CN111518392A - High-thermal-conductivity flame-retardant silicone gel and preparation method thereof - Google Patents

High-thermal-conductivity flame-retardant silicone gel and preparation method thereof Download PDF

Info

Publication number
CN111518392A
CN111518392A CN202010264729.5A CN202010264729A CN111518392A CN 111518392 A CN111518392 A CN 111518392A CN 202010264729 A CN202010264729 A CN 202010264729A CN 111518392 A CN111518392 A CN 111518392A
Authority
CN
China
Prior art keywords
vinyl
component
silicone resin
hydrogen
terminated
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202010264729.5A
Other languages
Chinese (zh)
Other versions
CN111518392B (en
Inventor
尹彬
雷勇
陈钢
陈建浩
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangzhou Yinhan Energy Technology Co ltd
Original Assignee
Guangzhou Yinhan Energy Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangzhou Yinhan Energy Technology Co ltd filed Critical Guangzhou Yinhan Energy Technology Co ltd
Priority to CN202010264729.5A priority Critical patent/CN111518392B/en
Publication of CN111518392A publication Critical patent/CN111518392A/en
Application granted granted Critical
Publication of CN111518392B publication Critical patent/CN111518392B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention relates to a high-thermal-conductivity flame-retardant silica gel and a preparation method thereof, belonging to the technical field of silica gel. The high-thermal-conductivity flame-retardant silicone gel prepared by the invention is applied to heat dissipation systems of electronic devices and power batteries, and the heat-conducting gel with extremely low oil permeability, excellent humidity and heat aging resistance and good resilience and compression permanent deformation is prepared by screening different vinyl-containing end-blocked polydimethylsiloxanes, reinforced vinyl silicone resin, reinforced hydrogen-containing silicone resin, modified hydrogen-containing cross-linking agent, heat-conducting powder and flame retardant, so that the heat-conducting gel is applied to various index requirements of the application of the electronic devices and the power batteries.

Description

High-thermal-conductivity flame-retardant silicone gel and preparation method thereof
Technical Field
The invention relates to a high-thermal-conductivity flame-retardant silica gel and a preparation method thereof, belonging to the technical field of silica gel.
Background
The heat-conducting interface material is widely applied to the fields of electronics and new energy automobile power batteries, and is commonly provided with four types of heat-conducting structure adhesives, heat-conducting gaskets, heat-conducting silicone grease and heat-conducting silicone gel. The adhesive with the heat-conducting structure has too high bonding strength and is not easy to disassemble and repair; the heat-conducting gasket cannot achieve a good filling effect in a complex structure, has high interface heat resistance and low heat-conducting efficiency when applied, and is not suitable for automatic production; the heat-conducting silicone grease has large oil leakage and does not meet the requirement of electronic application; the heat-conducting silica gel is better applied to the field of electronics and the field of new energy automobile power batteries.
However, in the current heat-conducting silica gel products applied to the electronic field and the new energy automobile power battery field in domestic and foreign markets, the damping effect is reduced due to insufficient oil permeability, insufficient humidity and heat aging resistance, poor resilience and compression permanent deformation, and the heat-conducting silica gel cracks during continuous vibration to cause poor heat dissipation of electronic devices and power batteries, so that the service life of the heat-conducting silica gel products is seriously shortened.
The invention prepares the heat-conducting gel with extremely low oil permeability, excellent humidity and heat aging resistance and good resilience and compression permanent deformation by screening different vinyl-containing end-blocked polydimethylsiloxane, reinforced vinyl silicone resin, reinforced hydrogen-containing silicone resin, modified hydrogen-containing cross-linking agent, heat-conducting powder and flame retardant.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the high-thermal-conductivity flame-retardant silicone gel and the preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: the high-thermal-conductivity flame-retardant silicone gel is composed of a component A and a component B, wherein the volume ratio of the component A to the component B is 1:1,
wherein the component A comprises the following components in percentage by mass: 7-13% of vinyl-terminated polydimethylsiloxane, 5-6% of reinforced vinyl resin, 63-74% of heat conducting powder, 13-20% of flame retardant powder and 0.3-0.5% of platinum catalyst;
the component B comprises the following components in percentage by mass: 4 to 9 percent of vinyl-terminated polydimethylsiloxane, 5 to 6 percent of reinforced vinyl silicone resin, 63 to 74 percent of heat conducting powder, 13 to 19 percent of flame retardant powder, 1.4 to 3.5 percent of hydrogen-containing silicone oil, 1 to 1.5 percent of reinforced hydrogen-containing silicone resin, 0.03 to 0.1 percent of inhibitor and 0.01 to 0.05 percent of carbon black.
As a preferable embodiment of the high thermal conductivity flame-retardant silicone gel, the high thermal conductivity flame-retardant silicone gel is composed of a component A and a component B, the volume ratio of the component A to the component B is 1:1,
wherein the component A comprises the following components in percentage by mass: 12.78% of vinyl-terminated polydimethylsiloxane, 5% of reinforced vinyl resin, 63.64% of heat conducting powder, 18.18% of flame retardant powder and 0.40% of platinum catalyst;
the component B comprises the following components in percentage by mass: 8.81% of vinyl-terminated polydimethylsiloxane, 5.01% of reinforced vinyl silicone resin, 63.57% of heat conducting powder, 18.15% of flame retardant powder, 3.34% of hydrogen-containing silicone oil, 1.00% of reinforced hydrogen-containing silicone resin, 0.10% of inhibitor and 0.02% of carbon black.
In the component A, the vinyl-terminated polydimethylsiloxane is at least one of double-terminated vinyl polydimethylsiloxane and single-terminated vinyl polydimethylsiloxane, the viscosity of the double-terminated vinyl polydimethylsiloxane is 300-20000 cps, and the viscosity of the single-terminated vinyl polydimethylsiloxane is 1000-20000 cps.
As a preferred embodiment of the high thermal conductive flame retardant silicone gel of the present invention, in the component a, the reinforcing vinyl resin is at least one of methyl vinyl MT silicone resin, methyl vinyl terminated hydroxyl-containing MT silicone resin, methyl vinyl MQ silicone resin, methyl vinyl terminated hydroxyl-containing MQ silicone resin, methyl vinyl MDT silicone resin, and methyl vinyl terminated hydroxyl-containing MDT silicone resin; the heat conducting powder is at least one of spherical alpha-alumina and hexagonal boron nitride, the particle size D99 of the spherical alpha-alumina is 20-100 mu m, and the particle size D99 of the hexagonal boron nitride is 20-60 mu m; the flame retardant powder is at least one of aluminum hydroxide and polysilicate; the concentration of the platinum catalyst is 500 to 20000 ppm.
In the component B, the vinyl-terminated polydimethylsiloxane is at least one of double-terminated vinyl polydimethylsiloxane and single-terminated vinyl polydimethylsiloxane, the viscosity of the double-terminated vinyl polydimethylsiloxane is 100-20000 cps, and the viscosity of the single-terminated vinyl polydimethylsiloxane is 1000-20000 cps.
In the component B, the reinforcing vinyl silicone resin is at least one of methyl vinyl MT silicone resin, methyl vinyl terminated hydroxyl-containing MT silicone resin, methyl vinyl MQ silicone resin and methyl vinyl terminated hydroxyl-containing MQ silicone resin; the heat conducting powder is at least one of spherical alpha-alumina and hexagonal boron nitride, the particle size D99 of the spherical alpha-alumina is 20-100 mu m, and the particle size D99 of the hexagonal boron nitride is 20-60 mu m; the flame retardant powder is at least one of aluminum hydroxide and polysilicate.
In a preferred embodiment of the highly heat-conductive flame-retardant silicone gel of the present invention, in the component B, the hydrogen-containing silicone oil is at least one of terminal hydrogen-containing silicone oil, side hydrogen-containing silicone oil, and terminal hydrogen-containing silicone oil, the hydrogen content of the terminal hydrogen-containing silicone oil is 0.06% to 0.36%, the hydrogen content of the side hydrogen-containing silicone oil is 0.1% to 0.75%, and the hydrogen content of the terminal hydrogen-containing silicone oil is 0.02% to 0.3%; the reinforcing hydrogen-containing silicone resin is at least one of methyl hydrogen group MT silicone resin, methyl hydrogen group terminated hydroxyl-containing MT silicone resin, methyl hydrogen group MQ silicone resin, methyl hydrogen group terminated hydroxyl-containing MQ silicone resin, methyl hydrogen group MDT silicone resin and methyl hydrogen group terminated hydroxyl-containing MDT silicone resin; the inhibitor is a tetravinyl cyclotetrasiloxane inhibitor.
In a second aspect, the invention provides a preparation method of the high thermal conductivity flame retardant silicone gel, which comprises the following steps:
(1) preparation of component A: adding vinyl-terminated polydimethylsiloxane, reinforcing vinyl resin, heat conducting powder, flame retardant powder and platinum catalyst into a stirrer, stirring, vacuumizing and continuously stirring after a paste is formed, and simultaneously starting circulating cooling water to obtain a component A;
(2) preparation of the component B: adding vinyl-terminated polydimethylsiloxane, reinforced vinyl silicone resin, heat conducting powder, flame retardant powder, hydrogen-containing silicone oil, reinforced hydrogen-containing silicone resin, inhibitor and carbon black into a stirrer, stirring until a paste is formed, vacuumizing and continuously stirring, and simultaneously starting circulating cooling water to obtain a component B;
(3) preparing high-thermal-conductivity flame-retardant silicone gel: and (3) uniformly mixing the component A obtained in the step (1) and the component B obtained in the step (2) to obtain the high-thermal-conductivity flame-retardant silicone gel.
As a preferred embodiment of the preparation method, in the step (1) and the step (2), the stirrer is a planetary stirrer, the stirring speed is 40r/min, the stirring time is 5-10 min, the stirrer is vacuumized until the vacuum degree is more than or equal to 0.08MPa, the continuous stirring speed is 40r/min, the dispersion speed is 600r/min, the stirring time is 60min, and the temperature of the material is controlled by circulating cooling water to be not higher than 80 ℃.
Compared with the prior art, the invention has the beneficial effects that: the high-thermal-conductivity flame-retardant silicone gel prepared by the invention is applied to heat dissipation systems of electronic devices and power batteries, and the heat-conducting gel with extremely low oil permeability, excellent humidity and heat aging resistance and good resilience and compression permanent deformation is prepared by screening different vinyl-containing end-blocked polydimethylsiloxanes, reinforced vinyl silicone resin, reinforced hydrogen-containing silicone resin, modified hydrogen-containing cross-linking agent, heat-conducting powder and flame retardant, so that the heat-conducting gel is applied to various index requirements of the application of the electronic devices and the power batteries.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
A high-thermal-conductivity flame-retardant silicone gel is composed of a component A and a component B, wherein the volume ratio of the component A to the component B is 1:1, and the preparation method comprises the following steps:
(1) preparation of component A: weighing 215.6g of 1000cps double-end-capped vinyl polydimethylsiloxane, 359.4g of 2000cps single-end-capped vinyl polydimethylsiloxane, 225g of methyl vinyl end-capped hydroxyl-containing MDT silicone resin, 2863g of 55 mu m spherical alumina powder, 818g of polysilicate and 18g of platinum catalyst, adding the materials into a planetary stirrer, stirring for 5-10 min at a stirring speed of 40r/min under normal pressure, vacuumizing to a vacuum degree of more than or equal to 0.08MPa after powder and liquid form a paste, stirring for 60min at a dispersing speed of 600r/min, simultaneously starting circulating cooling water, controlling the material temperature to be not higher than 80 ℃, and preparing a component A;
(2) preparation of the component B: weighing 108.4g of 1000cps double-end-capped vinyl polydimethylsiloxane, 314g of 2000cps single-end-capped vinyl polydimethylsiloxane, 240g of methyl vinyl MT silicon resin, 3047g of 55 mu m spherical alumina powder, 870g of polysilicate, 79.2g of 0.1% end-capped hydrogen-containing silicone oil, 80.8g of 0.08% end-side hydrogen-containing silicone oil, 48g of methylhydrogen MDT silicon resin, 5g of 10% tetra-vinyl cyclotetrasiloxane inhibitor and 1g of carbon black, adding the materials into a planetary stirrer, stirring for 5-10 min at a stirring speed of 40r/min under normal pressure, vacuumizing to a vacuum degree of more than or equal to 0.08MPa after the powder liquid is formed into a paste, stirring for 60min at a dispersing speed of 600r/min, simultaneously starting circulating cooling water, controlling the material temperature to be not more than 80 ℃, and preparing a component B;
(3) preparing high-thermal-conductivity flame-retardant silicone gel: and (3) uniformly mixing the component A obtained in the step (1) and the component B obtained in the step (2) to obtain the high-thermal-conductivity flame-retardant silicone gel.
Example 2
A high-thermal-conductivity flame-retardant silicone gel is composed of a component A and a component B, wherein the volume ratio of the component A to the component B is 1:1, and the preparation method comprises the following steps:
(1) preparation of component A: weighing 311.4g of 1000cps double-end-capped vinyl polydimethylsiloxane, 518.6g of 2000cps single-end-capped vinyl polydimethylsiloxane, 500g of methyl vinyl MDT silicone resin, 6067g of 95-micron spherical alumina powder, 1213g of 45-micron spherical alumina powder, 1360g of aluminum hydroxide and 30g of platinum catalyst, adding into a planetary stirrer, stirring at a stirring speed of 40r/min at normal pressure for 5-10 min, vacuumizing to a vacuum degree of more than or equal to 0.08Mpa and at a stirring speed of 40r/min after powder and liquid form paste, stirring at a dispersion speed of 600r/min for 60min, simultaneously starting circulating cooling water, controlling the material temperature to be not higher than 80 ℃, and preparing a component A;
(2) preparation of the component B: weighing 152.6g of 1000cps double-end-capped vinyl polydimethylsiloxane, 406.4g of 2000cps single-end-capped vinyl silicone oil, 500g of methyl vinyl end-capped hydroxyl-containing MQ silicone resin, 6120g of 95 μm spherical alumina powder, 1224g of 45 μm spherical alumina powder, 1331g of aluminum hydroxide, 100g of methyl hydrogen-based MDT silicone resin, 0.62g of 0.04% end-side type hydrogen-containing silicone oil, 82.2g of 0.1% end-side hydrogen-containing silicone oil, 79.12g of 0.08% end-side type hydrogen-containing silicone oil, 3g of 10% tetravinyl cyclotetrasiloxane inhibitor and 1g of carbon black, adding into a planetary stirrer, stirring at a stirring speed of 40r/min under normal pressure for 5-10 min, vacuumizing to a vacuum degree of not less than 0.08MPa after the powder liquid is formed into a paste, stirring at a dispersion speed of 600r/min for 60min, simultaneously starting circulating cooling water, controlling the material temperature to be not higher than 80 ℃, and preparing a component B;
(3) preparing high-thermal-conductivity flame-retardant silicone gel: and (3) uniformly mixing the component A obtained in the step (1) and the component B obtained in the step (2) to obtain the high-thermal-conductivity flame-retardant silicone gel.
Example 3
A high-thermal-conductivity flame-retardant silicone gel is composed of a component A and a component B, wherein the volume ratio of the component A to the component B is 1:1, and the preparation method comprises the following steps:
(1) preparation of component A: weighing 363.6g of 1000cps double-end-capped vinyl polydimethylsiloxane, 273.9g of 500cps double-end-capped vinyl polydimethylsiloxane, 92.5g of 2000cps single-end-capped vinyl polydimethylsiloxane, 600g of methyl vinyl MDT silicone resin, 6067g of 88 mu m spherical alumina powder, 1213g of 55 mu m spherical alumina powder, 1360g of aluminum hydroxide and 30g of platinum catalyst, adding the materials into a planetary stirrer, stirring at a stirring speed of 40r/min under normal pressure for 5-10 min, after the powder liquid is formed into a paste, vacuumizing to a vacuum degree of more than or equal to 0.08MPa, stirring at a stirring speed of 40r/min and a dispersion speed of 600r/min for 60min, simultaneously turning on circulating cooling water, and controlling the material temperature to be not higher than 80 ℃ to obtain a component A;
(2) preparation of the component B: weighing 157g of 1000cps double-end-capped vinyl polydimethylsiloxane, 275g of 2000cps single-end-capped vinyl polydimethylsiloxane, 600g of methyl vinyl end-capped hydroxyl-containing MT silicone resin, 6108g of 88μm spherical alumina powder, 1222g of 55μm spherical alumina powder, 1335g of aluminum hydroxide, 57.3g of 0.1% end-containing hydrogen silicone oil, 91.7g of 0.08% end-side type hydrogen-containing silicone oil, 150g of methyl hydrogen base MQ silicone resin, 3g of 10% tetra-vinyl cyclotetrasiloxane inhibitor and 1g of carbon black, adding into a planetary stirrer, stirring for 5-10 min at a stirring speed of 40r/min under normal pressure, vacuumizing to a vacuum degree of more than or equal to 0.08MPa after the powder liquid is formed into a paste, stirring for 60min at a dispersing speed of 600r/min, simultaneously starting circulating cooling water, controlling the material temperature to be not higher than 80 ℃, and preparing a component B;
(3) preparing high-thermal-conductivity flame-retardant silicone gel: and (3) uniformly mixing the component A obtained in the step (1) and the component B obtained in the step (2) to obtain the high-thermal-conductivity flame-retardant silicone gel.
Comparative example 1
A high-thermal-conductivity flame-retardant silicone gel is composed of a component A and a component B, wherein the volume ratio of the component A to the component B is 1:1, and the preparation method comprises the following steps:
(1) weighing 927.5g of 350cps double-end-capped vinyl polydimethylsiloxane, 927.5g of 20000cps double-end-capped vinyl polydimethylsiloxane, 1855g of 2000cps double-end-capped vinyl polydimethylsiloxane, 6326.4g of 30 mu m spherical alumina powder, 14761.7g of 20 mu m spherical alumina powder and 99.5g of platinum catalyst, adding into a planetary stirrer, stirring at a stirring speed of 40r/min at normal pressure for 5-10 min, vacuumizing to a vacuum degree of more than or equal to 0.08Mpa and at a stirring speed of 40r/min after the powder liquid is formed into a paste, stirring at a dispersion speed of 600r/min for 60min, simultaneously turning on circulating cooling water, controlling the material temperature to be not higher than 80 ℃, and preparing a component A;
(2) weighing 927.5g of 350cps double-end-capped vinyl polydimethylsiloxane, 927.5g of 20000cps double-end-capped vinyl polydimethylsiloxane, 1855g of 2000cps double-end-capped vinyl polydimethylsiloxane, 6326.5g of 30 mu m spherical alumina powder, 14761.7g of 20 mu m spherical alumina powder, 183.1g of 0.36% side hydrogen-containing silicone oil, 17.8g of 10% acetylene glycol and 2.3g of carbon black, adding the materials into a planetary stirrer, stirring at a stirring speed of 40r/min at normal pressure for 5-10 min, vacuumizing to a vacuum degree of more than or equal to 0.08MPa after the powder liquid is formed into a paste, stirring at a stirring speed of 40r/min at a dispersion speed of 600r/min for 60min, simultaneously starting circulating cooling water, and controlling the material temperature to be not higher than 80 ℃ to obtain a component B;
(3) preparing high-thermal-conductivity flame-retardant silicone gel: and (3) uniformly mixing the component A obtained in the step (1) and the component B obtained in the step (2) to obtain the high-thermal-conductivity flame-retardant silicone gel.
Examples of effects
And (3) performing glue performance test and colloid mechanical performance test on the performances of the high-thermal-conductivity flame-retardant silica gel prepared in the examples 1-3 and the comparative example 1. The standard and the result of the glue performance test are shown in table 1, and the mechanical property test method of the glue comprises the following steps: the colloid is aged for 1000h at 85 ℃, 85% humidity and RH, the mechanical properties are compared, and the test results are shown in Table 2.
TABLE 1
Figure BDA0002440836200000071
TABLE 2
Figure BDA0002440836200000072
As shown in tables 1 and 2, the high thermal conductivity flame retardant silicone gel prepared according to the formula of the invention has the advantages of extremely low oil permeability, excellent resistance to wet heat aging, and good resilience and compression permanent deformation. The performance of the high-thermal-conductivity flame-retardant silicone gel prepared in the example 1 is the best, namely when the component A comprises the following components in percentage by mass: 12.78% of vinyl-terminated polydimethylsiloxane, 5% of reinforced vinyl resin, 63.64% of heat conducting powder, 18.18% of flame retardant powder and 0.4% of platinum catalyst; the component B comprises the following components in percentage by mass: 8.81 percent of vinyl-terminated polydimethylsiloxane, 5.01 percent of reinforced vinyl silicone resin, 63.57 percent of heat conducting powder, 18.15 percent of flame retardant powder, 3.34 percent of hydrogen-containing silicone oil, 1.00 percent of reinforced hydrogen-containing silicone resin, 0.10 percent of inhibitor and 0.02 percent of carbon black, and the prepared high-heat-conductivity flame retardant silicone gel has the best performance.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (9)

1. The high-thermal-conductivity flame-retardant silicone gel is characterized by consisting of a component A and a component B, wherein the volume ratio of the component A to the component B is 1:1,
wherein the component A comprises the following components in percentage by mass: 7-13% of vinyl-terminated polydimethylsiloxane, 5-6% of reinforced vinyl resin, 63-74% of heat conducting powder, 13-20% of flame retardant powder and 0.3-0.5% of platinum catalyst;
the component B comprises the following components in percentage by mass: 4 to 9 percent of vinyl-terminated polydimethylsiloxane, 5 to 6 percent of reinforced vinyl silicone resin, 63 to 74 percent of heat conducting powder, 13 to 19 percent of flame retardant powder, 1.4 to 3.5 percent of hydrogen-containing silicone oil, 1 to 1.5 percent of reinforced hydrogen-containing silicone resin, 0.03 to 0.1 percent of inhibitor and 0.01 to 0.05 percent of carbon black.
2. The high thermal conductivity flame retardant silicone gel according to claim 1, wherein the high thermal conductivity flame retardant silicone gel is composed of a component A and a component B, the volume ratio of the component A to the component B is 1:1,
wherein the component A comprises the following components in percentage by mass: 12.78% of vinyl-terminated polydimethylsiloxane, 5% of reinforced vinyl resin, 63.64% of heat conducting powder, 18.18% of flame retardant powder and 0.4% of platinum catalyst;
the component B comprises the following components in percentage by mass: 8.81% of vinyl-terminated polydimethylsiloxane, 5.01% of reinforced vinyl silicone resin, 63.57% of heat conducting powder, 18.15% of flame retardant powder, 3.34% of hydrogen-containing silicone oil, 1.00% of reinforced hydrogen-containing silicone resin, 0.10% of inhibitor and 0.02% of carbon black.
3. The high thermal conductivity flame retardant silicone gel according to any one of claims 1 to 2, wherein in the component A, the vinyl terminated polydimethylsiloxane is at least one of a double terminated vinyl polydimethylsiloxane and a single terminated vinyl polydimethylsiloxane, the viscosity of the double terminated vinyl polydimethylsiloxane is 300 to 20000cps, and the viscosity of the single terminated vinyl polydimethylsiloxane is 1000 to 20000 cps.
4. The high thermal conductivity flame retardant silicone gel according to any one of claims 1 to 2, wherein in the component a, the reinforcing vinyl resin is at least one of methyl vinyl MT silicone resin, methyl vinyl terminated hydroxyl-containing MT silicone resin, methyl vinyl MQ silicone resin, methyl vinyl terminated hydroxyl-containing MQ silicone resin, methyl vinyl MDT silicone resin, and methyl vinyl terminated hydroxyl-containing MDT silicone resin; the heat conducting powder is at least one of spherical alpha-alumina and hexagonal boron nitride, the particle size D99 of the spherical alpha-alumina is 20-100 mu m, and the particle size D99 of the hexagonal boron nitride is 20-60 mu m; the flame retardant powder is at least one of aluminum hydroxide and polysilicate; the concentration of the platinum catalyst is 500 to 20000 ppm.
5. The silicone gel of any one of claims 1 to 2, wherein in the component B, the vinyl terminated polydimethylsiloxane is at least one of a double terminated vinyl polydimethylsiloxane and a single terminated vinyl polydimethylsiloxane, the viscosity of the double terminated vinyl polydimethylsiloxane is 100 to 20000cps, and the viscosity of the single terminated vinyl polydimethylsiloxane is 1000 to 20000 cps.
6. The high thermal conductivity flame retardant silicone gel according to any one of claims 1 to 2, wherein in the component B, the reinforcing vinyl silicone resin is at least one of methyl vinyl MT silicone resin, methyl vinyl terminated hydroxyl-containing MT silicone resin, methyl vinyl MQ silicone resin, and methyl vinyl terminated hydroxyl-containing MQ silicone resin; the heat conducting powder is at least one of spherical alpha-alumina and hexagonal boron nitride, the particle size D99 of the spherical alpha-alumina is 20-100 mu m, and the particle size D99 of the hexagonal boron nitride is 20-60 mu m; the flame retardant powder is at least one of aluminum hydroxide and polysilicate.
7. The highly thermally conductive flame-retardant silicone gel according to any one of claims 1 to 2, wherein in the component B, the hydrogen-containing silicone oil is at least one of terminal hydrogen-containing silicone oil, side hydrogen-containing silicone oil and terminal side hydrogen-containing silicone oil, the terminal hydrogen-containing silicone oil has a hydrogen content of 0.06% to 0.36%, the side hydrogen-containing silicone oil has a hydrogen content of 0.1% to 0.75%, and the terminal side hydrogen-containing silicone oil has a hydrogen content of 0.02% to 0.3%; the reinforcing hydrogen-containing silicone resin is at least one of methyl hydrogen group MT silicone resin, methyl hydrogen group terminated hydroxyl-containing MT silicone resin, methyl hydrogen group MQ silicone resin, methyl hydrogen group terminated hydroxyl-containing MQ silicone resin, methyl hydrogen group MDT silicone resin and methyl hydrogen group terminated hydroxyl-containing MDT silicone resin; the inhibitor is a tetravinyl cyclotetrasiloxane inhibitor.
8. The preparation method of the high-thermal-conductivity flame-retardant silicone gel according to any one of claims 1 to 7, comprising the following steps:
(1) preparation of component A: adding vinyl-terminated polydimethylsiloxane, reinforcing vinyl resin, heat conducting powder, flame retardant powder and platinum catalyst into a stirrer, stirring, vacuumizing and continuously stirring after a paste is formed, and simultaneously starting circulating cooling water to obtain a component A;
(2) preparation of the component B: adding vinyl-terminated polydimethylsiloxane, reinforced vinyl silicone resin, heat conducting powder, flame retardant powder, hydrogen-containing silicone oil, reinforced hydrogen-containing silicone resin, inhibitor and carbon black into a stirrer, stirring until a paste is formed, vacuumizing and continuously stirring, and simultaneously starting circulating cooling water to obtain a component B;
(3) preparing high-thermal-conductivity flame-retardant silicone gel: and (3) uniformly mixing the component A obtained in the step (1) and the component B obtained in the step (2) to obtain the high-thermal-conductivity flame-retardant silicone gel.
9. The preparation method according to claim 8, wherein in the step (1) and the step (2), the stirrer is a planetary stirrer, the stirring speed is 40r/min, the stirring time is 5-10 min, the vacuum degree is not less than 0.08MPa, the continuous stirring speed is 40r/min, the dispersion speed is 600r/min, the stirring time is 60min, and the material temperature is controlled to be not higher than 80 ℃ by circulating cooling water.
CN202010264729.5A 2020-04-03 2020-04-03 High-thermal-conductivity flame-retardant silicone gel and preparation method thereof Active CN111518392B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010264729.5A CN111518392B (en) 2020-04-03 2020-04-03 High-thermal-conductivity flame-retardant silicone gel and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010264729.5A CN111518392B (en) 2020-04-03 2020-04-03 High-thermal-conductivity flame-retardant silicone gel and preparation method thereof

Publications (2)

Publication Number Publication Date
CN111518392A true CN111518392A (en) 2020-08-11
CN111518392B CN111518392B (en) 2022-02-11

Family

ID=71901356

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010264729.5A Active CN111518392B (en) 2020-04-03 2020-04-03 High-thermal-conductivity flame-retardant silicone gel and preparation method thereof

Country Status (1)

Country Link
CN (1) CN111518392B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113604139A (en) * 2021-07-30 2021-11-05 杭州埃比森新材料有限公司 Transparent organic silicon coating and preparation method thereof
CN116103015A (en) * 2023-03-29 2023-05-12 广州市垠瀚能源科技有限公司 Pouring sealant and preparation method thereof
CN116554693A (en) * 2023-06-25 2023-08-08 江西天永诚高分子材料有限公司 Single-component high-heat-conductivity silicon mud and preparation method thereof
CN116554693B (en) * 2023-06-25 2024-06-11 江西天永诚高分子材料有限公司 Single-component high-heat-conductivity silicon mud and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102807757A (en) * 2012-07-31 2012-12-05 烟台德邦先进硅材料有限公司 Organic silica gel used for packaging IGBT (insulated gate bipolar translator) module, and preparation method of organic silica gel
CN107722920A (en) * 2017-11-08 2018-02-23 深圳市超硕电子有限公司 A kind of bi-component heat conductive flame-retarding gel and preparation method thereof
CN109294240A (en) * 2018-10-22 2019-02-01 广州市垠瀚能源科技有限公司 A kind of reworkable thermally conductive addition-type silicon rubber preparation method of the low cleavage strength of low adhesive strength
CN109438995A (en) * 2018-12-21 2019-03-08 广州市白云化工实业有限公司 The high-intensitive add-on type Silica hydrogel and preparation method thereof of hypotonic oil
CN110591371A (en) * 2019-07-31 2019-12-20 天永诚高分子材料(常州)有限公司 High-adhesion heat-conducting silica gel capable of being formed in situ and preparation method thereof
CN111051434A (en) * 2017-07-24 2020-04-21 陶氏东丽株式会社 Multi-component curable heat-conductive silicone gel composition, heat-conductive member, and heat-dissipating structure

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102807757A (en) * 2012-07-31 2012-12-05 烟台德邦先进硅材料有限公司 Organic silica gel used for packaging IGBT (insulated gate bipolar translator) module, and preparation method of organic silica gel
CN111051434A (en) * 2017-07-24 2020-04-21 陶氏东丽株式会社 Multi-component curable heat-conductive silicone gel composition, heat-conductive member, and heat-dissipating structure
CN107722920A (en) * 2017-11-08 2018-02-23 深圳市超硕电子有限公司 A kind of bi-component heat conductive flame-retarding gel and preparation method thereof
CN109294240A (en) * 2018-10-22 2019-02-01 广州市垠瀚能源科技有限公司 A kind of reworkable thermally conductive addition-type silicon rubber preparation method of the low cleavage strength of low adhesive strength
CN109438995A (en) * 2018-12-21 2019-03-08 广州市白云化工实业有限公司 The high-intensitive add-on type Silica hydrogel and preparation method thereof of hypotonic oil
CN110591371A (en) * 2019-07-31 2019-12-20 天永诚高分子材料(常州)有限公司 High-adhesion heat-conducting silica gel capable of being formed in situ and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
赵士贵: "含氢、含乙烯基硅树脂的合成及其作为高温硫化硅橡胶交联剂的研究", 《万方学位论文数据库》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113604139A (en) * 2021-07-30 2021-11-05 杭州埃比森新材料有限公司 Transparent organic silicon coating and preparation method thereof
CN116103015A (en) * 2023-03-29 2023-05-12 广州市垠瀚能源科技有限公司 Pouring sealant and preparation method thereof
CN116554693A (en) * 2023-06-25 2023-08-08 江西天永诚高分子材料有限公司 Single-component high-heat-conductivity silicon mud and preparation method thereof
CN116554693B (en) * 2023-06-25 2024-06-11 江西天永诚高分子材料有限公司 Single-component high-heat-conductivity silicon mud and preparation method thereof

Also Published As

Publication number Publication date
CN111518392B (en) 2022-02-11

Similar Documents

Publication Publication Date Title
CN107974232B (en) LED chip insulating heat-conducting die bond adhesive and preparation method thereof
CN110016205B (en) Epoxy resin heat-conducting insulating material and preparation method thereof
CN111518392B (en) High-thermal-conductivity flame-retardant silicone gel and preparation method thereof
CN110951254A (en) Boron nitride composite high-thermal-conductivity insulating polymer composite material and preparation method thereof
CN103059576A (en) High-heat-conductivity flexible silica gel gasket and preparation method thereof
CN112812740B (en) Double-component high-thermal-conductivity self-leveling pouring sealant and preparation method and application thereof
CN107141815B (en) High-temperature-resistant low-modulus heat-conducting organosilicon material and preparation method thereof
CN102337033A (en) Additive high-thermal-conductivity organic silicon electronic pouring sealant and preparation method thereof
CN106753208B (en) Graphene oxide modified LED heat-conducting pouring sealant and preparation method thereof
CN111073300A (en) Heat-conducting gel easy to repair and preparation method thereof
CN101928462A (en) Acetone-removing silicon rubber and preparation method thereof
CN110157375A (en) A kind of conductive and heat-conductive Silica hydrogel adhesive and preparation method thereof
CN117844255A (en) Silica gel sheet and preparation method and application thereof
CN112778766A (en) High-reliability high-thermal-conductivity silicone gel composition and preparation method and application thereof
CN115232444A (en) High-thermal-conductivity spherical boron nitride composite epoxy resin and preparation method thereof
CN105419672A (en) Preparation method of high-heat-dissipation electric-conductive glue used for high-power LED
CN113524741A (en) Vertically-arranged boron nitride nanosheet high-molecular composite material heat-conducting sheet and preparation method thereof
CN110746926A (en) Self-adhesive heat-conducting flame-retardant two-component electronic encapsulating silicone rubber and preparation method thereof
CN112322042A (en) High-thermal-conductivity single-component heat-conducting gel and preparation method thereof
CN110684359A (en) Silica gel gasket and preparation method thereof
CN114574154A (en) Low-viscosity two-component heat-conducting pouring sealant and preparation method thereof
CN116554685A (en) Bi-component heat-conducting gel and preparation method and application thereof
CN114106560A (en) Preparation method and product of heat-conducting silica gel
CN109161206A (en) A kind of high security new energy car battery
CN109897591A (en) A kind of low viscosity bi-component organic silicon high thermal conductivity casting glue and preparation method thereof for lithium battery

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant