CN104893295A - Additive for improving heat conduction of additional-type silicon rubber and preparation method thereof - Google Patents
Additive for improving heat conduction of additional-type silicon rubber and preparation method thereof Download PDFInfo
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- CN104893295A CN104893295A CN201510305059.6A CN201510305059A CN104893295A CN 104893295 A CN104893295 A CN 104893295A CN 201510305059 A CN201510305059 A CN 201510305059A CN 104893295 A CN104893295 A CN 104893295A
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Abstract
The invention discloses a preparation method of an additive for improving heat conduction of additional-type silicon rubber, comprising the following steps: adding a certain amount of aluminic acid ester in a reaction bottle, raising the temperature to 60-70 DEG C while stirring, dropwise adding water 1-3 times of mole amount of aluminic acid ester, reacting for 4-6h under the temperature of 60-70 DEG C, adding a vinyl silicane coupling agent 0.2-1.0 time of mole amount of aluminic acid ester in a reactant, adding organic acid under stirring, raising the temperature to 140-150 DEG C for reacting for 4-6h, cooling to 90-100 DEG C, and removing micromolecule impurities to obtain the additive. After the additive is added to the addition-type rubber, the heat conduction of the rubber is greatly improved and mechanical strength and other properties of the rubber are not influenced.
Description
Technical field
The application relates to a kind of addition-type silicon rubber additive, particularly relates to a kind of additive for improving addition-type silicon rubber thermal conductivity and preparation method thereof.
Background technology
Along with the develop rapidly of China's electronic industry, heat radiation (heat conduction) problem of electronic product becomes increasingly conspicuous, and also day by day improves the requirement of thermally conductive material.Because electronic product to have the requirement of insulation (non-conductive) to macromolecule heat conduction material, therefore macromolecule heat conduction material is in order to improve thermal conductivity, just can not add the very high metal powder of thermal conductivity, the lower inorganic materials powder of non-conductive thermal conductivity and metal oxide powder can only be added (such as: silicon carbide, silicon oxide, aluminium sesquioxide etc.).And the interpolation of these powders, high molecular physicals certainly will be reduced, as tensile strength, tearing strength, thus make macromolecule heat conduction material lose actual use value because of mechanical properties decrease.The interpolation of these powders simultaneously also can increase the viscosity of macromolecule heat conduction material, thus makes its viscosity excessive and cause macromolecule heat conduction material to lose flowability, and causes the difficulty of use.Namely the interpolation of these conduction powder can bring following shortcoming to addition-type silicon rubber: (1) reduces the physical strength of organo-silicone rubber; (2) increase the viscosity of organo-silicone rubber base-material, viscosity is too large before curing to make sizing material, thus causes sizing material to lose actual use properties.
Summary of the invention
The application provides a kind of additive for improving addition-type silicon rubber thermal conductivity and preparation method thereof, solves the problem that the interpolation conductive powder existed in prior art can cause addition-type silicon rubber physical strength to reduce.
A kind of method that can improve thermal conductivity and do not increase again macromolecule heat conduction material viscosity is provided to be exactly an aim of the present invention.Well-known: the transmission of (1) heat energy is mainly transmitted by hot load persons such as electronics, photon and phonons; (2) be best with the heat-transfer effect of electronics in these three kinds of heat energy load persons.This is also the reason of heat-transfer effect far above nonmetal (mainly conducting heat by phonon) of metallic substance.Based on this, if can metal group in grafting on the chain of organosilyl silica, so the heat-transfer effect of organo-silicone rubber should be improved.Select metal " aluminium " more applicable: one is that " aluminium " heat-conducting effect itself is also good, is better than other " metal " atoms being easy to the grafting of silica chain, as tin, titanium etc.; Two are the conductive powder of adding in heat-conducting silicon rubber is nothing but the materials such as aluminium sesquioxide, silicon nitride, silicon carbide, magnesium oxide, and be the most frequently used with aluminium sesquioxide, and on the chain of aluminium sesquioxide and silica, " metallic aluminium " group of grafting still has the effect interacting instead of mutually repel.By " metal " gene in grafting on the silica chain of its addition-type silicon rubber.Particularly in organo-silicone rubber, grafting " metallic aluminium " group, makes it to interact with the aluminium element added in conduction powder alchlor in silicon rubber, improves the heat-conducting effect of organo-silicone rubber, thus reaches the thermal conductivity improving organo-silicone rubber.
According to the first aspect of the application, this application provides a kind of preparation method of the additive for improving addition-type silicon rubber thermal conductivity, comprising the following steps:
(1) a certain amount of Aluminate is put into reaction flask, is warmed up to 60 DEG C ~ 70 DEG C under agitation, drip metering for the water of Aluminate 1.0 ~ 3.0 times of molar weights, after react 4 ~ 6 hours under the condition of 60 DEG C ~ 70 DEG C;
(2) in the reactant that (1) is obtained, add the vinyl silicane coupling agent of metering for Aluminate 0.2 ~ 1.0 times of molar weight after, add organic acid under agitation, be warmed up to 140 DEG C ~ 150 DEG C reactions 4 ~ 6 hours under agitation;
(3) cool to 90 DEG C-100 DEG C after, remove small molecular weight impurity, obtained additive.
According to the second aspect of the application, the application provides a kind of additive for improving addition-type silicon rubber thermal conductivity, and wherein additive is prepared by above-mentioned preparation method and obtains.
The beneficial effect of the application is: by being added with preparation method's preparation of the application and the additive that obtains toward addition-type silicon rubber, improve the thermal conductivity of addition-type silicon rubber material and do not affect its physical strength.
Embodiment
Below by embodiment, the present invention is described in further detail.
Additive prepared by the application due to silicon-oxygen backbone is grafted with aluminium base because of, can heat-conducting effect be improved; Main chain belt has the ethylene/propylene thiazolinyl group for addition reaction simultaneously, and ethylene/propylene thiazolinyl group can carry out addition reaction with addition-type silicon rubber, thus prepares reticulated structure silicon rubber.
The thermal conductivity that the application mentions is higher, and silicon rubber thermal conductivity is better.Thermal conductivity increase rate be addition-type silicon rubber before the addition of additives after thermal conductivity improve percentage.
A certain amount of Aluminate is put into reaction flask by the application.Be warmed up to 60 DEG C ~ 70 DEG C under agitation.Drip the water of metering for Aluminate 1 ~ 3 times of molar weight, dripped off in 40 minutes, react 4 ~ 6 hours under the condition of 60 DEG C ~ 70 DEG C afterwards.Add in above-mentioned reactant metering for Aluminate 0.2 ~ 1 times of molar weight vinyl silicane coupling agent, progressively add organic acid under agitation, be warmed up to 140 DEG C ~ 150 DEG C reactions 4 ~ 6 hours under agitation, cool to 90 DEG C ~ 100 DEG C afterwards, removed under reduced pressure small molecular weight impurity, the finally additive for improving addition-type silicon rubber thermal conductivity of obtained the application.
Wherein, Aluminate selects commercially available Aluminate, is aluminic acid three isopropyl ester or aluminic acid three isobutyl ester; Vinyl silicane coupling agent selects commercially available model to be the vinyl silicane coupling agent of A-151 or A-171; Organic acid, as catalyzer, is commercially available formic acid or acetic acid.
embodiment one:for improving a preparation method for the additive of addition-type silicon rubber thermal conductivity, comprise the following steps:
In 500ml there-necked flask, add 297 grams of (molar weight is 1.5 mol) aluminic acid three isobutyl esters, be warmed up to after 60 DEG C, drip 27 grams of (molar weight is 1.5 mol) water at agitation condition, dripped off in 40 minutes.And react 6 hours at 60 DEG C; 57 grams of (molar weight is 0.3 mol) vinyl silicane coupling agents are added in above-mentioned reactant, react 10 minutes after above-mentioned material adds, after add 4 grams of (0.06 mol) acetic acid again, under agitation be warmed up to 140 DEG C afterwards, react 6 hours with this understanding, cool to 90 DEG C, last removed under reduced pressure small molecular weight impurity, can obtain additive.
embodiment two:for improving a preparation method for the additive of addition-type silicon rubber thermal conductivity, comprise the following steps:
In 500ml there-necked flask, add 297 grams of (molar weight is 1.5 mol) aluminic acid three isobutyl esters, be warmed up to after 70 DEG C, drip 81 grams of (molar weight is 4.5 mol) water at agitation condition, dripped off in 40 minutes.And react 4 hours at 70 DEG C; 285 grams of (molar weight is 1.5mol) vinyl silicane coupling agents are added in above-mentioned reactant, react 15 minutes after above-mentioned material adds, after add 13.5 grams of (0.225mol) acetic acid again, under agitation be warmed up to 150 DEG C afterwards, react 4 hours with this understanding, cool to 100 DEG C, removed under reduced pressure small molecular weight impurity, can additive be obtained.
embodiment three:for improving a preparation method for the additive of addition-type silicon rubber thermal conductivity, comprise the following steps:
In 500ml there-necked flask, add 297 grams of (molar weight is 1.5 mol) aluminic acid three isobutyl esters, be warmed up to after 65 DEG C, drip 36 grams of (molar weight is 2 mol) water at agitation condition, dripped off in 40 minutes.And react 5 hours at 65 DEG C; 95 grams of (molar weight is 0.5 mol) vinyl silicane coupling agents are added in above-mentioned reactant, react 12 minutes after above-mentioned material adds, after add 5 grams of (0.08 mol) acetic acid again, under agitation be warmed up to 140 DEG C afterwards, react 5 hours with this understanding, cool to 95 DEG C, removed under reduced pressure small molecular weight impurity, can additive be obtained.
performance test: this test by DRL-
the thermal conductivity of sample tested by type heat flow method conductometer, omnipotent H & S material-testing machine surveys tensile strength, using the DC170 add-on type rubber of conventional Dow Corning Corporation as base glue, add additive prepared by embodiment 1-3, test result is as table 1; Using conventional domestic addition-type silicon rubber as base glue, add additive prepared by embodiment 1-3, test result is as table 2.
Table 1
Table 2
| Sample sequence number performance perameter | Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 | Sample 7 | Sample 8 | Sample 9 |
| Domestic molding silicone rubber (g) | 100 | 100 | 100 | 100 | 100 | 100 | 100 | 100 | 100 |
| Additive (g) prepared by embodiment 1 | 0 | 2 | 8 | 0 | 0 | 0 | 0 | 0 | 0 |
| Additive (g) prepared by embodiment 2 | 0 | 0 | 0 | 2 | 6 | 8 | 0 | 0 | 0 |
| Additive (g) prepared by embodiment 3 | 0 | 0 | 0 | 0 | 0 | 0 | 2 | 4 | 8 |
| Thermal conductivity (w/mk) | 0.5 | 0.58 | 0.66 | 0.62 | 0.64 | 0.66 | 0.60 | 0.62 | 0.66 |
| Thermal conductivity increase rate (%) | 0 | 16 | 32 | 21.5 | 22.5 | 32 | 20 | 21.5 | 32 |
| Tensile strength (MPa) | 2.5 | 2.5 | 2.5 | 2.51 | 2.5 | 2.5 | 2.5 | 2.51 | 2.5 |
Can take a fancy to from the test result of table 1 and table 2, the obtained additive of 2 ~ 8 parts of any one of embodiment 1-3 is added toward the DC170 add-on type rubber of the Dow Corning Corporations of 100 parts or domestic addition-type silicon rubber, thermal conductivity significantly improves 16%-37.5%, tensile strength is unchanged, and viscosity does not affect the further solidification processing of addition-type silicon rubber.
Above content is in conjunction with concrete embodiment further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made.
Claims (8)
1., for improving a preparation method for the additive of addition-type silicon rubber thermal conductivity, it is characterized in that: comprise the following steps:
(1) a certain amount of Aluminate is put into reaction flask, is warmed up to 60 DEG C ~ 70 DEG C under agitation, drip metering for the water of Aluminate 1.0 ~ 3.0 times of molar weights, after react 4 ~ 6 hours under the condition of 60 DEG C ~ 70 DEG C;
(2) in the reactant that (1) is obtained, add the vinyl silicane coupling agent of metering for Aluminate 0.2 ~ 1.0 times of molar weight after, add organic acid under agitation, be warmed up to 140 DEG C ~ 150 DEG C reactions 4 ~ 6 hours;
(3) cool to 90 DEG C ~ 100 DEG C, remove small molecular weight impurity, obtained additive.
2. preparation method according to claim 1, is characterized in that: described Aluminate is aluminic acid three isopropyl ester or aluminic acid three isobutyl ester.
3. preparation method according to claim 1, is characterized in that: described vinyl silicane coupling agent is
Vinyl silicane coupling agent A-151 or A-171.
4. preparation method according to claim 1, is characterized in that: described water time for adding is in 40 minutes.
5. preparation method according to claim 1, is characterized in that: described organic acid is formic acid or acetic acid.
6. preparation method according to claim 5, is characterized in that: described organic acid add-on is 1% ~ 3% of Aluminate, water and vinyl silicane coupling agent molar weight summation.
7. preparation method according to claim 1, is characterized in that: described small molecular weight impurity removes at reduced pressure conditions.
8. for improving an additive for addition-type silicon rubber thermal conductivity, it is characterized in that: described additive is the preparation method according to any one of claim 1-7 prepare and obtain.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051049A (en) * | 2009-10-29 | 2011-05-11 | 比亚迪股份有限公司 | Insulating and heat conducting silicon resin and preparation method thereof |
| CN103131381A (en) * | 2013-03-06 | 2013-06-05 | 广州市高士实业有限公司 | High-performance environmentally-friendly flame retardant type organic electron pouring sealant and preparation method thereof |
| CN103146340A (en) * | 2013-03-06 | 2013-06-12 | 广州市高士实业有限公司 | Low-viscosity high-heat-conductivity organic silicon electronic pouring sealant and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051049A (en) * | 2009-10-29 | 2011-05-11 | 比亚迪股份有限公司 | Insulating and heat conducting silicon resin and preparation method thereof |
| CN103131381A (en) * | 2013-03-06 | 2013-06-05 | 广州市高士实业有限公司 | High-performance environmentally-friendly flame retardant type organic electron pouring sealant and preparation method thereof |
| CN103146340A (en) * | 2013-03-06 | 2013-06-12 | 广州市高士实业有限公司 | Low-viscosity high-heat-conductivity organic silicon electronic pouring sealant and preparation method thereof |
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