CN106479394A - A kind of preparation method for organic silica gel system viscosifier - Google Patents
A kind of preparation method for organic silica gel system viscosifier Download PDFInfo
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- CN106479394A CN106479394A CN201611096586.1A CN201611096586A CN106479394A CN 106479394 A CN106479394 A CN 106479394A CN 201611096586 A CN201611096586 A CN 201611096586A CN 106479394 A CN106479394 A CN 106479394A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F230/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal
- C08F230/08—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon
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Abstract
The present invention relates to a kind of preparation method for organic silica gel system viscosifier, comprise the steps：Acrylate base monomer is added in reaction bulb with trimethoxy silicon hydrogen alkane, and adds toluene as solvent, heats up 60 80 DEG C, stirs 0.5h；Add chloroplatinic acid catalyst in reaction bulb, react 3 4h；Then Deca acrylate radical siloxane, and add base catalyst, stirring reaction 2 4h at 60 80 DEG C；Add acid to be neutralized to neutrality, stirring reaction 1h, stop heating, reaction finishes, cooling, and add dry white carbon black to be adsorbed, discharging；Add normal heptane, washing, dry, filtration, filtrate is put in revolving bottle, adopts rotavapor under vacuum to remove low molecule 2h at 100 120 DEG C, obtain final product water white viscosifier.It is used in dual composition addition type silicon resin system with the viscosifier of this method synthesis, the compatibility is very good, occur without that change is mixed to send out phenomenon turbid；No any abnormal flavour, the method raw material that the present invention prepares this viscosifier is easy to get, reaction condition is gentle, workable it is easy to industrialized production, be expected to be used widely in LED chip encapsulation field.
Description
Technical field
The present invention relates to organosilicon material class adhesive techniques field, particularly in a kind of add-on type LED encapsulation material
The preparation method of viscosifier.
Background technology
It is extremely low and can the spy such as deep layer vulcanization that add-on type liquid silicon rubber has no coupling product in sulfidation, shrinkage factor
Point, is the important auxiliary material of LED Packaging Industry, in electronic devices and components, power circuitry module, large-scale surface-mounted integrated circuit, LED etc.
Field is rapidly developed.But because after add-on type liquid silicon rubber sulfuration, the surface overwhelming majority is nonpolar organic group,
Show low cohesive energy, and lack the group with reactivity, thus it is poor to the adhesive property of base material, improves addition
The adhesive property of type liquid silastic is conducive to expanding its application in LED encapsulation field further.
At present, the cementability improving add-on type liquid silicon rubber with base material mainly has 3 kinds of methods:One is using silane coupling agent pair
Processed by viscous substrate surface, this method increased the use operation of silane coupling agent, increased production time and work load with
Production efficiency is caused to reduce；Two be by add the adhesion promoters of the silane containing reactive functional groups or siloxane oligomer Lai
Improve the cementability of add-on type liquid silicon rubber, introduce the polar functional group that some can promote cementability, such as epoxide group, propylene
Esters of gallic acid, but the method synthesis and post-processing step are more complicated and relatively costly, now also do not have industrialized production；Three is logical
Cross and improve cementability by adding viscosifier, this method is easy to operate, but it is compatible with base rubber to be usually present viscosifier
Property is poor, the problems such as catalyst is easily poisoned.
For viscosifier in addition-type silicon rubber, it first has to there is the preferable compatibility with silicone rubber main component, in energy
While playing bonding effect, do not affect various performances after original curing process and solidification.Consider above composite factor, existing
Mainly with viscosifier based on synthesizing, organosilicon systems introduce the various groups with cementability or element, such as epoxy
Base, acryloxy, ester group, NCO, alkoxyl, silicon hydrogen-based, Silatrane Derivatives, vinyl, B, N, S, P unit
Element etc., the silane with these groups or silicone condensation are become oligomer as viscosifier.Chinese invention patent application CN
102775611A discloses a kind of preparation method of viscosifier, the method adopt organotin catalyzed hydroxy silicon oil and KH-560 and
KH-570 obtains viscosifier, and described viscosifier are colourless or light yellow transparent liquid, uses in dual composition addition type silicones
When, intersolubility is very good, occurs without metachromatism, but when this viscosifier is used for LED organic silicon packaging glue, organotin may make
Pt catalyst poisoning.As the viscosifier of LED organic silicon packaging glue, silica gel and base material is not only needed to have preferable cementability, no
Easily make Pt catalyst poisoning, to also need to preparation method simple simultaneously, possesses economic worth.
Content of the invention
The present invention is directed to the deficiencies in the prior art, provides a kind of LED packaging plastic viscosifier and preparation method thereof, this thickening
Agent and organosilicon LED encapsulation material have the good compatibility, and the preparation process of this viscosifier does not produce hydrogen chloride etc. and is difficult
Recycling and the by-product that catalyst poisoning can be made.Utilize first step hydrosilylation simultaneously, change third can be passed through
The difference of olefin(e) acid ester based monomer, thus introducing different polar groups, second step adopts base catalyst, after the completion of reaction and lead to
Peracid neutralizes, thus being filtered to remove catalysts, operation is easier, has carried out improvement to existing viscosifier synthetic technology excellent
Change, improve the adhesive property of addition-type silicon rubber while not affecting other performances.
One of present invention additional organosilicon rubber viscosifier, its feature is：Acrylic acid is comprised in its structure
At least one in ester group, alkoxyl, and can be different according to the group on acrylate base monomer in first step reaction, introduce not
Same polar group.
In order to reach above-mentioned technique effect, the present invention takes technical scheme below：This viscosifier is to be tested by two steps,
The first step, using by the Alkoxy monomeric containing si-h bond and acrylate base monomer, is added by silicon hydrogen and obtains with alkoxyl
With acrylate-based intermediate product, second step passes through intermediate product and the acrylate radical siloxane of synthesis in base catalyst
In the presence of be hydrolyzed condensation, then using acid neutralization, filter, washing, be dried, revolving removes low molecule by-product, obtains colourless
Transparent viscosifier.
Specific experiment process of the present invention comprises the steps：The ratio of the amount of material is 1:1-1.2 acrylate-based list
Body is added in reaction bulb with trimethoxy silicon hydrogen alkane, and adds the toluene of 4 times of two kinds of total weight of monomer quality of quality as solvent,
Magneton stirring mixing；60-80 DEG C of intensification, stirs 0.5h；Add in reaction bulb and account for the chlorine that reactant gross mass are 20-80ppm
Platinic acid catalyst, reacts 3-4h；Then being added dropwise to the ratio of the amount of trimethoxy material is 1:1 acrylate radical siloxane,
And add and account for the base catalyst that gross mass is 0.8%, stirring reaction 2-4h at 60-80 DEG C；Add acid to be neutralized to neutrality, stir
Mix reaction 1h, stop heating, reaction finishes, cooling, and add dry white carbon black to be adsorbed, discharging；Add normal heptane, water
Wash, be dried, filter, filtrate is put in revolving bottle, adopt rotavapor under vacuum to remove low molecule 2h at 100-120 DEG C,
Obtain final product water white viscosifier.
Described acrylic ester monomer is just being selected from diacrylate -1,6-HD ester, n-butyl acrylate, methacrylic acid
One or more of butyl ester, glycidyl methacrylate.As the preferred version of the present invention, aforesaid propylene perester radical
Siloxane starting material is selected from 3- trimethoxy silane propyl acrylate, 2- acrylic acid 3- (diethoxymethyl silicyl) propyl diester
One of.
Described chloroplatinic acid catalyst is the aqueous isopropanol of 10000ppm for chloroplatinic acid content.Described base catalyst choosing
From KOH, NaOH, NaHCO3、LiOH·H2O and Ba (OH)2·2H2At least one in O, more preferably LiOH H2O.Acid is selected from
HCl、H2SO4、CH3COOH, stearic acid, at least one in p-phthalic acid and ethanedioic acid, more preferably stearic acid.Described third
The ratio preferably 1 of the amount of addition material of olefin(e) acid ester based monomer and trimethoxy silicon hydrogen alkane:1.2；Particularly preferably 1:1.1；
As the preferred version of the present invention, first step reaction temperature is preferably 60～80 DEG C, particularly preferably 70 DEG C；Add
Platinum catalyst amount be preferably 20～60ppm, particularly preferably 50ppm；Response time is preferably 3～4h, particularly preferably
For 4h；Base catalyst addition accounts for and adds the 0.5%～1% of monomer total amount, particularly preferably 0.8%；Reaction temperature is preferred
For 60～80 DEG C, particularly preferably 80 DEG C；As the preferred version of the present invention, the second step response time is preferably 2～4h, especially
It is preferably 3h；As the preferred version of the present invention, Rotary Evaporators remove low molecule temperature and are preferably 100～120 DEG C, especially excellent
Elect 110 DEG C as.
The invention has the beneficial effects as follows：It is used in dual composition addition type silicon resin system with the viscosifier of this method synthesis,
The compatibility is very good, occurs without that change is mixed to send out phenomenon turbid；No any abnormal flavour, the addition of the organic silicon rigidity-increasing stick being provided using the present invention
Type rubber composition and base material have good adhesive property；The method raw material that the present invention prepares this viscosifier is easy to get, reacts
Mild condition, workable it is easy to industrialized production, be expected to be used widely in LED chip encapsulation field.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not used to
Limit the present invention.
Embodiment 1
Add in 250mL there-necked flask 6.53g diacrylate -1,6-HD ester and 6.83g trimethoxy silicon hydrogen alkane in
In reaction bulb, add 50.26g toluene, heat up 70 DEG C, magneton stirring mixing 0.5h, it is subsequently adding 50ppm platinum catalyst, instead
Answer 4h, then slowly in there-necked flask, add 11.99g 2- acrylic acid 3- (diethoxymethyl silicyl) propyl diester, stir
After mixing 0.5h, add 0.16g LiOH H2O, reacts 3h after dripping, and adds 0.378g stearic acid, stirring reaction after addition
1h, stops heating, cooling, adds white carbon black to be adsorbed, discharging, after completion of the reaction, adds normal heptane, washing, layering, adds no
Aqueous sodium persulfate is dried, and filters, filtrate is put in revolving bottle, vacuum removal small molecule 2h at 110 DEG C, obtain final product water white
Viscosifier.
Embodiment 2
Add 7.12g glycidyl methacrylate and 6.71g trimethoxy silicon hydrogen alkane in anti-in 250mL there-necked flask
Answer in bottle, add 53.26g toluene, heat up 70 DEG C, magneton stirring mixing 0.5h, it is subsequently adding 50ppm platinum catalyst, reaction
4h, then slowly adds 12.05g 2- acrylic acid 3- (diethoxymethyl silicyl) propyl diester, stirring in there-necked flask
After 0.5h, add 0.165g LiOH H2O, reaction 3h after dripping, addition 0.382g stearic acid, stirring reaction 1h after addition,
Stop heating, cooling, add white carbon black to be adsorbed, discharging, after completion of the reaction, add normal heptane, washing, layering, add anhydrous
Sodium sulfate is dried, and filters, filtrate is put in revolving bottle, vacuum removal small molecule 2h at 110 DEG C, obtain final product water white increasing
Stick.
Embodiment 3
Add 7.18g n-BMA and 6.59g trimethoxy silicon hydrogen alkane in reaction bulb in 250mL there-necked flask
In, add 55.62g toluene, heat up 70 DEG C, magneton stirring mixing 0.5h, it is subsequently adding 50ppm platinum catalyst, react 4h, so
Slowly in there-necked flask, add 12.35g 2- acrylic acid 3- (diethoxymethyl silicyl) propyl diester afterwards, stir 0.5h
Afterwards, add 0.16g LiOH H2O, reacts 3h after dripping, and adds 0.385g stearic acid, stirring reaction 1h after addition, stops
Heating, cooling, add white carbon black to be adsorbed, discharging, after completion of the reaction, add normal heptane, washing, layering, add anhydrous slufuric acid
Sodium is dried, and filters, filtrate is put in revolving bottle, vacuum removal small molecule 2h at 110 DEG C, obtain final product water white thickening
Agent.
Embodiment 4
Add 6.53g diacrylate -1,6-HD ester and 3g trimethoxy silicon hydrogen alkane in reaction in 250mL there-necked flask
In bottle, add 41.85g toluene, heat up 70 DEG C, magneton stirring mixing 0.5h, it is subsequently adding 50ppm platinum catalyst, react 4h,
Then in there-necked flask, slowly add 12.85g 3- trimethoxy silane propyl acrylate, after stirring 0.5h, add 0.163g
LiOH·H2O, reacts 3h after dripping, and adds 0.382g stearic acid, stirring reaction 1h after addition, stops heating, cooling, adds
White carbon black is adsorbed, discharging, after completion of the reaction, adds normal heptane, washing, layering, adds anhydrous sodium sulfate drying, filter, will
Filtrate is put in revolving bottle, vacuum removal small molecule 2h at 110 DEG C, obtains final product water white viscosifier.
Embodiment 5
Add 7.26g glycidyl methacrylate and 6.71g trimethoxy silicon hydrogen alkane in anti-in 250mL there-necked flask
Answer in bottle, add 53.27g toluene, heat up 70 DEG C, magneton stirring mixing 0.5h, it is subsequently adding 50ppm platinum catalyst, reaction
4h, then slowly adds 12.85g 3- trimethoxy silane propyl acrylate in there-necked flask, after stirring 0.5h, adds
0.158g LiOH·H2O, reacts 3h after dripping, and adds 0.371g stearic acid, stirring reaction 1h after addition, stops heating, fall
Temperature, adds white carbon black to be adsorbed, discharging, after completion of the reaction, adds normal heptane, washing, layering, adds anhydrous sodium sulfate drying,
Filter, filtrate is put in revolving bottle, vacuum removal small molecule 2h at 110 DEG C, obtain final product water white viscosifier.
Embodiment 6
Add 7.32g n-BMA and 6.72g trimethoxy silicon hydrogen alkane in reaction bulb in 250mL there-necked flask
In, add 55.86g toluene, heat up 70 DEG C, magneton stirring mixing 0.5h, it is subsequently adding 50ppm platinum catalyst, react 4h, so
Slowly in there-necked flask, add 12.08g 2- acrylic acid 3- (diethoxymethyl silicyl) propyl diester afterwards, stir 0.5h
Afterwards, add 0.159g LiOH H2O, reacts 3h after dripping, and adds 0.379g stearic acid, stirring reaction 1h after addition, stops
Heating, cooling, add white carbon black to be adsorbed, discharging, after completion of the reaction, add normal heptane, washing, layering, add anhydrous slufuric acid
Sodium is dried, and filters, filtrate is put in revolving bottle, vacuum removal small molecule 2h at 110 DEG C, obtain final product water white thickening
Agent.
Comparative example
By 50.7g viscosity be 4500cp end-vinyl silicones, 48.75g viscosity be the hydrogeneous silicones of 3700cp, 1.5g
KH560 and 0.18g inhibitor carries out mix homogeneously, mix homogeneously, adds 0.11g platinum catalyst mix homogeneously, in vacuum
For deaeration 20min under 0.1MPa, then at 100 DEG C, solidify 1h, at 150 DEG C, solidify 3h.
For in embodiment 1-6, silica gel preparation is shown in that comparative example is above-mentioned, is then respectively adding the viscosifier in embodiment 1-6,
Base material is bondd and tests cohesive force, in addition, curing process condition is identical with comparative example.
Adhesive property is tested
Using thrust machine, according to the LED packaging plastic viscosifier prepared by GB/T11211-2009 testing example 1-6 to not
With the bonding force of bonding substrates, and contrasted with traditional viscosifier KH560.
Note 1. bonding force is primarily referred to as shear strength/MPa between different substrate materials；
2. viscosifier addition fraction is 1.5%.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention scope, every in the present invention
Spirit and principle within, any modification, equivalent substitution and improvement done etc., all this is included in protection scope of the present invention
Within.
Claims (6)
1. a kind of preparation method for organic silica gel system viscosifier is it is characterised in that comprise the steps：Amount by material
Ratio be 1:The acrylate base monomer of 1-1.2 is added in reaction bulb with trimethoxy silicon hydrogen alkane, and adds 4 times two kinds of quality
The toluene of total weight of monomer quality is as solvent, magneton stirring mixing；60-80 DEG C of intensification, stirs 0.5h；Add in reaction bulb and account for
Reactant gross mass are the chloroplatinic acid catalyst of 20-80ppm, react 3-4h；Then be added dropwise to the amount of trimethoxy material it
Than for 1:1 acrylate radical siloxane, and add and account for the base catalyst that gross mass is 0.8%, stir anti-at 60-80 DEG C
Answer 2-4h；Add acid to be neutralized to neutrality, stirring reaction 1h, stop heating, reaction finishes, cooling, and add dry white carbon black to enter
Row absorption, discharging；Add normal heptane, washing, dry, filtration, filtrate is put in revolving bottle, using rotation at 100-120 DEG C
Turn evaporimeter vacuum removal low molecule 2h, obtain final product water white viscosifier.
2. the preparation method according to right 1 is it is characterised in that described acrylic ester monomer is selected from diacrylate -1,6-
One or more of hexanediol ester, n-butyl acrylate, n-BMA, glycidyl methacrylate.
3. the preparation method according to right 1 is it is characterised in that described acrylate-based siloxane starting material is selected from 3- front three
TMOS propyl acrylate, one of 2- acrylic acid 3- (diethoxymethyl silicyl) propyl diester.
4. the preparation method according to right 1 is it is characterised in that described chloroplatinic acid catalyst for chloroplatinic acid content is
The aqueous isopropanol of 10000ppm.
5. the preparation method according to right 1 is it is characterised in that described base catalyst is selected from KOH, NaOH, NaHCO3、
LiOH·H2O and Ba (OH)2·2H2One of O.
6. the preparation method according to right 1 is it is characterised in that described acid is selected from HCl, H2SO4、CH3COOH, stearic acid, right
One of phthalic acid and ethanedioic acid.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108192551A (en) * | 2017-12-30 | 2018-06-22 | 广州市白云化工实业有限公司 | Transparent, high adhesiveness silane-modified adhesive and preparation method thereof |
| CN112979961A (en) * | 2019-12-17 | 2021-06-18 | 中蓝晨光化工研究设计院有限公司 | Preparation method of macromolecular silicone rubber tackifier |
| CN116987245A (en) * | 2023-07-25 | 2023-11-03 | 杰瑞高科(广东)有限公司 | Thermoplastic pipeline non-excavation repair material and preparation method thereof |
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| CN104877139A (en) * | 2015-05-14 | 2015-09-02 | 深圳新宙邦科技股份有限公司 | Tackifier for LED packaging adhesive and preparation method of tackifier |
| CN105368339A (en) * | 2015-11-27 | 2016-03-02 | 广州市回天精细化工有限公司 | Tackifier for addition-cured organosilicone adhesive sealant, preparation method and composition used in preparation |
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| CN102936414A (en) * | 2012-08-27 | 2013-02-20 | 湖北环宇化工有限公司 | High refraction and high adhesion large power LED packaging organosilicon material and preparation method thereof |
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| CN112979961A (en) * | 2019-12-17 | 2021-06-18 | 中蓝晨光化工研究设计院有限公司 | Preparation method of macromolecular silicone rubber tackifier |
| CN116987245A (en) * | 2023-07-25 | 2023-11-03 | 杰瑞高科(广东)有限公司 | Thermoplastic pipeline non-excavation repair material and preparation method thereof |
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