CN101875725B - Vinyl silicon resin for reinforcing organic silicon pouring sealant and preparation method thereof - Google Patents
Vinyl silicon resin for reinforcing organic silicon pouring sealant and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a vinyl silicon resin for reinforcing an organic silicon pouring sealant and a preparation method thereof. The preparation method comprises the following steps of: adding an appropriate amount of hexamethyl disiloxane and tetramethyl divinylsiloxane into a mixture of hydrochloric acid, an organic solvent and water to perform reaction for some time and then adding tetraethoxysilane and bis-functional or trifunctional siloxane to perform reaction; adding a certain amount of hexamethyl disiloxane and tetramethyl divinylsiloxane according to circumstances, standing and demixing after the reaction is finished, washing lower mixed liquor with deionized water until the liquor is neutral, and drying the liquor to obtain the vinyl silicon resin. The spherical core of the silicon resin prepared by the method, namely SiO2 has high content, and the spherical shell is tightly encircled by an R3SiO0.5 layer, so the silicon resin has good reinforcing effect; and the resin has high solubility or dispersibility in silicon rubber, can be separately used as a reinforcing filler for the organic silicon pouring sealant, and can also be matched with other fillers, so that the organic silicon pouring sealant with required performance can be obtained.
Description
Technical field
The present invention relates to a kind of preparation method of silicone resin, relate in particular to for the preparation method of organic silicon potting adhesive reinforcement with silicone resin.
Background technology
Along with the high-tech areas such as electronic devices and components, power circuit module, large-scale surface-mounted integrated circuit, LED further realize high-performance, high reliability and miniaturization, and Working environment is harsher, require the embedding part must be between low temperature and the high temperature, move under the condition such as high speed rotating, this just requires Embedding Material to have good high and low temperature resistance, mechanical mechanics property, electrical insulation capability etc., could satisfy power circuit to the particular requirement of Embedding Material.In addition, Embedding Material generally also should be namely by low viscosity, higher toughness and dipping property, and the impregnation rate is greater than 98% between line, cure shrinkage, coefficient of linear expansion and internal stress are little, have excellent electrical property, 120 ℃ of dielectric characteristics variations are little, and flame retardant properties reaches UL V-0 level.
Using more Embedding Material at present is various synthetic polymers, and wherein the application with Resins, epoxy, urethane and silicon rubber is more extensive.Silicon rubber can keep elasticity for a long time in very wide temperature range, and do not absorb heat during sulfuration, not heat release, and have good electric property and chemical stability, be the preferred material of electric assembly embedding.By sulfuration mechanism, organic silicon electronic potting adhesive can be divided into two kinds of condensed type and add-on types, wherein additional organosilicon electronic potting adhesive owing to have in sulfidation, do not produce by product, shrinking percentage minimum, can deep layer vulcanization etc. characteristics, become the class joint sealant greatly developed work " organosilicon synthesis technique and product application " Chemical Industry Press such as () good fortune Song Min both at home and abroad.But the typical case is usually very poor without the performance of the silicon rubber of filling, as stretch and be no more than 0.4MPa the intensity, thermal conductivity is no more than 0.2W/MK, flame retardant rating does not reach UL V-0 level yet, thereby almost there is not use value (Feng Shengyu etc. work " organosilicon macromolecule and application thereof " Chemical Industry Press, 83).Therefore, in order to obtain to have the organosilicon electronic encapsulation material of corresponding better performance, just must correspondingly add the filler that some have reinforcement or heat conduction or flame retardant properties and other performance, improve the performance of potting compound.
The traditional reinforced filling of silicon rubber is white carbon black.A lot of as the organic silicon potting adhesive patent of reinforced filling with white carbon black both at home and abroad, US Patent No. 20077294682 and US20050212008 all adopt gas-phase silica reinforcement LED organosilicon material for packaging; Domestic patent CN 101121870A and CN 101565600A also all mention with white carbon black as reinforced filling.
Although can effectively improve the intensity of silicon rubber with white carbon black as reinforced filling, the sizing material viscosity after the reinforcement is usually all very large, is difficult to the embedding of electronic devices and components.
The MQ silicone resin is the good reinforced filling of room temperature vulcanized silicone rubber.The MQ silicone resin is by simple function silica unit (R
3SiO
0.5, i.e. M) and four sense silica unit (SiO
2, i.e. Q) and the more special organopolysiloxane of structure that forms, when R partly is vinyl substituted, then be called the vinyl MQ silicone resin.Little to the viscosity of sizing material with MQ silicone resin reinforcement silicon rubber.
The MQ silicone resin is as the reinforced filling of joint sealant, not only requires the viscosity of sizing material not quite, also requires to have preferably reinforcing effect.Retrieval is found, Chinese patent CN 101323667 discloses the preparation method that a kind of LED encapsulated strengthening is used methyl vinyl MQ resin, prepared vinyl MQ silicone resin clear, refractive index 1.46～1.51, but its number-average molecular weight only is 200～500, and reinforcing property is obviously not enough.Patent CN 101531760A discloses the preparation method of high performance silicon resin, and the method raw materials cost is low, and interpolation about 8% just can significantly improve the bonding strength of room temperature vulcanization organosilicon sizing agent, but prepared MQ silicone resin reinforcing property is unknown.Patent CN 101613475A discloses preparing MQ silicon resin by organic acid catalysis, has lowered the content of organic ion in the MQ silicone resin by utilizing organic acid catalyst, but the also reinforcing property of not mentioned silicone resin.Find also that by retrieval the patent that does not also prepare MDQ and MTQ silicone resin at present occurs.
Summary of the invention
The objective of the invention is the deficiency for current condition, a kind of HR highly reinforcing vinyl MQ (MDQ and MTQ) silicone resin and preparation method thereof and application are provided.
The preparation method of silicone resin of the present invention comprises the steps:
(1) add hexamethyldisiloxane and tetramethyl divinyl disiloxane in the mixture of concentrated hydrochloric acid, organic solvent and water, react in 70～80 ℃, the reaction times is 3～5min; Organic solvent described in this step is one or more of toluene, ethanol, dimethylbenzene; The molar mass summation of the hexamethyldisiloxane that adds in this step and tetramethyl divinyl siloxanes be in the system tetraethoxy molar mass 3/20～7/20.
(2) add tetraethoxy and two senses or trifunctional siloxanes in 300s-600s, reaction is 30～60min; Two functional silicones described in this step are one or more of dimethyldimethoxysil,ne, dimethyldiethoxysilane; Described trifunctional siloxanes is one or more of methyltrimethoxy silane, Union carbide A-162; Two functional silicone mole dosage maximums are no more than 0.19 of tetraethoxy molar mass, and minimum can be 0; The trifunctional siloxanes is one or more of methyltrimethoxy silane, Union carbide A-162; Trifunctional siloxanes mole dosage maximum is no more than 0.2 of tetraethoxy molar mass, and its content minimum also can be 0; When described two functional silicones or trifunctional content of siloxane are minimum value 0, the preparation product is the vinyl MQ silicone resin, and when adding two functional silicones, the preparation product is vinyl MDQ silicone resin, when adding the trifunctional siloxanes, the preparation product is vinyl MTQ silicone resin.
(3) if the hexamethyldisiloxane of (1) step adding and the molar weight sum of tetramethyl divinyl disiloxane are not more than 1/4 of tetraethoxy molar weight, then add some hexamethyldisiloxane and tetramethyl divinyl siloxanes, reaction 30～60min; The amount of hexamethyldisiloxane that this step adds and tetramethyl-divinyl sily oxide answers the mole total amount (comprising that (1) step adds) of added hexamethyldisiloxane and tetramethyl-divinyl sily oxide in the guarantee system to be no more than 0.85 of tetraethoxy molar weight in the system;
If the hexamethyldisiloxane that (1) step added and the molar weight sum of tetramethyl divinyl disiloxane then need not to add hexamethyldisiloxane and tetramethyl divinyl disiloxane greater than 1/4 of tetraethoxy molar weight again;
It is 3%～10% that the tetramethyl divinyl disiloxane that adds is measured the massfraction (m (vinyl)/(m (hexamethyldisiloxane)+m (tetramethyl divinyl disiloxane)+m (tetraethoxy) * 0.28)) that should satisfy the system medium vinyl;
(4) with (3) mixture standing demix, take out lower floor's liquid, extremely neutral with deionized water wash;
(5) desolventize and low-boiling-point substance in decompression and 130 ℃ of lower oven dry, steamings, get final product to get the vinyl MQ silicone resin; Reduced pressure described in this step is generally-0.1MPa; Low-boiling-point substance described in this step refers to not participate in the alkylsiloxane of reaction.
The vinyl polysiloxane characteristics of utilizing preparation method of the present invention to prepare are that the MQ silicone resin ball core segment that synthesizes is SiO
2Content is higher, and spherical shell is by R
3SiO
0.5Layer closely surrounds, thereby has higher reinforcing effect, and the dissolving in silicon rubber (or dispersion) better, is particularly suitable for doing the reinforced filling of organic silicon potting adhesive; The MDQ silicone resin is because having two senses link, and not only reinforcing effect is good, and its snappiness also is improved; Adding the MTQ silicone resin that the T functional unit makes also has better reinforcing effect, and the three all can do separately the reinforced filling of organic silicon potting adhesive, also can with share with other fillers, thereby obtain the organic silicon potting adhesive of desired properties.This synthetic method production efficiency is high in addition, is suitable for industrial production.
Embodiment
Specific embodiment 1:
In the 500mL there-necked flask, add the 11.3g hexamethyldisiloxane, 28.8g tetramethyl divinyl disiloxane, 30g concentrated hydrochloric acid, 30g toluene, 15g ethanol, 45g water under agitation reacts 3min in 70-80 ℃, the 156g tetraethoxy is added in 60min in the bottle react 60min, move into the separating funnel standing demix, take out lower floor's mixed solution, to neutral, namely get vinyl MQ silicone resin in decompression and 130 ℃ of lower oven dry with deionized water wash.
The 7g vinyl MQ silicone resin of above-mentioned preparation is dissolved with 10g toluene, the adding viscosity is 500mPa.s, contents of ethylene is in 1.2% the 100g vinyl silicone oil, remove solvent after stirring under reduced pressure, adding 140g median size is that aluminum oxide, the 60g median size of 15 μ m is the aluminium hydroxide of 23 μ m, 15.4g hydrogen content is 0.35% containing hydrogen silicone oil, 0.38g platinum catalyst, 0.01g inhibitor, deaeration 8 minutes under 0.1MPa after mixing, then inject in the mould of a 3mm * 160mm * 160mm, self-vulcanizing 24 hours, make film.
Specific embodiment 2:
In the 500mL there-necked flask, add the 28.9g hexamethyldisiloxane, 8.3g tetramethyl divinyl disiloxane, 30g concentrated hydrochloric acid, 30g toluene, 15g ethanol, 45g water under agitation reacts 3min in 70-80 ℃, 156g tetraethoxy and 20.4g methyltrimethoxy silane is added in 60min in the bottle react 60min, move into the separating funnel standing demix, take out lower floor's mixed solution, to neutral, namely get vinyl MTQ silicone resin in decompression and 130 ℃ of lower oven dry with deionized water wash.
The sample preparation is with example 1
Specific embodiment 3:
In the 500mL there-necked flask, add 17.94 hexamethyldisiloxane, 7.02g tetramethyl divinyl disiloxane, the 30g concentrated hydrochloric acid, 45g ethanol, 45g water, under agitation react 5min in 70-80 ℃, with the 156g tetraethoxy in 60min, add the bottle in react 30min, then add 21.84g hexamethyldisiloxane and 2.52g tetramethyl divinyl disiloxane, reaction 30min moves into the separating funnel standing demix, takes out lower floor's mixed solution, to neutral, namely get vinyl MQ silicone resin in decompression and 130 ℃ of lower oven dry with deionized water wash.
The sample preparation is with example 1.
Specific embodiment 4:
In the 500mL there-necked flask, add the 12.48g hexamethyldisiloxane, 6.39g tetramethyl divinyl disiloxane, the 30g concentrated hydrochloric acid, 45g toluene, 45g water, under agitation react 3min in 70-80 ℃, with the 156g tetraethoxy in 60min, add the bottle in react 30min, then add 76.44g hexamethyldisiloxane and 8.82g tetramethyl divinyl disiloxane, reaction 30min moves into the separating funnel standing demix, takes out lower floor's mixed solution, to neutral, namely get vinyl MQ silicone resin in decompression and 130 ℃ of lower oven dry with deionized water wash.
The sample preparation is with example 1.
Specific embodiment 5
In the 500mL there-necked flask, add the 23.4g hexamethyldisiloxane, 7.7g tetramethyl divinyl disiloxane, the 30g concentrated hydrochloric acid, 15g toluene, 30g ethanol, 45g water, under agitation react 3min in 70-80 ℃, with the 156g tetraethoxy in 60min, add the bottle in react 30min, then add 16.38g hexamethyldisiloxane and 1.89g tetramethyl divinyl disiloxane, the reaction 30min, move into the separating funnel standing demix, take out lower floor's mixed solution, to neutral, namely get vinyl MQ silicone resin in decompression and 130 ℃ of lower oven dry with deionized water wash.
The sample preparation is with example 1.
Specific embodiment 6
In the 500mL there-necked flask, add the 34.3g hexamethyldisiloxane, 8.9g tetramethyl divinyl disiloxane, 30g concentrated hydrochloric acid, 30g toluene, 15g ethanol, 45g water under agitation reacts 3min in 70-80 ℃, 156g tetraethoxy and 20.96g dimethyldiethoxysilane is added in 60min in the bottle react 60min, move into the separating funnel standing demix, take out lower floor's mixed solution, to neutral, namely get according to vinyl MDQ silicone resin in decompression and 130 ℃ of lower oven dry with deionized water wash.
The sample preparation is with example 1.
Specific embodiment 7
The vinyl MQ silicone resin 7g that buys is dissolved with 10g toluene, the adding viscosity is 500mPa.s, contents of ethylene is in 1.2% the 100g vinyl silicone oil, remove solvent after stirring under reduced pressure, adding 140g median size is that aluminum oxide, the 60g median size of 15 μ m is the aluminium hydroxide of 23 μ m, 15.4g hydrogen content is 0.35% containing hydrogen silicone oil, 0.38g platinum catalyst, 0.01g inhibitor, deaeration 8 minutes under 0.1MPa after mixing, then inject in the mould of a 3mm * 160mm * 160mm, self-vulcanizing 24 hours, make film.
Specific embodiment 8
Be 500mPa.s at viscosity, contents of ethylene is in 1.2% the 100g vinyl silicone oil, and the aluminum oxide, the 60g median size that add the 140g median size and be 15 μ m are the aluminium hydroxide of 23 μ m, and the 3g specific surface area is 200m
2The thermal silica of/g, 15.4g hydrogen content are 0.35% containing hydrogen silicone oil, the 0.38g platinum catalyst, 0.01g inhibitor, then deaeration 8 minutes under 0.1MPa injects in the mould of a 3mm * 160mm * 160mm after mixing, self-vulcanizing 24 hours, make film.
Specific embodiment 9
Be 500mPa.s at viscosity, contents of ethylene is in 1.2% the 100g vinyl silicone oil, adding 140g median size is that aluminum oxide, the 60g median size of 15 μ m is the aluminium hydroxide of 23 μ m, 15.4g hydrogen content is 0.35% containing hydrogen silicone oil, 0.38g platinum catalyst, 0.01g inhibitor, deaeration 8 minutes under 0.1MPa after mixing, then inject in the mould of a 3mm * 160mm * 160mm, self-vulcanizing 24 hours, make film.
Above-described embodiment 1-6 participates in reactant and system medium vinyl content numbers illustrated such as following table:
| Project | A | B | C | D | E | F |
| Example 1 | 6/20 | 0.3 | 10％ | 10％ | 0 | 0 |
| Example 2 | 6/20 | 0.3 | 3％ | 3％ | 0 | 0.2 |
| Example 3 | 4/20 | 0.4 | 3％ | 3％ | 0 | 0 |
| Example 4 | 3/20 | 0.85 | 3％ | 3％ | 0 | 0 |
| Example 5 | 5/20 | 0.4 | 3％ | 3％ | 0 | 0 |
| Example 6 | 7/20 | 0.35 | 3％ | 3％ | 0.19 | 0 |
Annotate: the molar mass sum of A---added hexamethyldisiloxane of (1) step and tetramethyl divinyl siloxanes is the multiple of tetraethoxy molar weight
After B---(2) went on foot and finishes, the molar mass sum of added hexamethyldisiloxane and tetramethyl divinyl siloxanes was the multiple of tetraethoxy molar weight in the system
The system medium vinyl content that C---by formula calculated after (1) step
The system medium vinyl content that D---by formula calculated after (2) step
E---two functional silicone molar weights are the multiple of tetraethoxy molar weight
F---trifunctional siloxanes molar weight is the multiple of tetraethoxy molar weight
The diaphragm of above-mentioned 9 examples is carried out the performance analysis contrast, test result such as following table:
By above table as can be known, the organosilicon sizing material that the silicone resin that adopts the present invention to synthesize is made is better mechanical property not only, and viscosity is lower, and levelling property is better, is especially suitable for use as the reinforced filling of joint sealant.
Claims (8)
1. the preparation method of a vinyl silicon resin for reinforcing organic silicon pouring sealant is characterized in that specifically may further comprise the steps:
(1) add hexamethyldisiloxane and tetramethyl divinyl disiloxane in the mixture of concentrated hydrochloric acid, organic solvent and water, react in 70～80 ℃, the reaction times is 3～5min, and keeps homo(io)thermism;
(2) after finish (1), in 60min, add tetraethoxy and two senses or trifunctional siloxanes, reaction 30～60min;
(3) after finish (2), if the hexamethyldisiloxane that (1) step added and the molar weight sum of tetramethyl divinyl disiloxane are not more than 1/4 of tetraethoxy molar weight, then add hexamethyldisiloxane and tetramethyl divinyl siloxanes, reaction 30～60min; Otherwise, then do not need to add again hexamethyldisiloxane or tetramethyl divinyl disiloxane;
(4) with (3) mixture standing demix, take out lower floor's liquid, extremely neutral with deionized water wash;
(5) desolventize and low-boiling-point substance in decompression and 130 ℃ of lower oven dry, steamings, get final product to get vinyl polysiloxane.
2. preparation method according to claim 1 is characterized in that organic solvent described in the step (1) is one or more of toluene, ethanol, dimethylbenzene.
3. preparation method according to claim 1, it is characterized in that two functional silicones described in the step (2) are one or both combinations of dimethyldimethoxysil,ne, dimethyldiethoxysilane, its content minimum is 0, and maximum is no more than 0.19 of tetraethoxy molar mass.
4. preparation method according to claim 1, it is characterized in that trifunctional siloxanes described in the step (2) is one or both combinations of methyltrimethoxy silane, Union carbide A-162, its content minimum is 0, and maximum is no more than 0.2 of tetraethoxy molar mass.
5. preparation method according to claim 1, the molar mass sum that it is characterized in that the hexamethyldisiloxane that adds in the step (1) and tetramethyl divinyl siloxanes be in the system tetraethoxy molar mass 3/20～7/20; The massfraction (m (vinyl)/(m (hexamethyldisiloxane)+m (tetramethyl divinyl disiloxane)+m (tetraethoxy) * 0.28)) of system medium vinyl was 3%～10% after the amount of added tetramethyl divinyl siloxanes should satisfy step (1) and finishes in this step;
6. preparation method according to claim 1, the molar mass sum that it is characterized in that the hexamethyldisiloxane that adds in step (1) and the step (3) and tetramethyl divinyl siloxanes are no more than 0.85 of tetraethoxy molar mass in the system; Sum that tetramethyl divinyl disiloxane is measured should satisfy 3%～10% of system medium vinyl massfraction (m (vinyl)/(m (hexamethyldisiloxane)+m (tetramethyl divinyl disiloxane)+m (tetraethoxy) * 0.28)) in two steps;
7. preparation method according to claim 1 is characterized in that two functional silicones that step (2) adds, when the trifunctional content of siloxane is minimum value 0, and the preparation product is the vinyl MQ silicone resin; When step (2) added two functional silicones, the preparation product was vinyl MDQ silicone resin; When step (2) added the trifunctional siloxanes, the preparation product was vinyl MTQ silicone resin.
8. vinyl MQ, MDQ and MTQ silicone resin that is made by preparation method claimed in claim 1.
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| CN103102689B (en) * | 2011-11-15 | 2015-04-01 | 佛山市金戈消防材料有限公司 | Organic-silicon pouring sealant composition with high thermal conductivity and application thereof |
| CN102617860B (en) * | 2012-04-11 | 2013-09-04 | 成都拓利化工实业有限公司 | Preparation method for organic silicon resin |
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| CN102775612B (en) * | 2012-07-24 | 2014-08-27 | 东莞兆舜有机硅新材料科技有限公司 | Vinyl MQ silicon resin and preparation method thereof |
| CN102964983B (en) * | 2012-12-12 | 2015-01-07 | 广州市高士实业有限公司 | Silicon hybrid composite coating electronic adhesive and preparation method thereof |
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| CN103524741B (en) * | 2013-09-18 | 2015-09-02 | 烟台德邦先进硅材料有限公司 | A kind of Synthetic method of methyl vinyl MQ silicon resin |
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| CN110204900B (en) * | 2019-05-08 | 2021-09-03 | 广州慧谷化学有限公司 | Flame-retardant organopolysiloxane composition and preparation method thereof |
| CN110423351A (en) * | 2019-07-29 | 2019-11-08 | 中科广化（重庆）新材料研究院有限公司 | A kind of Vinyl MQ silicon resin and preparation method thereof |
| CN112063176A (en) * | 2020-09-10 | 2020-12-11 | 江苏天辰新材料股份有限公司 | Addition type encapsulating silicon rubber for encapsulating transformer and preparation method thereof |
| CN114381123A (en) * | 2022-01-24 | 2022-04-22 | 新纳奇材料科技江苏有限公司 | Preparation method of ceramic flame-retardant foamed silica gel material |
| CN114835951B (en) * | 2022-05-24 | 2024-06-04 | 广东金戈新材料股份有限公司 | MQ surface modified heat conducting powder and preparation method and application thereof |
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