| CN105131296B (en) | A kind of self-cross linking type LED encapsulation gum resin and preparation method thereof | |
| CN108164704A (en) | The preparation method of high refractive index additional organosilicon packaging plastic adhesive accelerant | |
| JP2009102297A (en) | (thio)phenoxyphenyl silane composition and method for producing the same | |
| CN113583216A (en) | Bio-based epoxy resin containing silicon-oxygen bond and preparation and application methods thereof | |
| CN108300408A (en) | A kind of high lux maintenance LED organosilicon material for packaging | |
| CN101619170A (en) | Preparation and application of silica gel for LED packaging | |
| CN104140535A (en) | Phenyl-containing MQ silicon resin and preparation method thereof | |
| CN105778100B (en) | A kind of organic silicon rigidity-increasing stick and preparation method thereof and a kind of addition-type silicon rubber composition | |
| CN107814935A (en) | A kind of arm epoxy resin of POSS bases organic inorganic hybridization eight and preparation method thereof | |
| CN104945628B (en) | A kind of polyglycerol-modified organosilicon and preparation method thereof | |
| CN109705352A (en) | A kind of vinyl polysiloxane and its preparation method and application | |
| CN102219905B (en) | Organic silicon episulfide resin and preparation method thereof |
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 | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 200235 Caobao Road, Xuhui District, Shanghai, No. 120-121 Patentee after: SHANGHAI INSTITUTE OF TECHNOLOGY Address before: 200235 Caobao Road, Xuhui District, Shanghai, No. 120-121 Patentee before: Shanghai Institute of Technology |
|
| CP01 | Change in the name or title of a patent holder | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20180706 Address after: No. 3288, Shanghai City, Jia Zhu highway Patentee after: SHANGHAI RESIN FACTORY Co.,Ltd. Address before: 200235 Caobao Road, Xuhui District, Shanghai, No. 120-121 Patentee before: Shanghai Institute of Technology |
|
| TR01 | Transfer of patent right |