CN1903972A - Production method of heat conductive silica gel - Google Patents
Production method of heat conductive silica gel Download PDFInfo
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- CN1903972A CN1903972A CN 200610052673 CN200610052673A CN1903972A CN 1903972 A CN1903972 A CN 1903972A CN 200610052673 CN200610052673 CN 200610052673 CN 200610052673 A CN200610052673 A CN 200610052673A CN 1903972 A CN1903972 A CN 1903972A
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Abstract
The present invention discloses a production method of heat conduction silica gel, belonging to the field of organic silicon chemical technology. Said method includes the following steps: (1), mixing polymethylsiloxane containing active group and multifunctional polymethylsiloxane according to the weight ratio of 6:4-8:2 at room temperature, uniformly stirring tem to obtain component A; (2), uniformly mixing 1-10% of catalyst, 1-5% of polyether, 50-70% of isopropanol, 20-40% of polydimethylsiloxane and 0.5%-1.5% of accelerating agent, refluxing for 4-6 h at 80 deg.C-90 deg.C so as to obtain component B; and (3), mixing component A and component B according to the weight ratio of 100:0.5-10 at room temperature, uniformly stirring them so as to obtain the invented product.
Description
Technical field
The invention discloses a kind of production method of heat conductive silica gel, belong to the organic silicon chemical technical field.
Background technology
The rectifier power supply is one of key equipment of surface treatment industries such as plating, aluminaization, and well-known the sector bad working environment is the important factor in puzzlement reliable production equipment, stability and life-span always, therefore to effective protection of the electron device of rectifier power supply cause close important.The professional rectifier equipment of surface treatment industry is equipped with a large amount of electron devices and PCB device, with materials such as traditional insullac such as alcohol acids impregnating varnish, polyester impregnating varnish or epoxies dripping impregnating varnishs as its protective coating.The equipment that this quasi-tradition technology is made, must give good ventilation, isolation and frequent maintenance in the production scene, even the periodic replacement device is the basis, guarantee the reliable running of equipment, and in the such rugged environment of Electroplating Production, such maintenance becomes and is the complicated daily trouble in workshop, one of factory's stably manufactured big hidden danger especially, and be exactly on good maintenance management basis, the power unit of surface treatment industry, great frequency of maintenance reaches 1 year more than 2 times.As seen there is very big defective in traditional insullac process for protecting in the power unit of surface treatment industry, be the major hidden danger of equipment dependability.
Summary of the invention
For overcoming the shortcoming that above-mentioned prior art exists, the invention provides a kind of production method of heat conductive silica gel, the heat conductive silica gel use properties of being produced by this method is strong, alternative traditional insullac.
For achieving the above object, the technical solution adopted in the present invention is: a kind of production method of heat conductive silica gel is: (1) is that 6: 4～8: 2 polymethyl siloxane that contains active group and multi-functional polymethyl siloxane at room temperature mixes, stirs with weight ratio, obtains component A; (2) weight percent is respectively 1～10%, 1～5%, 50～70%, 20～40% and 0.5%～1.5% catalyzer, polyethers, Virahol, polydimethylsiloxane and promotor uniform mixing, refluxed 4～6 hours down at 80 ℃～90 ℃, obtain B component; (3) be that 100: 0.5～10 component A and B component are at room temperature mixed, stirring gets final product with weight ratio.
Described active group is-OH-CH=CH
2, OEt, a kind of among the OMe.
Described polyfunctional group is-H ,-OH ,-CH=CH
2, a kind of among the OEt.
Described catalyzer is a kind of in organo-metallic oxide compound, metal organic acid salt, the platinum acid chloride solution.
Described organo-metallic oxide compound is Bu
2SnO, Ti (OBu)
4In a kind of; Metal organic acid salt is a kind of in di-n-octyl two lauric acid, dibutyl two lauric acid.
Described promotor is silane coupling agent, and silane coupling agent is a kind of in γ-methacryloxypropyl trimethoxy silane, γ-aminopropyl Union carbide A-162, γ-An Bingjisanyiyangjiguiwan, N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan.
The described polymethyl siloxane that contains active group is made by following steps: the siloxanes of dimethyl siloxane and band active group is dropped into reactor; stirring is warming up to 80 ℃～90 ℃; react and add dimethyl siloxane and the catalyzer that end group contains active group after 0.5～1.5 hour; under nitrogen protection, be warming up to 130 ℃～150 ℃; reacted 3～6 hours; being warming up to 170 ℃ again vacuumizes; keep more than 2 hours; remove the base polymer that low-boiling-point substance gets certain viscosity at last; the polymethyl siloxane that promptly contains active group; dimethyl siloxane wherein; the siloxanes of band active group and the weight percent of the dimethyl siloxane that end group contains active group are respectively 80～90%; 5～15% and 5～15%, the weight ratio of dimethyl siloxane and catalyzer is 100: 0.05～1.Described multi-functional polymethyl siloxane is made by following steps: weight percent is respectively 85～95% and 5～15% polyfunctional group siloxanes and dimethyl siloxane drops into reactor; stirring is warming up to 80 ℃～90 ℃; react and add catalyzer after 0.5～1.5 hour; under nitrogen protection, be warming up to 130 ℃～150 ℃; reacted 3～6 hours; being warming up to 150 ℃ again vacuumizes; keep more than 1 hour; remove the Synergist S-421 95 that low-boiling-point substance gets certain viscosity at last; be multi-functional polymethyl siloxane, wherein the weight ratio of dimethyl siloxane and catalyzer is 100: 0.05～1.Described catalyzer is made by following steps: weight percent is respectively 1～10% and 90～99% oxyhydroxide and siloxanes drops in the reactor; stirring is warming up to 80 ℃～120 ℃; react under nitrogen protection and got final product in 4～6 hours, described oxyhydroxide is a kind of in potassium hydroxide, sodium hydroxide, the ammonium hydroxide.
The heat conductive silica gel chemical reagent-resistant performance that the present invention produces is strong, excellent weather resistance and hard, use temperature height and environmental protection, alternative traditional insullac, the erosion of the anti-acid ﹠ alkali liquid body of the more effective realization of energy, gas, the short circuit that waterproof (condensed water), damp atmosphere cause destroys, have good heat conduction function, electric insulation function, full intensity and adhesion strength simultaneously, maintenance or reparation construction reach to convenient.According to user's rig-site utilization, generally can realize using 5 years continuously, non-maintaining.
Embodiment
The invention will be further described below by specific embodiment, but the present invention is not limited by following examples.
Table one. the weight ratio corresponding relation of each embodiment of component A
| The polymethyl siloxane that contains active group | Multi-functional polymethyl siloxane | |
| Embodiment 1 | 6 | 4 |
| Embodiment 2 | 6.5 | 4.3 |
| Embodiment 3 | 7 | 3 |
| Embodiment 4 | 7.5 | 1.9 |
| Embodiment 5 | 8 | 2 |
Table two. the weight percent corresponding relation of each embodiment of B component
| Catalyzer % | Polyethers % | Virahol % | Polydimethylsiloxane % | Promotor % | |
| Embodiment 1 | 6.2 | 3 | 50 | 40 | 0.8 |
| Embodiment 2 | 1 | 5 | 56.8 | 36 | 1.2 |
| Embodiment 3 | 7 | 2.5 | 60 | 30 | 0.5 |
| Embodiment 4 | 10 | 1 | 63 | 24.5 | 1.5 |
| Embodiment 5 | 5 | 4 | 70 | 20 | 1 |
Table three. the weight ratio corresponding relation of component A and each embodiment of B component
| Component A | B component | |
| Embodiment 1 | 100 | 0.5 |
| Embodiment 2 | 100 | 2.5 |
| Embodiment 3 | 100 | 4 |
| Embodiment 4 | 100 | 8 |
| Embodiment 5 | 100 | 10 |
Table four. produce the weight percent corresponding relation of each embodiment of the polymethyl siloxane that contains active group
| Dimethyl siloxane % | The siloxanes % of band active group | End group contains the dimethyl siloxane % of active group | |
| Embodiment 1 | 80 | 15 | 5 |
| Embodiment 2 | 80 | 5 | 15 |
| Embodiment 3 | 85 | 7.5 | 7.5 |
| Embodiment 4 | 82 | 10 | 8 |
| Embodiment 5 | 90 | 5 | 5 |
Table five. produce the weight ratio corresponding relation of dimethyl siloxane and each embodiment of catalyzer in the polymethyl siloxane contain active group
| Dimethyl siloxane | Catalyzer | |
| Embodiment 1 | 100 | 0.05 |
| Embodiment 2 | 100 | 0.25 |
| Embodiment 3 | 100 | 0.5 |
| Embodiment 4 | 100 | 0.8 |
| Embodiment 5 | 100 | 1 |
Table six. produce the weight percent corresponding relation of each embodiment of multi-functional polymethyl siloxane
| Polyfunctional group siloxanes % | Dimethyl siloxane % | |
| Embodiment 1 | 85 | 15 |
| Embodiment 2 | 88 | 12 |
| Embodiment 3 | 90 | 10 |
| Embodiment 4 | 93 | 7 |
| Embodiment 5 | 95 | 5 |
Table seven. produce the weight ratio corresponding relation of dimethyl siloxane and each embodiment of catalyzer in the multi-functional polymethyl siloxane
| Dimethyl siloxane | Catalyzer | |
| Embodiment 1 | 100 | 1 |
| Embodiment 2 | 100 | 0.8 |
| Embodiment 3 | 100 | 0.5 |
| Embodiment 4 | 100 | 0.25 |
| Embodiment 5 | 100 | 0.05 |
Table eight. produce the weight percent corresponding relation of each embodiment of catalyst system therefor in the process of the polymethyl siloxane contain active group and multi-functional polymethyl siloxane
| Oxyhydroxide % | Siloxanes % | |
| Embodiment 1 | 10 | 90 |
| Embodiment 2 | 8 | 92 |
| Embodiment 3 | 5 | 95 |
| Embodiment 4 | 3 | 97 |
| Embodiment 5 | 1 | 99 |
The production method of above each embodiment of heat conductive silica gel of the present invention is as follows:
Embodiment 1
1. will at room temperature mix, stir by the polymethyl siloxane that contains active group and the multi-functional polymethyl siloxane of certain weight ratio, obtain component A.
(1) polymethyl siloxane that contains active group is made by following steps: will drop into reactor by the dimethyl siloxane of certainweight per-cent and the siloxanes of band active group, stirring is warming up to 80 ℃, react the end group that adds certainweight per-cent after 1.5 hours again and contain the dimethyl siloxane and the catalyzer of active group, wherein catalyzer becomes certain weight ratio with dimethyl siloxane, under nitrogen protection, be warming up to 150 ℃, reacted 3 hours, being warming up to 170 ℃ again vacuumizes, keep more than 2 hours, remove the base polymer that low-boiling-point substance gets certain viscosity at last, promptly contain the polymethyl siloxane of active group; Above active group is-OH.
(2) multi-functional polymethyl siloxane is made by following steps: will drop into reactor by the polyfunctional group siloxanes and the dimethyl siloxane of certainweight per-cent, stirring is warming up to 80 ℃, react and add catalyzer after 1.5 hours, wherein catalyzer becomes certain weight ratio with dimethyl siloxane, under nitrogen protection, be warming up to 150 ℃, reacted 3 hours, being warming up to 150 ℃ again vacuumizes, keep more than 1 hour, remove the Synergist S-421 95 that low-boiling-point substance gets certain viscosity at last, promptly multi-functional polymethyl siloxane; Above polyfunctional group is-H.
(3) catalyzer is made by following steps: will drop in the reactor by the potassium hydroxide and the siloxanes of certainweight per-cent, stir and be warming up to 120 ℃, reaction got final product in 4 hours under nitrogen protection.
2. will be by the Bu of certainweight per-cent
2SnO, polyethers, Virahol, polydimethylsiloxane and γ-methacryloxypropyl trimethoxy silane uniform mixing refluxed 6 hours down at 80 ℃, obtained B component.
3. will at room temperature mix by the component A and the B component of certain weight ratio, stir get final product heat conductive silica gel.
Embodiment 2
1. will at room temperature mix, stir by the polymethyl siloxane that contains active group and the multi-functional polymethyl siloxane of certain weight ratio, obtain component A.
(1) polymethyl siloxane that contains active group is made by following steps: will drop into reactor by the dimethyl siloxane of certainweight per-cent and the siloxanes of band active group, stirring is warming up to 82 ℃, react the end group that adds certainweight per-cent after 1.2 hours again and contain the dimethyl siloxane and the catalyzer of active group, wherein catalyzer becomes certain weight ratio with dimethyl siloxane, under nitrogen protection, be warming up to 145 ℃, reacted 4 hours, being warming up to 170 ℃ again vacuumizes, keep more than 2 hours, remove the base polymer that low-boiling-point substance gets certain viscosity at last, promptly contain the polymethyl siloxane of active group; Above active group is-CH=CH
2
(2) multi-functional polymethyl siloxane is made by following steps: will drop into reactor by the polyfunctional group siloxanes and the dimethyl siloxane of certainweight per-cent, stirring is warming up to 82 ℃, react and add catalyzer after 1.2 hours, wherein catalyzer becomes certain weight ratio with dimethyl siloxane, under nitrogen protection, be warming up to 145 ℃, reacted 4 hours, being warming up to 150 ℃ again vacuumizes, keep more than 1 hour, remove the Synergist S-421 95 that low-boiling-point substance gets certain viscosity at last, promptly multi-functional polymethyl siloxane; Above polyfunctional group is-OH.
(3) catalyzer is made by following steps: will drop in the reactor by the potassium hydroxide and the siloxanes of certainweight per-cent, stir and be warming up to 110 ℃, reaction got final product in 4.5 hours under nitrogen protection.
2. will be by the Ti (OBu) of certainweight per-cent
4, polyethers, Virahol, polydimethylsiloxane and γ-aminopropyl Union carbide A-162 uniform mixing, refluxed 5.5 hours down at 82 ℃, obtain B component.
3. will at room temperature mix by the component A and the B component of certain weight ratio, stir get final product heat conductive silica gel.
Embodiment 3
1. will at room temperature mix, stir by the polymethyl siloxane that contains active group and the multi-functional polymethyl siloxane of certain weight ratio, obtain component A.
(1) polymethyl siloxane that contains active group is made by following steps: will drop into reactor by the dimethyl siloxane of certainweight per-cent and the siloxanes of band active group, stirring is warming up to 85 ℃, react the end group that adds certainweight per-cent after 1 hour again and contain the dimethyl siloxane and the catalyzer of active group, wherein catalyzer becomes certain weight ratio with dimethyl siloxane, under nitrogen protection, be warming up to 140 ℃, reacted 4.5 hours, being warming up to 170 ℃ again vacuumizes, keep more than 2 hours, remove the base polymer that low-boiling-point substance gets certain viscosity at last, promptly contain the polymethyl siloxane of active group; Above active group is OEt.
(2) multi-functional polymethyl siloxane is made by following steps: will drop into reactor by the polyfunctional group siloxanes and the dimethyl siloxane of certainweight per-cent, stirring is warming up to 85 ℃, react and add catalyzer after 1 hour, wherein catalyzer becomes certain weight ratio with dimethyl siloxane, under nitrogen protection, be warming up to 140 ℃, reacted 4.5 hours, being warming up to 150 ℃ again vacuumizes, keep more than 1 hour, remove the Synergist S-421 95 that low-boiling-point substance gets certain viscosity at last, promptly multi-functional polymethyl siloxane; Above polyfunctional group is-CH=CH
2
(3) catalyzer is made by following steps: will drop in the reactor by the sodium hydroxide and the siloxanes of certainweight per-cent, stir and be warming up to 100 ℃, reaction got final product in 5 hours under nitrogen protection.
2. will reflux 5 hours down at 85 ℃ by platinum acid chloride solution, polyethers, Virahol, polydimethylsiloxane and the γ-An Bingjisanyiyangjiguiwan uniform mixing of certainweight per-cent, obtain B component.
3. will at room temperature mix by the component A and the B component of certain weight ratio, stir get final product heat conductive silica gel.
Embodiment 4
1. will at room temperature mix, stir by the polymethyl siloxane that contains active group and the multi-functional polymethyl siloxane of certain weight ratio, obtain component A.
(1) polymethyl siloxane that contains active group is made by following steps: will drop into reactor by the dimethyl siloxane of certainweight per-cent and the siloxanes of band active group, stirring is warming up to 88 ℃, react the end group that adds certainweight per-cent after 0.8 hour again and contain the dimethyl siloxane and the catalyzer of active group, wherein catalyzer becomes certain weight ratio with dimethyl siloxane, under nitrogen protection, be warming up to 135 ℃, reacted 5 hours, being warming up to 170 ℃ again vacuumizes, keep more than 2 hours, remove the base polymer that low-boiling-point substance gets certain viscosity at last, promptly contain the polymethyl siloxane of active group; Above active group is OMe.
(2) multi-functional polymethyl siloxane is made by following steps: will drop into reactor by the polyfunctional group siloxanes and the dimethyl siloxane of certainweight per-cent, stirring is warming up to 88 ℃, react and add catalyzer after 0.8 hour, wherein catalyzer becomes certain weight ratio with dimethyl siloxane, under nitrogen protection, be warming up to 135 ℃, reacted 5 hours, being warming up to 150 ℃ again vacuumizes, keep more than 1 hour, remove the Synergist S-421 95 that low-boiling-point substance gets certain viscosity at last, promptly multi-functional polymethyl siloxane; Above polyfunctional group is OEt.
(3) catalyzer is made by following steps: will drop in the reactor by the ammonium hydroxide and the siloxanes of certainweight per-cent, stir and be warming up to 90 ℃, reaction got final product in 5.5 hours under nitrogen protection.
2. will reflux 4.5 hours down at 88 ℃ by di-n-octyl two lauric acid, polyethers, Virahol, polydimethylsiloxane and N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan uniform mixing of certainweight per-cent, obtain B component.
3. will at room temperature mix by the component A and the B component of certain weight ratio, stir get final product heat conductive silica gel.
Embodiment 5
1. will at room temperature mix, stir by the polymethyl siloxane that contains active group and the multi-functional polymethyl siloxane of certain weight ratio, obtain component A.
(1) polymethyl siloxane that contains active group is made by following steps: will drop into reactor by the dimethyl siloxane of certainweight per-cent and the siloxanes of band active group, stirring is warming up to 90 ℃, react the end group that adds certainweight per-cent after 0.5 hour again and contain the dimethyl siloxane and the catalyzer of active group, wherein catalyzer becomes certain weight ratio with dimethyl siloxane, under nitrogen protection, be warming up to 130 ℃, reacted 6 hours, being warming up to 170 ℃ again vacuumizes, keep more than 2 hours, remove the base polymer that low-boiling-point substance gets certain viscosity at last, promptly contain the polymethyl siloxane of active group; Above active group is-CH=CH
2
(2) multi-functional polymethyl siloxane is made by following steps: will drop into reactor by the polyfunctional group siloxanes and the dimethyl siloxane of certainweight per-cent, stirring is warming up to 90 ℃, react and add catalyzer after 0.5 hour, wherein catalyzer becomes certain weight ratio with dimethyl siloxane, under nitrogen protection, be warming up to 130 ℃, reacted 6 hours, being warming up to 150 ℃ again vacuumizes, keep more than 1 hour, remove the Synergist S-421 95 that low-boiling-point substance gets certain viscosity at last, promptly multi-functional polymethyl siloxane; Above polyfunctional group is-CH=CH
2
(3) catalyzer is made by following steps: will drop in the reactor by the sodium hydroxide and the siloxanes of certainweight per-cent, stir and be warming up to 80 ℃, reaction got final product in 6 hours under nitrogen protection.
2. will reflux 4 hours down at 90 ℃ by dibutyl two lauric acid, polyethers, Virahol, polydimethylsiloxane and N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan uniform mixing of certainweight per-cent, obtain B component.
3. will at room temperature mix by the component A and the B component of certain weight ratio, stir get final product heat conductive silica gel.
The construction technology of the heat conductive silica gel that the present invention produced is as follows:
1. component A and B component are at room temperature mixed (in weight ratio is 100: 0.5～10 scope) by required proportioning, stir, can apply or flood construction.
2. condition of cure: room temperature
3. set time: do on the surface needs 30～60 minutes, and completely solidified needs 24 hours.
4. security: component A and B component are no-solvent type, and be nonflammable, nontoxic.
5. store: component A and B component can be packed with iron or plastic tank respectively, and effective storage period is 3 years under the room temperature; After component A and B component mixing, be 1～4 hour duration of service, presses the actual needs allotment.
Characteristic before the film forming of the heat conductive silica gel that the present invention produced:
Color water white transparency or translucent
Component A, B two-pack
Main component contains the organosilicon polysiloxane of multifunctional active group
Viscosity (25 ℃) 200cPs～1000cPs
Solids content 100%
Characteristic after the film forming:
Film forming thickness 0.2～1.0mm (pressing the actual needs adjustment)
Hardness (Shao Shi A) 30～40
Proportion 1.05～1.10
Intensity 1.5～3.0MPa
Elongation at break 〉=100%
Volume specific resistance＞1 * 10
13～15Ω .cm
Dielectric strength＞20KV/mm
Anti-electric arc 100～300 seconds
Thermal conductivity＞2W/M.K
Rate of perviousness 0.04 * 10
-8～0.10 * 10
-8%
The performance synopsis of the heat conductive silica gel that the present invention produced and traditional insullac:
| Preventive means | Tradition insullac | Heat conductive silica gel |
| Antiacid alkali ability | Generally | By force |
| Electric insulation | By force | By force |
| Anti-electric arc | 90 seconds | 140 seconds |
| Use temperature | F level (＜150 ℃) | H level (＜180 ℃ of life-time service) |
| Hydrophobic nature | Generally (water-intake rate 0.07%) | Excellent (water-intake rate＜0.05%) |
| Weathering resistance | Difference (keeping 60% in 250 hours) | Excellent (keeping 80% in 2000 hours) |
| Cementability and intensity | Excellent | Excellent |
| Solvent | Need solvent (as toluene) | Environment-friendly solvent-free |
| Severe environment following work-ing life | 2 years, need regular maintenance | 5 years, non-maintaining |
The heat conductive silica gel coating chemical reagent-resistant performance table that the present invention produced:
| Chemical reagent | Resistivity | Chemical reagent | Resistivity | Chemical reagent | Resistivity |
| Acetic acid | Excellent | Sodium hydroxide (10%) | Excellent | Sulfurous gas | Very |
| Hydrochloric acid (36%) | Very | Sodium hydroxide (50%) | Excellent | Hydrogen peroxide | Excellent |
| Nitric acid (10%) | Very | Yellow soda ash | Excellent | Ethanol | Excellent |
| Sulfuric acid (30%) | Very | Salt solution (26%) | Excellent | Mineral oil | Excellent |
| Phosphoric acid (dense) | Very | Hydrogenchloride | Very | Water | Excellent |
| Stearic acid | Excellent |
The characteristics of the heat conductive silica gel that the present invention produced:
Weather-proof, anti-electric arc, heat-resisting, waterproof, acid and alkali-resistance chemical property are outstanding;
Tackiness is strong, surface luster;
Shock-resistance, vibration resistance are outstanding;
To non-corrosivenesss such as copper.
The heat conductive silica gel purposes that the present invention produced:
The moisture protection that can be used for electrical equipment, communication Instrument, washing machine, electronic scale etc.;
The insulating protection coating that also can be used for electron devices such as PCB, coil, interconnecting devices.
Claims (10)
1. the production method of a heat conductive silica gel, (1) are that 6: 4～8: 2 polymethyl siloxane that contains active group and multi-functional polymethyl siloxane at room temperature mixes, stirs with weight ratio, obtain component A; (2) weight percent is respectively 1～10%, 1～5%, 50～70%, 20～40% and 0.5%～1.5% catalyzer, polyethers, Virahol, polydimethylsiloxane and promotor uniform mixing, refluxed 4～6 hours down at 80 ℃～90 ℃, obtain B component; (3) be that 100: 0.5～10 component A and B component are at room temperature mixed, stirring gets final product with weight ratio.
2. according to the production method of the described heat conductive silica gel of claim 1, it is characterized in that described active group is-OH-CH=CH
2, OEt, a kind of among the OMe.
3. according to the production method of the described heat conductive silica gel of claim 1, it is characterized in that described polyfunctional group be-H ,-OH ,-CH=CH
2, a kind of among the OEt.
4. according to the production method of the described heat conductive silica gel of claim 1; it is characterized in that the described polymethyl siloxane that contains active group is made by following steps: the siloxanes of dimethyl siloxane and band active group is dropped into reactor; stirring is warming up to 80 ℃～90 ℃; react and add dimethyl siloxane and the catalyzer that end group contains active group after 0.5～1.5 hour; under nitrogen protection, be warming up to 130 ℃～150 ℃; reacted 3～6 hours; being warming up to 170 ℃ again vacuumizes; keep more than 2 hours; remove the base polymer that low-boiling-point substance gets certain viscosity at last; the polymethyl siloxane that promptly contains active group; dimethyl siloxane wherein; the siloxanes of band active group and the weight percent of the dimethyl siloxane that end group contains active group are respectively 80～90%; 5～15% and 5～15%, the weight ratio of dimethyl siloxane and catalyzer is 100: 0.05～1.
5. according to the production method of the described heat conductive silica gel of claim 1; it is characterized in that described multi-functional polymethyl siloxane is made by following steps: weight percent is respectively 85～95% and 5～15% polyfunctional group siloxanes and dimethyl siloxane drops into reactor; stirring is warming up to 80 ℃～90 ℃; react and add catalyzer after 0.5～1.5 hour; under nitrogen protection, be warming up to 130 ℃～150 ℃; reacted 3～6 hours; being warming up to 150 ℃ again vacuumizes; keep more than 1 hour; remove the Synergist S-421 95 that low-boiling-point substance gets certain viscosity at last; be multi-functional polymethyl siloxane, wherein the weight ratio of dimethyl siloxane and catalyzer is 100: 0.05～1.
6. according to the production method of claim 4 or 5 described heat conductive silica gels; it is characterized in that described catalyzer is made by following steps: weight percent is respectively 1～10% and 90～99% oxyhydroxide and siloxanes drops in the reactor; stirring is warming up to 80 ℃～120 ℃; react under nitrogen protection and got final product in 4～6 hours, described oxyhydroxide is a kind of in potassium hydroxide, sodium hydroxide, the ammonium hydroxide.
7. according to the production method of the described heat conductive silica gel of claim 1, it is characterized in that described catalyzer is a kind of in organo-metallic oxide compound, metal organic acid salt, the platinum acid chloride solution.
8. according to the production method of the described heat conductive silica gel of claim 7, it is characterized in that described organo-metallic oxide compound is Bu
2SnO, Ti (OBu)
4In a kind of; Metal organic acid salt is a kind of in di-n-octyl two lauric acid, dibutyl two lauric acid.
9. according to the production method of the described heat conductive silica gel of claim 1, it is characterized in that described promotor is silane coupling agent.
10. according to the production method of the described heat conductive silica gel of claim 9, it is characterized in that described silane coupling agent is a kind of in γ-methacryloxypropyl trimethoxy silane, γ-aminopropyl Union carbide A-162, γ-An Bingjisanyiyangjiguiwan, N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan.
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|---|---|---|---|---|
| CN101781550B (en) * | 2009-06-30 | 2012-10-17 | 深圳市八发汽车用品有限公司 | Making method of heat and electric conducting silica gel and heat generating device of silica obtained by applying the same |
| CN103275492A (en) * | 2013-06-28 | 2013-09-04 | 惠州市粤泰翔科技有限公司 | Heat-conducting silica gel accelerating heat conduction of electrons and electric appliances, and preparation method of heat-conducting silica gel |
| CN113674992A (en) * | 2021-08-30 | 2021-11-19 | 西安微电子技术研究所 | Process method for impregnating wound part by using heat-conducting sizing material |
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