CN115894927A - Thermal insulation material of foaming organic silicon gel and preparation method - Google Patents
Thermal insulation material of foaming organic silicon gel and preparation method Download PDFInfo
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- CN115894927A CN115894927A CN202211562727.XA CN202211562727A CN115894927A CN 115894927 A CN115894927 A CN 115894927A CN 202211562727 A CN202211562727 A CN 202211562727A CN 115894927 A CN115894927 A CN 115894927A
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- 238000005187 foaming Methods 0.000 title claims abstract description 29
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 29
- 239000010703 silicon Substances 0.000 title claims abstract description 29
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000012774 insulation material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 238000001879 gelation Methods 0.000 title description 2
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 31
- 239000003054 catalyst Substances 0.000 claims abstract description 25
- 239000011810 insulating material Substances 0.000 claims abstract description 21
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000004088 foaming agent Substances 0.000 claims abstract description 15
- 239000003112 inhibitor Substances 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001257 hydrogen Substances 0.000 claims abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 12
- 239000011159 matrix material Substances 0.000 claims description 11
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical group N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 9
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 8
- 229920002554 vinyl polymer Polymers 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 7
- 239000004604 Blowing Agent Substances 0.000 claims description 5
- 239000003085 diluting agent Substances 0.000 claims description 4
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 3
- 239000004156 Azodicarbonamide Substances 0.000 claims description 3
- XOZUGNYVDXMRKW-AATRIKPKSA-N azodicarbonamide Chemical compound NC(=O)\N=N\C(N)=O XOZUGNYVDXMRKW-AATRIKPKSA-N 0.000 claims description 3
- 235000019399 azodicarbonamide Nutrition 0.000 claims description 3
- CEBKHWWANWSNTI-UHFFFAOYSA-N 2-methylbut-3-yn-2-ol Chemical compound CC(C)(O)C#C CEBKHWWANWSNTI-UHFFFAOYSA-N 0.000 claims description 2
- INASARODRJUTTN-UHFFFAOYSA-N 3-methyldodec-1-yn-3-ol Chemical compound CCCCCCCCCC(C)(O)C#C INASARODRJUTTN-UHFFFAOYSA-N 0.000 claims description 2
- TVMKDEBREPFNDL-UHFFFAOYSA-N C(=C)[SiH]1O[SiH](O[SiH](O[SiH](O1)C=C)C=C)C=C.[Pt] Chemical compound C(=C)[SiH]1O[SiH](O[SiH](O[SiH](O1)C=C)C=C)C=C.[Pt] TVMKDEBREPFNDL-UHFFFAOYSA-N 0.000 claims description 2
- VJRITMATACIYAF-UHFFFAOYSA-N benzenesulfonohydrazide Chemical compound NNS(=O)(=O)C1=CC=CC=C1 VJRITMATACIYAF-UHFFFAOYSA-N 0.000 claims description 2
- DSVRVHYFPPQFTI-UHFFFAOYSA-N bis(ethenyl)-methyl-trimethylsilyloxysilane;platinum Chemical compound [Pt].C[Si](C)(C)O[Si](C)(C=C)C=C DSVRVHYFPPQFTI-UHFFFAOYSA-N 0.000 claims description 2
- ZPOLOEWJWXZUSP-WAYWQWQTSA-N bis(prop-2-enyl) (z)-but-2-enedioate Chemical compound C=CCOC(=O)\C=C/C(=O)OCC=C ZPOLOEWJWXZUSP-WAYWQWQTSA-N 0.000 claims description 2
- JUWSSMXCCAMYGX-UHFFFAOYSA-N gold platinum Chemical compound [Pt].[Au] JUWSSMXCCAMYGX-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 23
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- -1 vinyl methyl Chemical group 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 239000000499 gel Substances 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 25
- 238000002485 combustion reaction Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000013021 overheating Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- NBOCQTNZUPTTEI-UHFFFAOYSA-N 4-[4-(hydrazinesulfonyl)phenoxy]benzenesulfonohydrazide Chemical compound C1=CC(S(=O)(=O)NN)=CC=C1OC1=CC=C(S(=O)(=O)NN)C=C1 NBOCQTNZUPTTEI-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011825 aerospace material Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920002627 poly(phosphazenes) Polymers 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 239000012812 sealant material Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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- Silicon Polymers (AREA)
Abstract
The invention discloses a foaming organic silicon gel heat-insulating material and a preparation method thereof. The disclosed heat insulation material is composed of the following raw materials in parts by weight: 50 parts of hydrogen-containing silicon bonded methyl organic silicon; 50 parts of vinyl methyl silicone; 1-10 parts of azo foaming agent; the catalyst is not more than 1 part; the inhibitor is not more than 0.2 part. The low-heat-conduction low-density foaming organic silicon gel heat-insulating material with certain mechanical strength is prepared by a process method of pre-curing and then heating for foaming. The cell structure, density and thermal conductivity of the foaming material can be regulated and controlled by matching with the content of the foaming agent, the content of the catalyst and the precuring condition. The density and thermal conductivity of the foamed silicone gel material is significantly reduced compared to an unfoamed silicone gel.
Description
Technical Field
The invention belongs to the technical field of heat-insulating aerospace materials, and particularly relates to a heat-insulating material of foaming organic silicon gel and a preparation method thereof.
Background
The temperature of the combustion chamber of the rocket engine is high in the working process, the temperature of the combustion chamber can reach more than 2000K no matter the rocket engine is a solid rocket engine, a liquid rocket engine or a ramjet engine, the shell temperature of the combustion chamber can be effectively reduced to avoid the failure of the shell due to overheating through the modes of applying heat insulating materials on the inner wall of the combustion chamber and actively cooling, but necessary heat insulation needs to be carried out on electronic elements near the combustion chamber, so that the failure of the electronic elements due to overheating is avoided. With the development of advanced power technology, the temperature of the combustion chamber is higher and higher, the thermal service time is longer and longer, and higher requirements are provided for the heat insulation performance of a heat insulation material for the thermal protection of electronic components.
The pouring sealant material is a common electronic component packaging and heat insulating material, has the characteristics of good thermal stability, simple forming process and good environmental adaptability, can effectively reduce the heat conductivity of the material by introducing the air hole structure into the pouring sealant through the foaming process, and is a direction for developing a rapid potential of high-performance heat insulating materials. In the prior art, air components are introduced into the material mainly by regulating and controlling process bubbles generated in the curing process of the organic silicon gel and adding hollow microspheres, so that the function of reducing heat conduction is achieved.
Disclosure of Invention
Aiming at the defects or shortcomings of the prior art, the invention provides a foaming organic silicon gel heat insulation material.
Therefore, the foaming silicone gel heat-insulating material provided by the invention comprises the following raw materials in parts by mass: 50 parts of hydrogen-containing silicon-bonded methyl organosilicon, 50 parts of vinyl-containing methyl organosilicon, 1-10 parts of azo foaming agent, not more than 1 part of catalyst and not more than 0.2 part of inhibitor;
the hydrogen-silicon bond-containing methyl organosilicon is selected from GN-512 or GN-521;
the vinyl-containing methyl silicone is selected from GN-512 or GN-521;
the inhibitor is selected from one or the combination of more than two of ethynyl cyclohexanol, diallyl maleate, 2-methyl-3-butyn-2-ol and 3-methyl-1-dodecyn-3-ol;
the catalyst is selected from a Kanst catalyst or an Ashby catalyst.
Optionally, the azo blowing agent is selected from Azobisisobutyronitrile (AIBN), azodicarbonamide (AC), or 4,4' -Oxybis Benzenesulfonylhydrazide (OBSH).
Optionally, the kast catalyst is selected from a platinum gold catalyst or a platinum-divinyltetramethyldisiloxane complex diluent. The Ashby catalyst platinum-2,4,6,8-tetravinyl cyclotetrasiloxane complex diluent.
The invention also provides a preparation method of the heat insulation material. The preparation method comprises the following steps:
mixing hydrogen-silicon-bond-containing methyl organic silicon, vinyl-containing methyl organic silicon, an azo foaming agent, a catalyst and an inhibitor according to the formula amount to obtain a mixture;
and after the mixture is subjected to defoaming treatment, preheating the mixture at the temperature of not higher than 100 ℃, and curing the mixture at the temperature of more than 110 ℃ to prepare the foamed organic silicon gel heat-insulating material.
Further, the preparation method comprises the following steps: mixing hydrogen-containing silicon bond methyl organic silicon and azo foaming agent according to the formula amount to obtain a first matrix; mixing the vinyl methyl-containing organosilicon with the inhibitor according to the formula amount to obtain a second matrix; and mixing the first substrate and the second substrate, adding a catalyst, and uniformly mixing to obtain a mixture.
According to the invention, the foaming multiplying power is regulated and controlled by selecting the content of the foaming agent, the preheating temperature, the preheating time, the curing temperature and the curing time, so that the adjustment of the cell structure of the foamed organic silicon gel heat-insulating material is realized.
The lightweight organic silicon gel heat insulation material is prepared by a foaming process, and the density and the heat conductivity of the organic silicon gel are reduced by introducing low-density gas and increasing the section heat resistance, so that the negative quality of the heat insulation material is reduced and the heat insulation performance is improved. The density and thermal conductivity of the foamed silicone gel material is significantly reduced compared to an unfoamed silicone gel.
Drawings
FIG. 1 is a macro topography of a material prepared in example 1 of the present invention;
FIG. 2 is a microscopic morphology of the material prepared in example 1 of the present invention;
FIG. 3 is a comparison of the effects of example 1 of the present invention and comparative examples 1 to 4.
Detailed Description
Unless otherwise defined, scientific and technical terms used herein are to be understood as commonly understood by one of ordinary skill in the relevant art.
It should be noted that, in the preparation method of the present invention, defoaming treatment is required to eliminate process bubbles generated in the mixing process of the silicone gel. In the method, the strength of the silica gel melt can be adjusted by controlling the preheating temperature and time, so that the foaming ratio of the colloid is controlled. The preheating time length needs to ensure that the whole mixture after defoaming reaches the corresponding temperature, and the preheating time length is determined by combining the thermal environment and the amount of the base glue in the specific scheme; it should be noted that a preheating time that is too long may result in too high a degree of cure to allow foaming.
In addition, the foaming ratio of the silicone gel foaming material in a free state is limited, and the cell diameter and the density of the foaming material can be regulated and controlled by changing the content of the foaming agent.
It is also worth noting that azo blowing agents and the gases generated by their pyrolysis poison the silicone gel and do not cure, thus requiring the addition of a catalyst, which generally increases as the blowing agent content increases.
In particular, the materials of the silicone gel heat insulating material of the present invention should be prevented from being heated and cured in advance due to an excessively high stirring rate during the mixing process.
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Example 1:
the foamed silicone gel heat insulation material of the embodiment is composed of the following raw materials in parts by weight:
50 parts of hydrogen-containing silicon-bonded methyl organic silicon, 50 parts of vinyl-containing methyl organic silicon, 4 parts of azodiisobutyronitrile foaming agent, 0.5 part of catalyst and 0.05 part of inhibitor;
the preparation method of the polyphosphazene system-based heat insulating material comprises the following steps:
s1, stirring 50 parts by mass of hydrogen-containing silicon bond methyl organic silicon and 4 parts by mass of azodiisobutyronitrile foaming agent until the materials are uniformly mixed to obtain a first matrix;
s2, stirring 50 parts of vinyl methyl organic silicon and 0.05 part of ethynyl cyclohexanol inhibitor until the components are uniformly mixed to obtain a second matrix;
s3, mixing the first substrate and the second substrate, adding 0.5 part of platinum catalyst, and stirring until the mixture is uniformly mixed to obtain a third substrate;
s4, defoaming the third matrix by using a centrifuge at the rotation speed of 1000r/min for 1.5min to obtain a fourth matrix;
s5, placing the fourth matrix in an oven for preheating, wherein the temperature of the oven is 100 ℃, and the preheating time is 1min, so as to obtain a fifth matrix;
s6, curing the fifth matrix at the oven temperature of 120 ℃ for 10min to obtain the completely foamed organic silicon gel heat-insulating material.
In particular, during the mixing of the foamed silicone gel material, excessive stirring speed and time should be avoided, which leads to the material heating and curing.
Comparative example 1:
this comparative example differs from example 1 in that: no blowing agent was added.
Comparative example 2:
this comparative example differs from example 1 in that: step S4 is not performed.
Comparative example 3:
this comparative example differs from example 1 in that: 2 parts of azodiisobutyronitrile foaming agent and 0.5 part of catalyst.
Comparative example 4:
this comparative example differs from example 1 in that: the preheating time is 4min.
Comparative example 5:
this comparative example differs from example 1 in that: the curing is directly carried out, preheating is not carried out, the curing time is the total time of the preheating and the curing of the embodiment 1, and the obtained product cannot form a foaming material.
Comparative example 6:
this comparative example differs from example 1 in that: no inhibitor was added; the foamed structure is not formed inside the obtained product.
Comparative example 7:
this comparative example differs from example 1 in that: no catalyst is added; the foamed structure is not formed inside the obtained product.
Further, the thermal conductivity and the foaming ratio of the materials obtained in the above example 1 and comparative examples 1 to 4 were measured, and specifically, the thermal conductivity was measured according to ISO 22007-2 using a Hotdisk 2500S thermal conductivity meter; the foaming ratio is calculated by dividing the thickness of the foaming material by the thickness of the non-foaming material, wherein the non-foaming material specifically refers to the material prepared in comparative example 1, and the test results are shown in the following table 1:
TABLE 1
Thermal conductivity W/m.K | Density g/cm 3 | Expansion ratio | |
Comparative example 1 | 0.1806 | 0.9436 | 1 |
Comparative example 2 | 0.1632 | 0.8846 | 1.07 |
Comparative example 3 | 0.1464 | 0.6154 | 1.533 |
Comparative example 4 | 0.1531 | 0.6434 | 1.467 |
Example 1 | 0.1365 | 0.5898 | 1.6 |
As can be seen from Table 1, the thermal conductivity of the foamed silicone gel thermal insulation material of the present invention is decreased by 24.4% and the density is decreased by 37.5% compared to the non-foamed silicone gel thermal insulation material prepared in comparative example 1;
compared with the organosilicon gel heat-insulating material with the process cells in the comparative example 2, the heat conductivity of the foaming organosilicon gel heat-insulating material is respectively reduced by 16.4 percent, the density is reduced by 33.3 percent, and the effect is obvious.
It is thus understood that the foamed silicone gel heat insulating material of the present invention has a higher heat insulating performance than the unfoamed silicone gel heat insulating material and the silicone gel heat insulating material having process bubbles.
As can be seen from table 1, the foamed silicone gel foamed materials with different foaming ratios can be obtained by adjusting the content of the foaming agent and the pre-curing time, and the thermal conductivity of the materials can be adjusted by controlling the foaming ratio: the higher the foaming ratio, the lower the thermal conductivity;
compared with comparative example 4, the thermal conductivity of the material prepared in example 1 is reduced by 10.8%; the higher the expansion ratio, the lower the thermal conductivity, and the thermal conductivity of the material prepared in example 1 was reduced by 6.8% as compared with that of comparative example 3.
It is understood from this that the silicone gel heat insulating material of the embodiment of the present application has a higher heat insulating performance than silicone gel heat insulating materials of other expansion ratios.
The preferred embodiments of the present disclosure are described in detail with reference to the accompanying drawings, however, the present disclosure is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present disclosure within the technical idea of the present disclosure, and these simple modifications all belong to the protection scope of the present disclosure.
It should be noted that, in the above embodiments, the various features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations will not be further described in the present disclosure.
In addition, any combination of various embodiments of the present disclosure may be made, and the same should be considered as the disclosure of the present disclosure, as long as it does not depart from the spirit of the present disclosure.
Claims (7)
1. The foaming organic silicon gel heat insulation material is characterized by comprising the following raw materials in parts by mass:
50 parts of hydrogen-containing silicon-bonded methyl organosilicon, 50 parts of vinyl-containing methyl organosilicon, 1-10 parts of azo foaming agent, not more than 1 part of catalyst and not more than 0.2 part of inhibitor;
the hydrogen-silicon bond-containing methyl organosilicon is selected from GN-512 or GN-521;
the vinyl-containing methyl silicone is selected from GN-512 or GN-521;
the inhibitor is one or the combination of more than two of ethynylcyclohexanol, diallyl maleate, 2-methyl-3-butyn-2-ol and 3-methyl-1-dodecyn-3-ol;
the catalyst is selected from a Kaster catalyst or an Ashby catalyst.
2. The foamed silicone gel thermal insulation material of claim 1, wherein the azo-based blowing agent is selected from azobisisobutyronitrile, azodicarbonamide, or 4,4' -oxybis benzenesulfonylhydrazide.
3. The foamed silicone gel insulation material of claim 1, wherein the kast catalyst is selected from a platinum gold catalyst or a platinum-divinyltetramethyldisiloxane complex diluent.
4. The foamed silicone gel insulation material of claim 1, wherein the Ashby catalyst platinum-2,4,6,8-tetravinylcyclotetrasiloxane complex diluent.
5. The method of manufacturing the foamed silicone gel thermal insulating material according to any one of claims 1 to 4, characterized in that the manufacturing method comprises:
mixing hydrogen-containing silicon-bonded methyl organic silicon, vinyl-containing methyl organic silicon, an azo foaming agent, a catalyst and an inhibitor according to the formula ratio to obtain a mixture;
and after the mixture is subjected to defoaming treatment, preheating the mixture at the temperature of not higher than 100 ℃, and curing the mixture at the temperature of more than 110 ℃ to prepare the foamed organic silicon gel heat-insulating material.
6. The method of preparing a foamed silicone gel insulation material according to claim 5, wherein the first matrix is obtained by mixing the hydrogen-bonded methyl silicone and the azo-based foaming agent in the prescribed amounts; mixing the vinyl-containing methyl silicone and the inhibitor in a formula amount to obtain a second matrix; and mixing the first substrate and the second substrate, adding a catalyst, and uniformly mixing to obtain a mixture.
7. The method for preparing the foamed silicone gel thermal insulation material according to claim 5, wherein the cell structure of the foamed silicone gel thermal insulation material is adjusted by controlling the foaming ratio through selection of the content of the foaming agent, the preheating temperature, the preheating time, the curing temperature and the curing time.
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CN105504827A (en) * | 2015-12-09 | 2016-04-20 | 国网智能电网研究院 | Silica gel filling material and preparation method thereof |
CN106905705A (en) * | 2017-03-17 | 2017-06-30 | 深圳市维西科技有限公司 | A kind of silicone sealant gel and preparation method thereof |
CN106977724A (en) * | 2017-05-17 | 2017-07-25 | 东莞市兆科电子材料科技有限公司 | A kind of foamed silastic and preparation method thereof |
CN115386228A (en) * | 2021-05-24 | 2022-11-25 | 天津科技大学 | Novel silicon rubber foam material and preparation method thereof |
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2022
- 2022-12-07 CN CN202211562727.XA patent/CN115894927B/en active Active
Patent Citations (6)
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JP2002187971A (en) * | 2000-12-20 | 2002-07-05 | Ge Toshiba Silicones Co Ltd | Silicone foam material, foam, and method for producing the foam |
CN103502337A (en) * | 2011-12-09 | 2014-01-08 | 迈图高新材料日本合同公司 | Composition for silicone rubber foam, manufacturing method of silicone rubber foam, and silicone rubber foam |
CN105504827A (en) * | 2015-12-09 | 2016-04-20 | 国网智能电网研究院 | Silica gel filling material and preparation method thereof |
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CN115386228A (en) * | 2021-05-24 | 2022-11-25 | 天津科技大学 | Novel silicon rubber foam material and preparation method thereof |
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