CN104086784B - A kind of self-emulsifying modified organic silicone resin emulsion and preparation method thereof and application - Google Patents
A kind of self-emulsifying modified organic silicone resin emulsion and preparation method thereof and application Download PDFInfo
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Abstract
The invention belongs to electronic package material technical field, disclose a kind of self-emulsifying modified organic silicone resin emulsion and preparation method thereof and application. The preparation method of described self-emulsifying modified organic silicone resin emulsion is: the PEPA containing sulfonic group/carboxyl first with containing isocynate silane coupling agent is reacted, then add siloxanyl monomers to react, obtain the organic siliconresin of self-emulsifying modification, then the organic siliconresin of self-emulsifying modification is added water and carries out emulsification, and add nertralizer to neutralize, obtain self-emulsifying modified organic silicone resin emulsion. Self-emulsifying modified organic silicone resin emulsion of the present invention has good automatic emulsifying performance, good mechanical property and good curing performance, can be used for the encapsulation of ceramic resistor.
Description
Technical field
The invention belongs to electronic package material technical field, be specifically related to a kind of self-emulsifying modified organic silicone resinEmulsion and preparation method thereof and application.
Background technology
Encapsulating material refers to and the resistance capacitance of electron trade etc. can be sealed, seals or filling oneElectron-like adhesive, can play the effects such as waterproof, protection against the tide, heat radiation.
Organic siliconresin has the skeleton that silica silicon key replaces, and at high temperature, the organic group on silicon atomGroup decomposes, and intermolecularly forms new silica silicon key or silica carbon bond, so it is steady to have excellent thermal oxideQualitative, there is good electrical insulation capability, moisture resistance, waterproof, the performance such as weather-proof simultaneously, due to above feature,Conventional organic siliconresin is as packaging plastic.
But conventional organic silicon packaging glue mostly is solvent-borne type packaging plastic now, mainly molten with benzene class or alcoholsAgent is main, and organic siliconresin exists intensity lower, and baking temperature is high, need to make two when low-temperature settingThe shortcomings such as component.
In view of the foregoing, the present invention combines the pluses and minuses of polyurethane and organic siliconresin, learn from other's strong points to offset one's weaknesses,Ceramic resistor encapsulation self-emulsifying modified organic silicone resin emulsion is provided, has there is excellent heat resistance, bondingProperty, alcohol resistance and electrical insulating property, and can solve the shortcoming of existing packaging plastic.
Summary of the invention
In order to solve the shortcoming and defect part of prior art, it is certainly a kind of that primary and foremost purpose of the present invention is to provideThe preparation method of emulsification modified organic silicone resin emulsion.
Another object of the present invention is to provide a kind of self-emulsifying modification being prepared by above-mentioned preparation method to haveMachine silicones emulsion.
A further object of the present invention is to provide a kind of above-mentioned self-emulsifying modified organic silicone resin emulsion in ceramic electricalApplication in resistance encapsulation.
The object of the invention is achieved through the following technical solutions:
A preparation method for self-emulsifying modified organic silicone resin emulsion, comprises following operating procedure:
(1) to add 11.73～12.46 mass parts containing sulphur with the reactor of agitator and condensation reflux unitThe PEPA of acidic group/carboxyl, under 120～130 DEG C of conditions, vacuumizes the 1.5～2h that dewaters, and is cooled to65～70 DEG C, control speed of agitator is 150～175rpm, then in reactor, adds 7.54～8.27 qualityPart, containing isocynate silane coupling agent, is warming up to 75～80 DEG C of reaction 10～20min, is then cooled to immediately60 DEG C, add 80 mass parts siloxanyl monomers, and drip continuously 24.23～24.70 mass parts deionized waters,Time for adding is 0.5h, then in 0.25～0.3h, is warming up to 90～100 DEG C, after insulation 1～1.5h, is distilled toSteam without cut, be then cooled to 40 DEG C of dischargings, obtain self-emulsifying modified organic silicone resin;
(2) in above-mentioned self-emulsifying modified organic silicone resin, add 350～400 mass parts deionized waters, at heightUnder speed shear mixer, setting speed is that 1500～2000rpm carries out emulsification 10～15min, adds 0.25～0.27The neutralization of mass parts nertralizer, continues emulsification 10～15min, obtains self-emulsifying modified organic silicone resin emulsion.
The number-average molecular weight of the PEPA containing sulfonic group/carboxyl described in step (1) is 733～771,This material can prepare by the preparation method in patent CN103396541A.
Described in step (1), contain the preferred 3-NCO of isocynate silane coupling agent propyl trimethoxy siliconAlkane (KH-901) or 3-NCO propyl-triethoxysilicane (KH-907), more preferably 3-isocyanic acidEster group propyl-triethoxysilicane (KH-907);
Siloxanyl monomers described in step (1) be dimethyldimethoxysil,ne, MTMS,In dimethyldiethoxysilane and MTES, the composition of at least two kinds and silester is mixedCompound, the methyl being directly connected with silicon atom in siloxanyl monomers and the mol ratio of silicon atom are 1.3～1.5; InstituteState the combination of the preferred dimethyldiethoxysilane of composition and MTES; Described silesterAccount for 25% of siloxanyl monomers gross mass.
The described nertralizer of step (2) is HMDS.
A kind of self-emulsifying modified organic silicone resin emulsion, prepares by above-mentioned preparation method.
The application of above-mentioned self-emulsifying modified organic silicone resin emulsion in ceramic resistor encapsulation, concrete application processFor: in mass parts, by 1 part of self-emulsifying modified organic silicone resin emulsion, 5 parts of quartz sand, 1 part of silica flour,0.5 part of talcum powder at room temperature mixes, stir after 5min and obtain slurry, by filling slurry in pottery is housedIn the groove of porcelain resistance, at 100 DEG C, solidify 1min, obtain the ceramic resistor after encapsulation.
Have the following advantages and beneficial effect by preparation method of the present invention and the product tool that obtains:
(1) the present invention contains the PEPA of sulfonic group/carboxyl by introducing, at hydrophilic radical sulfonic group and carboxylicUnder the effect of base, make resin just can reach the effect of emulsification without emulsifying agent, self-emulsifying forms emulsion; SimultaneouslyThe carboxyl of introducing can be used as the catalyst of organosilicon hydrolyzation condensation reaction, has avoided use small molecule salt acid conductCatalyst impacts product property;
(2) the present invention adopts isocyanates to carry out modification simultaneously, combines organic siliconresin and polyurethane resinAdvantage, overcome the low weakness of organic siliconresin intensity, in application and ceramic resistor encapsulation, have excellentPerformance;
(3) the present invention adopts HMDS as nertralizer, on the one hand can in and carboxyl, obtainBetter hydrophily; On the other hand, in solidification process, the release again of HMDS, playsThe effect of curing agent, simultaneously again obtain carboxyl, hydrophily weakens, can reduce solidification temperature, reduce residualRemaining moisture and shorten hardening time.
(4) the present invention makes water as decentralized medium, has reduced the row of VOC (VOC)Put, meet environmental protection demand; And preparation method's reaction condition gentleness of the present invention, easy and simple to handle, be easy to workIndustryization is produced.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limitIn this.
Embodiment 1
The preparation method of a kind of self-emulsifying modified organic silicone resin emulsion of the present embodiment, comprises following operation stepRapid:
(1) in the reactor with agitator and condensation reflux unit, add the equal molecule of 11.73 mass fractionAmount is 733 the PEPA containing sulfonic group/carboxyl, under 120 DEG C of conditions, vacuumizes the 1.5～2h that dewaters,Be cooled to 65 DEG C, controlling speed of agitator is under 150rpm condition, in reactor, adds 7.54 mass parts 3-NCO propyl trimethoxy silicane (KH-901), is warming up to 75～80 DEG C of reaction 10min, then verticalBe cooled to 60 DEG C, add 8.9 mass parts MTMSs, 51.1 mass parts dimethylformamide dimethyl oxygenBase silane and 20 mass parts silester, and drip continuously 24.23 mass parts deionized waters, time for adding is0.5h is then warming up to 90 DEG C in 0.25h, after insulation 1h, is distilled to without cut and steams, and is cooled to 40 DEG CRear discharging, obtains self-emulsifying modified organic silicone resin;
(2) in above-mentioned self-emulsifying modified organic silicone resin, add 350 mass parts deionized waters, cutting at a high speedCut under mixer, setting speed is that 1500rpm carries out emulsification 10min, adds 0.25 mass parts hexamethyl twoSilazane neutralization, continues emulsification 10min, obtains self-emulsifying modified organic silicone resin emulsion.
The encapsulation of ceramic resistor:
In mass parts, by the self-emulsifying modified organic silicone resin emulsion of 1 part of the present embodiment, 5 parts of quartz sands,1 part of silica flour, 0.5 part of talcum powder at room temperature mixes, and after stirring 5min, obtains slurry, and slurry is filled withBe loaded in the groove that ceramic resistor (demarcation resistance value: (2 ± 0.05) k Ω, rated power 5W) is housed,At 100 DEG C, solidify 1min, obtain the ceramic resistor after encapsulation.
Embodiment 2
The preparation method of a kind of self-emulsifying modified organic silicone resin emulsion of the present embodiment, comprises following operation stepRapid:
(1) in the reactor with agitator and condensation reflux unit, add the equal molecule of 12.46 mass fractionAmount is 750 the PEPA containing sulfonic group/carboxyl, under 130 DEG C of conditions, vacuumizes the 2h that dewaters, and fallsTemperature is to 70 DEG C, and controlling speed of agitator is under 160rpm condition, in reactor, adds 8.27 mass parts 3-differentCyanate ester based propyl trimethoxy silicane (KH-901), is warming up to 80 DEG C of reactions and is cooled to immediately after 20min60 DEG C, add 23.14 mass parts MTMSs, 38.86 mass parts dimethyldimethoxysil,neWith 20 mass parts silester, and drip continuously 24.70 mass parts deionized waters, time for adding is 0.5h,Then in 0.3h, be warming up to 100 DEG C, insulation is distilled to without cut after 1.5h and steams, and goes out after being cooled to 40 DEG CMaterial, obtains self-emulsifying modified organic silicone resin,
(2) in above-mentioned self-emulsifying modified organic silicone resin, add 400 mass parts deionized waters, cutting at a high speedCut under mixer, setting speed is that 2000rpm carries out emulsification 15min, adds 0.27 mass parts hexamethyl twoSilazane neutralization, continues emulsification 15min, obtains self-emulsifying modified organic silicone resin emulsion.
The encapsulation of ceramic resistor:
In mass parts, by the self-emulsifying modified organic silicone resin emulsion of 1 part of the present embodiment, 5 parts of quartz sands,1 part of silica flour, 0.5 part of talcum powder at room temperature mixes, and after stirring 5min, obtains slurry, and slurry is filled withBe loaded in the groove that ceramic resistor (demarcation resistance value: (2 ± 0.05) k Ω, rated power 5W) is housed,At 100 DEG C, solidify 1min, obtain the ceramic resistor after encapsulation.
Embodiment 3
The preparation method of a kind of self-emulsifying modified organic silicone resin emulsion of the present embodiment, comprises following operation stepRapid:
(1) in the reactor with agitator and condensation reflux unit, add the equal molecule of 11.73 mass fractionAmount is 771 the PEPA containing sulfonic group/carboxyl, under 130 DEG C of conditions, vacuumizes the 2h that dewaters, and fallsTemperature is to 70 DEG C, and controlling speed of agitator is under 170rpm condition, in reactor, adds 8.27 mass parts 3-differentCyanate ester based propyl-triethoxysilicane (KH-907), is warming up to 80 DEG C of reactions and is cooled to immediately after 20min60 DEG C, add 11.4 mass parts MTESs, 48.6 mass parts dimethyldiethoxysilanes and20 mass parts silester, and drip continuously 24.23 mass parts deionized waters, time for adding is 0.5h, soAfter in 0.25h, be warming up to 100 DEG C, insulation is distilled to without cut after 1h and steams, be cooled to 40 DEG C after discharging,Obtain self-emulsifying modified organic silicone resin;
(2) in above-mentioned self-emulsifying modified organic silicone resin, add 350 mass parts deionized waters, cutting at a high speedCut under mixer, setting speed is that 2000rpm carries out emulsification 15min, adds 0.25 mass parts hexamethyl twoSilazane neutralization, continues emulsification 15min, obtains self-emulsifying modified organic silicone resin emulsion.
The encapsulation of ceramic resistor:
In mass parts, by the self-emulsifying modified organic silicone resin emulsion of 1 part of the present embodiment, 5 parts of quartz sands,1 part of silica flour, 0.5 part of talcum powder at room temperature mixes, and after stirring 5min, obtains slurry, and slurry is filled withBe loaded in the groove that ceramic resistor (demarcation resistance value: (2 ± 0.05) k Ω, rated power 5W) is housed,At 100 DEG C, solidify 1min, obtain the ceramic resistor after encapsulation.
Embodiment 4
The preparation method of a kind of self-emulsifying modified organic silicone resin emulsion of the present embodiment, comprises following operation stepRapid:
(1) in the reactor with agitator and condensation reflux unit, add the equal molecule of 12.46 mass fractionAmount is 733 the PEPA containing sulfonic group/carboxyl, under 120 DEG C of conditions, vacuumizes the 1.5h that dewaters,Be cooled to 65 DEG C, controlling speed of agitator is under 175rpm condition, in reactor, adds 7.54 mass parts 3-NCO propyl-triethoxysilicane (KH-907), be warming up to 75 DEG C reaction 10min after immediately coolingTo 60 DEG C, add 29.71 mass parts MTESs, 30.29 mass parts dimethyl diethoxy siliconAlkane and 20 mass parts silester, and drip continuously 24.23 mass parts deionized waters, time for adding is 0.5h,Then in 0.3h, be warming up to 90 DEG C, insulation is distilled to without cut after 1.5h and steams, and goes out after being cooled to 40 DEG CMaterial, obtains self-emulsifying modified organic silicone resin;
(2) in above-mentioned self-emulsifying modified organic silicone resin, add 400 mass parts deionized waters, cutting at a high speedCut under mixer, setting speed is that 1500rpm carries out emulsification 10min, adds 0.27 mass parts hexamethyl twoSilazane neutralization, continues emulsification 10min, obtains self-emulsifying modified organic silicone resin emulsion.
The encapsulation of ceramic resistor:
In mass parts, by the self-emulsifying modified organic silicone resin emulsion of 1 part of the present embodiment, 5 parts of quartz sands,1 part of silica flour, 0.5 part of talcum powder at room temperature mixes, and after stirring 5min, obtains slurry, and slurry is filled withBe loaded in the groove that ceramic resistor (demarcation resistance value: (2 ± 0.05) k Ω, rated power 5W) is housed,At 100 DEG C, solidify 1min, obtain the ceramic resistor after encapsulation.
Embodiment 5
The preparation method of a kind of self-emulsifying modified organic silicone resin emulsion of the present embodiment, comprises following operation stepRapid:
(1) in the reactor with agitator and condensation reflux unit, add the equal molecule of 12.00 mass fractionAmount is 771 the PEPA containing sulfonic group/carboxyl, under 125 DEG C of conditions, vacuumizes the 1.6h that dewaters,Be cooled to 67 DEG C, controlling speed of agitator is under 150rpm condition, in reactor, adds 8.03 mass parts 3-NCO propyl-triethoxysilicane (KH-907), be warming up to 78 DEG C reaction 16min after immediately coolingTo 60 DEG C, add 10.63 mass parts MTESs, 49.37 mass parts dimethyl diethoxy siliconAlkane and 20 mass parts silester, and drip continuously 24.54 mass parts deionized waters, time for adding is 0.5h,Then in 0.28h, be warming up to 93 DEG C, after insulation 1.25h, be distilled to without cut and steam, be cooled to after 40 DEG CDischarging, obtains self-emulsifying modified organic silicone resin;
(2) in above-mentioned self-emulsifying modified organic silicone resin, add 380 mass parts deionized waters, cutting at a high speedCut under mixer, setting speed is that 1800rpm carries out emulsification 15min, adds 0.26 mass parts hexamethyl twoSilazane neutralization, continues emulsification 15min, obtains self-emulsifying modified organic silicone resin emulsion.
The encapsulation of ceramic resistor:
In mass parts, by the self-emulsifying modified organic silicone resin emulsion of 1 part of the present embodiment, 5 parts of quartz sands,1 part of silica flour, 0.5 part of talcum powder at room temperature mixes, and after stirring 5min, obtains slurry, and slurry is filled withBe loaded in the groove that ceramic resistor (demarcation resistance value: (2 ± 0.05) k Ω, rated power 5W) is housed,At 100 DEG C, solidify 1min, obtain the ceramic resistor after encapsulation.
To in above embodiment encapsulation after ceramic resistor carry out Performance Detection, detection method and performance indications asShown in table 1, testing result is as shown in table 2.
Table 1 detection method and index
In table, Δ R represents the difference between the resistance value before resistance value and the test after test; R0 represents testFront resistance value.
Table 2 the performance test results
Can be found out by table 2 result, encapsulate by self-emulsifying modified organic silicone resin emulsion of the present inventionAfter the ceramic resistor wire resistor of comparing not encapsulation on service life, obtained obvious lifting.
Above-described embodiment is preferably embodiment of the present invention, but embodiments of the present invention are not subject to above-mentioned realityExecute routine restriction, other any do not deviate from the change done under Spirit Essence of the present invention and principle, modification,Substitute, combine, simplify, all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (10)
1. a preparation method for self-emulsifying modified organic silicone resin emulsion, is characterized in that comprising following operationStep:
(1) to add 11.73～12.46 mass parts containing sulphur with the reactor of agitator and condensation reflux unitThe PEPA of acidic group and carboxyl, under 120～130 DEG C of conditions, vacuumizes the 1.5～2h that dewaters, and is cooled to65～70 DEG C, control speed of agitator is 150～175rpm, then in reactor, adds 7.54～8.27 mass partsContaining isocynate silane coupling agent, be warming up to 75～80 DEG C of reaction 10～20min, be then cooled to immediately 60 DEG C,Add the mixture of 80 mass parts siloxanyl monomers and silester, and drip continuously 24.23～24.70 qualityPart deionized water, time for adding is 0.5h, then in 0.25～0.3h, is warming up to 90～100 DEG C, insulation 1～1.5hAfter be distilled to without cut and steam, be then cooled to 40 DEG C of dischargings, obtain self-emulsifying modified organic silicone resin;
(2) in above-mentioned self-emulsifying modified organic silicone resin, add 350～400 mass parts deionized waters, at heightUnder speed shear mixer, setting speed is that 1500～2000rpm carries out emulsification 10～15min, adds 0.25～0.27The neutralization of mass parts nertralizer, continues emulsification 10～15min, obtains self-emulsifying modified organic silicone resin emulsion.
2. the preparation method of a kind of self-emulsifying modified organic silicone resin emulsion according to claim 1, itsBe characterised in that: the number-average molecular weight of the described PEPA containing sulfonic group and carboxyl is 733～771.
3. the preparation method of a kind of self-emulsifying modified organic silicone resin emulsion according to claim 1, itsBe characterised in that: described containing isocynate silane coupling agent be 3-NCO propyl trimethoxy silicane or3-NCO propyl-triethoxysilicane.
4. the preparation method of a kind of self-emulsifying modified organic silicone resin emulsion according to claim 3, itsBe characterised in that: described is 3-NCO propyl-triethoxysilicane containing isocynate silane coupling agent.
5. the preparation method of a kind of self-emulsifying modified organic silicone resin emulsion according to claim 3, itsBe characterised in that: described siloxanyl monomers is dimethyldimethoxysil,ne, MTMS, twoThe composition of at least two kinds in methyldiethoxysilane and MTES, in siloxanyl monomers withThe methyl that silicon atom is direct connected and the mol ratio of silicon atom are 1.3～1.5.
6. the preparation method of a kind of self-emulsifying modified organic silicone resin emulsion according to claim 5, itsBe characterised in that: described composition is the combination of dimethyldiethoxysilane and MTES.
7. the preparation method of a kind of self-emulsifying modified organic silicone resin emulsion according to claim 5, itsBe characterised in that: the addition of described silester accounts for 25% of siloxanyl monomers gross mass.
8. the preparation method of a kind of self-emulsifying modified organic silicone resin emulsion according to claim 1, itsBe characterised in that: described nertralizer is HMDS.
9. a self-emulsifying modified organic silicone resin emulsion, is characterized in that: arbitrary by claim 1～8Preparation method described in prepares.
10. self-emulsifying modified organic silicone resin emulsion claimed in claim 9 answering in ceramic resistor encapsulationWith, it is characterized in that concrete application process is: in mass parts, by 1 part of self-emulsifying modified organic silicone resinEmulsion, 5 parts of quartz sands, 1 part of silica flour, 0.5 part of talcum powder at room temperature mix, and stir after 5minObtain slurry, in the groove of ceramic resistor is housed, at 100 DEG C, solidify 1min by filling slurry, obtainCeramic resistor after encapsulation.
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| WO2010008154A2 (en) * | 2008-07-15 | 2010-01-21 | Korea Bio-Gen Co., Ltd | Room temperature moisture curable hybrid resin, method of preparing the same and application thereof |
| CN101802046A (en) * | 2007-07-12 | 2010-08-11 | 陶氏环球技术公司 | Room temperature curable polymers and precursors thereof |
| CN103396541A (en) * | 2013-07-01 | 2013-11-20 | 华南理工大学 | Polyester polyol containing sulfonic/carboxyl and preparation method thereof |
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| CN101802046A (en) * | 2007-07-12 | 2010-08-11 | 陶氏环球技术公司 | Room temperature curable polymers and precursors thereof |
| WO2010008154A2 (en) * | 2008-07-15 | 2010-01-21 | Korea Bio-Gen Co., Ltd | Room temperature moisture curable hybrid resin, method of preparing the same and application thereof |
| CN103396541A (en) * | 2013-07-01 | 2013-11-20 | 华南理工大学 | Polyester polyol containing sulfonic/carboxyl and preparation method thereof |
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