[go: up one dir, main page]

CN116253885B - A thermally conductive powder modifier and preparation method thereof and thermally conductive potting glue - Google Patents

A thermally conductive powder modifier and preparation method thereof and thermally conductive potting glue Download PDF

Info

Publication number
CN116253885B
CN116253885B CN202310123842.5A CN202310123842A CN116253885B CN 116253885 B CN116253885 B CN 116253885B CN 202310123842 A CN202310123842 A CN 202310123842A CN 116253885 B CN116253885 B CN 116253885B
Authority
CN
China
Prior art keywords
thermally conductive
vinyl
container
weight
conductive powder
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.)
Active
Application number
CN202310123842.5A
Other languages
Chinese (zh)
Other versions
CN116253885A (en
Inventor
李马刚
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.)
Suzhou Lingyu Electronic Technology Co Ltd
Original Assignee
Suzhou Lingyu Electronic 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 Suzhou Lingyu Electronic Technology Co Ltd filed Critical Suzhou Lingyu Electronic Technology Co Ltd
Priority to CN202310123842.5A priority Critical patent/CN116253885B/en
Publication of CN116253885A publication Critical patent/CN116253885A/en
Application granted granted Critical
Publication of CN116253885B publication Critical patent/CN116253885B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/38—Polysiloxanes modified by chemical after-treatment
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Sealing Material Composition (AREA)
  • Silicon Polymers (AREA)

Abstract

本发明主要公开了一种导热粉体改性剂的制备方法，包括以下步骤：以乙烯基三甲氧基硅烷或乙烯基三乙氧基硅烷为底物，通过酯交换反应合成出乙烯基烷氧基硅烷；通过单羟基硅油和所述乙烯基烷氧基硅烷的缩合反应得到含有硅氧烷链节的乙烯基长链烷氧基硅烷。该方法能获得能适用于导热粉体改性的导热粉体改性剂，且该方法制作获得的导热粉体改性剂能应用于导热灌封胶的制作中，以降低制作获得的导热灌封胶的粘度，提高其导热散热性能，降低介电常数，减缓导热灌封胶内导热粉体沉降和板结的出现，提升导热灌封胶的存储稳定性。The present invention mainly discloses a method for preparing a thermally conductive powder modifier, comprising the following steps: using vinyl trimethoxysilane or vinyl triethoxysilane as a substrate, synthesizing vinyl alkoxysilane through an ester exchange reaction; obtaining a vinyl long-chain alkoxysilane containing a siloxane chain segment through a condensation reaction of monohydroxy silicone oil and the vinyl alkoxysilane. The method can obtain a thermally conductive powder modifier suitable for thermally conductive powder modification, and the thermally conductive powder modifier prepared by the method can be applied to the preparation of thermally conductive potting glue to reduce the viscosity of the prepared thermally conductive potting glue, improve its thermal conductivity and heat dissipation performance, reduce the dielectric constant, slow down the sedimentation and agglomeration of thermally conductive powder in the thermally conductive potting glue, and improve the storage stability of the thermally conductive potting glue.

Description

Heat conducting powder modifier, preparation method thereof and heat conducting pouring sealant
Technical Field
The utility model relates to the field of production of organic silicon heat-conducting materials, in particular to a preparation method of a heat-conducting powder modifier.
Background
The organic silicon heat conduction pouring sealant, also called pouring silica gel or electronic silica gel, is widely applied to the electric field, the electronic integration field, the electric appliance packaging field, the electric automobile field and the like, and is beneficial to improving the safety and the service life of electric and electronic devices.
Silicone oil and inorganic heat conducting powder can be used in the preparation of the traditional organic silicon heat conducting pouring sealant, wherein the use of the heat conducting powder can ensure that the finished organic silicon heat conducting pouring sealant has higher heat conductivity coefficient. In order to improve the compatibility of the heat-conducting powder and the silicone oil, the heat-conducting powder needs to be modified, and commonly used heat-conducting powder modifying agents include alkoxy silane, stearic acid, titanate and the like.
However, when the heat-conducting powder modified by the modifier is actually used, the compatibility of the heat-conducting powder and silicone oil is still difficult to say to be excellent, and particularly, the heat-conducting powder in the organic silicon heat-conducting pouring sealant can be settled, thickened and the like when the finished organic silicon heat-conducting pouring sealant is placed for a long time, so that the use and heat-conducting performance of the organic silicon heat-conducting pouring sealant are affected.
Disclosure of utility model
The utility model aims to provide a preparation method of a heat conducting powder modifier, which can solve one or more of the problems.
According to one aspect of the present utility model, there is provided a heat conductive powder modifier comprising a vinyl long chain alkoxysilane containing siloxane units.
The heat conducting powder modifier has the beneficial effects that the heat conducting powder modifier can be suitable for modifying heat conducting powder and can be applied to manufacturing of heat conducting pouring sealant, so that the viscosity of the manufactured heat conducting pouring sealant is reduced, the heat conducting and radiating performance of the heat conducting pouring sealant is improved, the dielectric constant is reduced, the occurrence of sedimentation and hardening of the heat conducting powder in the heat conducting pouring sealant is slowed down, and the storage stability of the heat conducting pouring sealant is improved.
According to one aspect of the present utility model, there is provided a method for preparing a heat conductive powder modifier, comprising the steps of:
vinyl trimethoxy silane or vinyl triethoxy silane is used as a substrate, and vinyl alkoxy silane is synthesized through transesterification;
The vinyl long-chain alkoxy silane containing siloxane chain is obtained through condensation reaction of monohydroxy silicone oil and the vinyl alkoxy silane.
The preparation method of the heat conducting powder modifier has the beneficial effects that the heat conducting powder modifier which can be suitable for heat conducting powder modification can be obtained, and the heat conducting powder modifier prepared by the method can be applied to the preparation of the heat conducting pouring sealant, so that the viscosity of the heat conducting pouring sealant obtained by the preparation is reduced, the heat conducting and heat dissipating properties of the heat conducting pouring sealant are improved, the dielectric constant is reduced, the occurrence of sedimentation and hardening of the heat conducting powder in the heat conducting pouring sealant is slowed down, and the storage stability of the heat conducting pouring sealant is improved.
In some embodiments, a method of preparing a thermally conductive powder modifier comprises the steps of:
Adding R 2 OH and a solvent into a first container under the protection of nitrogen, heating the first container to a first temperature, wherein the first temperature is 50-80 ℃, adding a catalyst while stirring at the first temperature, and the stirring time is 0.5-1 h;
diluting Vi-Si- (OR 1)3) with a solvent in a second container to obtain Vi-Si- (OR 1)3) solution, dropwise adding the Vi-Si- (OR 1)3) solution into the first container after stirring is finished, wherein the dropwise adding time is 3-10 h, and enabling the first container to carry out transesterification reaction:
Vi-Si-(OR1)3+ R2OH←→Vi-Si-(OR2)3+ R1OH,
Obtaining Vi-Si- (OR 2)3 and R 1 OH, wherein Vi-Si- (OR 1)3) is vinyl trimethoxysilane OR vinyl triethoxysilane, and Vi-Si- (OR 2)3) is vinyl alkoxysilane;
Heating the first container after the completion of dropwise adding of the Vi-Si- (OR 1)3) solution to a second temperature which is 100-120 ℃, carrying out primary heat preservation on the first container at the second temperature for 2-5 hours, evaporating R 1 OH and part of solvent,
Cooling the first container subjected to the first heat preservation to 50-70 ℃, then dropwise adding a monohydroxy silicone oil solution into the first container for 1-2 h, and performing a second heat preservation for 2-5 h after the dropwise adding is finished, so that the condensation reaction can be performed in the first container:
Vi-Si-(OR2)3+ OH-Si(CH3)2-O-[ Si(CH3)2-O]m- Si(CH3)3←→Vi-Si(OR2)2-O-Si(CH3)2-O-[ Si(CH3)2-O]mSi(CH3)3,
Obtaining Vi-Si(OR2)2-O-Si(CH3)2-O-[ Si(CH3)2-O]mSi(CH3)3, the OH-Si (CH 3)2-O-[ Si(CH3)2-O]m- Si(CH3)3 is monohydroxy silicone oil, and Vi-Si(OR2)2-O-Si(CH3)2-O-[ Si(CH3)2-O]mSi(CH3)3 is vinyl long-chain alkoxysilane containing siloxane units;
and heating the first container to 110-130 ℃ after the second heat preservation, and distilling to remove R 2 OH and the residual solvent to obtain the heat-conducting powder modifier.
In the preparation method of the heat conducting powder modifier, the efficient transesterification reaction between Vi-Si- (OR 1)3 and R 2 OH can be ensured, and the efficient condensation reaction between Vi-Si- (OR 2)3 and OH-Si (CH 3)2-O-[ Si(CH3)2-O]m- Si(CH3)3) can be ensured
And R 1OH、R2 OH and solvent are eliminated as much as possible through multiple timely heating, so that the purity of the obtained heat conducting powder modifier is effectively improved.
In some embodiments, the catalyst is a basic material.
In some embodiments, the R 2 OH is n-decanol, n-dodecanol, or n-octanol.
In some embodiments, the R 1 OH is methanol.
In some embodiments, the viscosity of the monohydroxy silicone oil is 10cps to 50cps.
According to one aspect of the present utility model, there is provided a heat conductive pouring sealant, to which the heat conductive powder modifier according to claim 1 or 2 is applied.
The heat-conducting pouring sealant has the beneficial effects that the viscosity of the heat-conducting pouring sealant can be effectively reduced, the heat-conducting and heat-radiating properties can be effectively improved, the dielectric constant is reduced, the occurrence of sedimentation and hardening of heat-conducting powder in the heat-conducting pouring sealant is slowed down, and the storage stability is enhanced through testing.
In some embodiments, the formulation of the heat conductive pouring sealant comprises a component A and a component B,
The component A comprises 45-55 parts by weight of vinyl silicone oil, 540-560 parts by weight of heat conducting powder, 4-6 parts by weight of heat conducting powder modifier and 1.5-2.5 parts by weight of catalyst;
The component B comprises 45-55 parts by weight of vinyl silicone oil, 5-7 parts by weight of hydrogen-containing silicone oil, 540-560 parts by weight of heat conducting powder, 4-6 parts by weight of heat conducting powder modifier and 0.8-1.2 parts by weight of inhibitor;
The component A and the component B are mixed according to the weight ratio of 0.8-1.2:0.8-1.2, and are cured for 30min and more at 70-90 ℃.
Detailed Description
The utility model is described in further detail below with reference to the accompanying drawings.
Example 1
The first container is preferably a four-port reaction flask, the second container is preferably a flask, R 2 OH is preferably n-octanol, the solvent is preferably water, the catalyst is preferably NaOH, and Vi-Si- (OR 1)3) is preferably vinyltrimethoxysilane.
A preparation method of a heat conducting powder modifier comprises the following steps:
Adding R 2 OH and a solvent into a first container under the protection of nitrogen, heating the first container to a first temperature of about 50 ℃, adding a catalyst while stirring at the first temperature, and stirring for about 0.5h.
Diluting Vi-Si- (OR 1)3) with a solvent in a second container to obtain Vi-Si- (OR 1)3) solution, dropwise adding the Vi-Si- (OR 1)3) solution into the first container after stirring is finished, wherein the dropwise adding time is about 3h, and enabling transesterification reaction to be carried out in the first container:
Vi-Si-(OR1)3+ R2OH←→Vi-Si-(OR2)3+ R1OH,
Obtaining Vi-Si- (OR 2)3 and R 1 OH, wherein Vi-Si- (OR 2)3) is vinyl alkoxy silane, and R 1 OH is methanol;
The first vessel after the completion of the dropwise addition of the Vi-Si- (OR 1)3) solution was warmed to a second temperature of about 120℃to allow the first vessel to be subjected to a first incubation at the second temperature for about 2 hours, and R 1 OH and a part of the solvent were distilled off by the first incubation.
Cooling the first container with the first heat preservation to about 50 ℃, then dropwise adding a monohydroxy silicone oil solution with the viscosity of 20cps into the first container for about 1h, and carrying out the second heat preservation for about 2h after the dropwise adding, so that the condensation reaction can be carried out in the first container:
Vi-Si-(OR2)3+ OH-Si(CH3)2-O-[ Si(CH3)2-O]m- Si(CH3)3←→Vi-Si(OR2)2-O-Si(CH3)2-O-[ Si(CH3)2-O]mSi(CH3)3, Wherein OH-Si (CH 3)2-O-[ Si(CH3)2-O]m- Si(CH3)3 refers to the monohydroxy silicone oil, and the obtained Vi-Si(OR2)2-O-Si(CH3)2-O-[ Si(CH3)2-O]mSi(CH3)3,Vi-Si(OR2)2-O-Si(CH3)2-O-[ Si(CH3)2-O]mSi(CH3)3 is vinyl long-chain alkoxy silane containing siloxane chain segments.
And heating the first container after the second heat preservation to about 120 ℃, and distilling to remove R 2 OH and the residual solvent to obtain the heat-conducting powder modifier.
Example 2
The first vessel is preferably a four-port reaction flask, the second vessel is preferably a flask, R 2 OH is preferably n-decanol, the solvent is preferably water, the catalyst is preferably KOH, and Vi-Si- (OR 1)3) is preferably vinyltriethoxysilane.
A preparation method of a heat conducting powder modifier comprises the following steps:
adding R 2 OH and a solvent into a first container under the protection of nitrogen, heating the first container to a first temperature of about 60 ℃, adding a catalyst while stirring at the first temperature, and stirring for about 1h.
Diluting Vi-Si- (OR 1)3 with solvent in a second container to obtain Vi-Si- (OR 1)3) solution, dropwise adding Vi-Si- (OR 1)3) solution into the first container after stirring for about 5h, and allowing transesterification reaction in the first container:
Vi-Si-(OR1)3+ R2OH←→Vi-Si-(OR2)3+ R1OH,
Obtaining Vi-Si- (OR 2)3 and R 1 OH, wherein Vi-Si- (OR 2)3) is vinyl alkoxy silane, and R 1 OH is methanol;
the first vessel after the completion of the dropwise addition of the Vi-Si- (OR 1)3) solution was warmed to a second temperature of about 130℃to allow the first vessel to be subjected to a first incubation at the second temperature for about 5 hours, and R 1 OH and a part of the solvent were distilled off by the first incubation.
Cooling the first container with the first heat preservation to about 60 ℃, then dropwise adding a monohydroxy silicone oil solution with the viscosity of 10cps into the first container for about 2 hours, and carrying out the second heat preservation for about 5 hours after the completion of dropwise adding, so that the condensation reaction can be carried out in the first container:
Vi-Si-(OR2)3+ OH-Si(CH3)2-O-[ Si(CH3)2-O]m- Si(CH3)3←→Vi-Si(OR2)2-O-Si(CH3)2-O-[ Si(CH3)2-O]mSi(CH3)3, Wherein OH-Si (CH 3)2-O-[ Si(CH3)2-O]m- Si(CH3)3 refers to the monohydroxy silicone oil, and the obtained Vi-Si(OR2)2-O-Si(CH3)2-O-[ Si(CH3)2-O]mSi(CH3)3,Vi-Si(OR2)2-O-Si(CH3)2-O-[ Si(CH3)2-O]mSi(CH3)3 is vinyl long-chain alkoxy silane containing siloxane chain segments.
And heating the first container after the second heat preservation to about 130 ℃, and distilling to remove R 2 OH and the residual solvent to obtain the heat-conducting powder modifier.
Example 3
The first container is preferably a four-port reaction flask, the second container is preferably a flask, R 2 OH is preferably n-dodecanol, the solvent is preferably water, the catalyst is preferably NaOH, and Vi-Si- (OR 1)3) is preferably vinyltrimethoxysilane.
A preparation method of a heat conducting powder modifier comprises the following steps:
adding R 2 OH and a solvent into a first container under the protection of nitrogen, heating the first container to a first temperature of about 60 ℃, adding a catalyst while stirring at the first temperature, and stirring for about 1h.
Diluting Vi-Si- (OR 1)3) with a solvent in a second container to obtain Vi-Si- (OR 1)3) solution, dropwise adding the Vi-Si- (OR 1)3) solution into the first container after stirring is finished, wherein the dropwise adding time is about 2h, and enabling transesterification reaction to be carried out in the first container:
Vi-Si-(OR1)3+ R2OH←→Vi-Si-(OR2)3+ R1OH,
Obtaining Vi-Si- (OR 2)3 and R 1 OH, wherein Vi-Si- (OR 2)3) is vinyl alkoxy silane, and R 1 OH is methanol;
The first vessel after the completion of the dropwise addition of the Vi-Si- (OR 1)3) solution was warmed to a second temperature of about 110℃to allow the first vessel to be subjected to a first incubation at the second temperature for about 4 hours, and R 1 OH and a part of the solvent were distilled off by the first incubation.
Cooling the first container with the first heat preservation to about 60 ℃, then dropwise adding a monohydroxy silicone oil solution with the viscosity of 30cps into the first container for about 2 hours, and carrying out the second heat preservation for about 4 hours after the completion of dropwise adding, so that the condensation reaction can be carried out in the first container:
Vi-Si-(OR2)3+ OH-Si(CH3)2-O-[ Si(CH3)2-O]m- Si(CH3)3←→Vi-Si(OR2)2-O-Si(CH3)2-O-[ Si(CH3)2-O]mSi(CH3)3, Wherein OH-Si (CH 3)2-O-[ Si(CH3)2-O]m- Si(CH3)3 refers to the monohydroxy silicone oil, and the obtained Vi-Si(OR2)2-O-Si(CH3)2-O-[ Si(CH3)2-O]mSi(CH3)3,Vi-Si(OR2)2-O-Si(CH3)2-O-[ Si(CH3)2-O]mSi(CH3)3 is vinyl long-chain alkoxy silane containing siloxane chain segments.
And heating the first container after the second heat preservation to about 110 ℃, and distilling to remove R 2 OH and the residual solvent to obtain the heat-conducting powder modifier.
Example 4
The first container is preferably a four-port reaction flask, the second container is preferably a flask, R 2 OH is preferably n-octanol, the solvent is preferably water, the catalyst is preferably KOH, and Vi-Si- (OR 1)3) is preferably vinyltriethoxysilane.
A preparation method of a heat conducting powder modifier comprises the following steps:
adding R 2 OH and a solvent into a first container under the protection of nitrogen, heating the first container to a first temperature of about 60 ℃, adding a catalyst while stirring at the first temperature, and stirring for about 1h.
Diluting Vi-Si- (OR 1)3 with solvent in a second container to obtain Vi-Si- (OR 1)3) solution, dropwise adding Vi-Si- (OR 1)3) solution into the first container after stirring for about 5h, and allowing transesterification reaction in the first container:
Vi-Si-(OR1)3+ R2OH←→Vi-Si-(OR2)3+ R1OH,
Obtaining Vi-Si- (OR 2)3 and R 1 OH, wherein Vi-Si- (OR 2)3) is vinyl alkoxy silane, and R 1 OH is methanol;
the first vessel after the completion of the dropwise addition of the Vi-Si- (OR 1)3) solution was warmed to a second temperature of about 130℃to allow the first vessel to be subjected to a first incubation at the second temperature for about 5 hours, and R 1 OH and a part of the solvent were distilled off by the first incubation.
Cooling the first container with the first heat preservation to about 60 ℃, then dropwise adding a monohydroxy silicone oil solution with the viscosity of 50cps into the first container for about 2 hours, and carrying out the second heat preservation for about 5 hours after the dropwise adding, so that the condensation reaction can be carried out in the first container:
Vi-Si-(OR2)3+ OH-Si(CH3)2-O-[ Si(CH3)2-O]m- Si(CH3)3←→Vi-Si(OR2)2-O-Si(CH3)2-O-[ Si(CH3)2-O]mSi(CH3)3,
Wherein OH-Si (CH 3)2-O-[ Si(CH3)2-O]m- Si(CH3)3 refers to the monohydroxy silicone oil, and the obtained Vi-Si(OR2)2-O-Si(CH3)2-O-[ Si(CH3)2-O]mSi(CH3)3,Vi-Si(OR2)2-O-Si(CH3)2-O-[ Si(CH3)2-O]mSi(CH3)3 is vinyl long-chain alkoxy silane containing siloxane chain segments.
And heating the first container after the second heat preservation to about 130 ℃, and distilling to remove R 2 OH and the residual solvent to obtain the heat-conducting powder modifier.
Example 5
The heat-conducting powder modifier obtained by the preparation method of the heat-conducting powder modifier disclosed in the embodiments 1-4 contains vinyl long-chain alkoxysilane with siloxane chain units, and can be applied to the preparation of heat-conducting pouring sealants.
The heat-conducting powder modifiers obtained in examples 1-4 can be applied to the following heat-conducting pouring sealant formulations.
The formula of the heat-conducting pouring sealant comprises a component A and a component B which are respectively and independently stored.
The component A comprises 45-55 parts by weight of vinyl silicone oil, 540-560 parts by weight of heat conducting powder, 4-6 parts by weight of heat conducting powder modifier and 1.5-2.5 parts by weight of catalyst. Preferably, the vinyl silicone oil is preferably 50 parts by weight, the heat conductive powder is preferably 550 parts by weight, the heat conductive powder modifier is preferably 5 parts by weight, and the catalyst is preferably 2 parts by weight.
The component B comprises 45-55 parts by weight of vinyl silicone oil, 5-7 parts by weight of hydrogen-containing silicone oil, 540-560 parts by weight of heat conducting powder, 4-6 parts by weight of heat conducting powder modifier and 0.8-1.2 parts by weight of inhibitor. Preferably, the vinyl silicone oil is preferably 50 parts by weight, the hydrogen-containing silicone oil is preferably 6 parts by weight, the heat conductive powder is preferably 550 parts by weight, the heat conductive powder modifier is preferably 5 parts by weight, and the inhibitor is preferably 1 part by weight.
And mixing the component A and the component B according to the weight ratio of 0.8-1.2:0.8-1.2, and curing for 30min and above at 70-90 ℃. Preferably, component A and component B are mixed in a 1:1 weight ratio and cured at 80℃for 30min.
Example 6
The heat-conducting pouring sealant obtained by applying the heat-conducting powder modifier prepared in the examples 1-4 to the formula of the heat-conducting pouring sealant disclosed in the example 5 is subjected to performance test respectively.
The heat conductive potting adhesive obtained by the formulation disclosed in the following comparative example was also subjected to performance test, respectively.
Comparative example 1
The comparative example provides a heat-conducting pouring sealant formulation comprising a component A and a component B which are stored independently.
The component A contains 50 parts by weight of vinyl silicone oil, 550 parts by weight of heat conducting powder, 5 parts by weight of commercially available heat conducting powder modifier KH560 (the main component is gamma-glycidoxypropyl trimethoxysilane) and 2 parts by weight of catalyst.
The component B contains 50 parts by weight of vinyl silicone oil, 6 parts by weight of hydrogen-containing silicone oil, 550 parts by weight of heat conducting powder, 5 parts by weight of commercially available heat conducting powder modifier KH560 (the main component is gamma-glycidoxypropyl trimethoxysilane) and 1 part by weight of inhibitor.
After mixing component A and component B in a 1:1 weight ratio, curing was carried out at 80℃for 30min.
Comparative example 2
The comparative example provides a heat-conducting pouring sealant formulation comprising a component A and a component B which are stored independently.
The component A contains 50 parts by weight of vinyl silicone oil, 550 parts by weight of heat conducting powder, 5 parts by weight of commercially available heat conducting powder modifier A-171 (the main component is vinyl trimethoxy silane) and 2 parts by weight of catalyst.
The component B contains 50 parts by weight of vinyl silicone oil, 6 parts by weight of hydrogen-containing silicone oil, 550 parts by weight of heat conducting powder, 5 parts by weight of commercial heat conducting powder modifier A-171 and 1 part by weight of inhibitor.
After mixing component A and component B in a 1:1 weight ratio, curing was carried out at 80℃for 30min.
The above test results are collated in table 1 below.
Table 1 test results
As can be seen from the test results of table 1,
The heat-conducting powder modifier which is obtained by the method disclosed in the embodiments 1-4 and can be suitable for modification of heat-conducting powder can be effectively applied to manufacturing of heat-conducting pouring sealant, the viscosity of the heat-conducting pouring sealant manufactured by the heat-conducting powder modifier is effectively reduced, the heat-conducting heat-radiating performance of the heat-conducting pouring sealant is improved, the dielectric constant of the heat-conducting pouring sealant is reduced, the occurrence of sedimentation and hardening of the heat-conducting powder in the heat-conducting pouring sealant is slowed down, and therefore the storage stability of the heat-conducting pouring sealant is improved.
What has been described above is merely some embodiments of the present utility model. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit of the utility model.

Claims (6)

1.一种导热粉体改性剂，其特征在于，包括含有硅氧烷链节的乙烯基长链烷氧基硅烷，1. A thermally conductive powder modifier, characterized in that it comprises a vinyl long-chain alkoxysilane containing a siloxane chain segment, 所述导热粉体改性剂的制备方法，其特征在于，包括以下步骤：The preparation method of the thermally conductive powder modifier is characterized by comprising the following steps: 以乙烯基三甲氧基硅烷或乙烯基三乙氧基硅烷为底物，通过酯交换反应合成出乙烯基烷氧基硅烷，Vinyl alkoxysilane is synthesized by transesterification reaction using vinyl trimethoxysilane or vinyl triethoxysilane as substrate. 将R2OH和溶剂在氮气保护下加入到第一容器中，对所述第一容器进行加热，升温至第一温度，所述第一温度为50℃~80℃，在所述第一温度下边搅拌边加入催化剂，所述搅拌时间为0.5h~1h；Add R 2 OH and solvent into a first container under nitrogen protection, heat the first container to a first temperature of 50° C. to 80° C., add a catalyst while stirring at the first temperature, and the stirring time is 0.5 h to 1 h; 将Vi-Si-(OR1) 3于第二容器中用溶剂稀释，获得Vi-Si-(OR1) 3溶液，滴加所述Vi-Si-(OR1) 3溶液到搅拌结束后的第一容器中，滴加时间为3h~10h，使第一容器内能进行酯交换反应：Dilute Vi-Si-(OR 1 ) 3 with a solvent in a second container to obtain a Vi-Si-(OR 1 ) 3 solution, and dropwise add the Vi-Si-(OR 1 ) 3 solution into the first container after stirring for 3 h to 10 h, so that the first container can undergo an ester exchange reaction: Vi-Si-(OR1) 3 + R2OH←→Vi-Si-(OR2) 3 + R1OH，Vi-Si-(OR 1 ) 3 + R 2 OH←→Vi-Si-(OR 2 ) 3 + R 1 OH, 获得Vi-Si-(OR2) 3和R1OH，所述Vi-Si-(OR1) 3为乙烯基三甲氧基硅烷或乙烯基三乙氧基硅烷，所述R2OH为正癸醇、正十二醇或者正辛醇，所述Vi-Si-(OR2) 3为乙烯基烷氧基硅烷；Obtaining Vi-Si-(OR 2 ) 3 and R 1 OH, wherein the Vi-Si-(OR 1 ) 3 is vinyl trimethoxy silane or vinyl triethoxy silane, the R 2 OH is n-decanol, n-dodecyl alcohol or n-octanol, and the Vi-Si-(OR 2 ) 3 is vinyl alkoxy silane; 通过单羟基硅油和所述乙烯基烷氧基硅烷的缩合反应得到含有硅氧烷链节的乙烯基长链烷氧基硅烷，A vinyl long-chain alkoxysilane containing a siloxane segment is obtained by a condensation reaction of monohydroxy silicone oil and the vinyl alkoxysilane. 将滴加Vi-Si-(OR1) 3溶液结束后的所述第一容器升温至第二温度，所述第二温度为100℃~120℃，使所述第一容器在第二温度进行2h~5h的第一次保温，蒸出R1OH和部分溶剂，After the addition of the Vi-Si-(OR 1 ) 3 solution is completed, the temperature of the first container is raised to a second temperature of 100° C. to 120° C. The first container is kept at the second temperature for 2 h to 5 h to evaporate R 1 OH and part of the solvent. 将第一次保温结束的所述第一容器降温至50℃~70℃，之后于所述第一容器内滴加单羟基硅油溶液，滴加时间为1h~2h，滴加完成后进行2h~5h的第二次保温，使第一容器内能进行缩合反应：After the first heat preservation, the first container is cooled to 50°C-70°C, and then the monohydroxy silicone oil solution is added dropwise to the first container for 1h-2h. After the addition, a second heat preservation is performed for 2h-5h to allow the condensation reaction to proceed in the first container: Vi-Si-(OR2)3+OH-Si(CH3)2-O-[Si(CH3)2-O]m-Si(CH3)3←→Vi-Si(OR2)2-O-Si(CH3)2-O-[Si(CH3)2-O]mSi(CH3) 3，Vi-Si-(OR 2 ) 3 +OH-Si(CH 3 ) 2 -O-[Si(CH 3 ) 2 -O] m -Si(CH 3 ) 3 ←→Vi-Si(OR 2 ) 2 - O-Si(CH 3 ) 2 -O-[Si(CH 3 ) 2 -O] m Si(CH 3 ) 3 , 获得Vi-Si(OR2) 2-O-Si(CH3)2-O-[Si(CH3) 2-O]mSi(CH3) 3，所述OH-Si(CH3) 2-O-[Si(CH3) 2-O] m-Si(CH3) 3为单羟基硅油，所述Vi-Si(OR2) 2-O-Si(CH3)2-O-[Si(CH3) 2-O] mSi(CH3) 3为含有硅氧烷链节的乙烯基长链烷氧基硅烷；Obtaining Vi-Si(OR 2 ) 2 -O-Si(CH 3 ) 2 -O-[Si(CH 3 ) 2 -O] m Si(CH 3 ) 3 , wherein the OH-Si(CH 3 ) 2 -O-[Si(CH 3 ) 2 -O] m -Si(CH 3 ) 3 is a monohydroxy silicone oil, and the Vi-Si(OR 2 ) 2 -O-Si(CH 3 ) 2 -O-[Si(CH 3 ) 2 -O] m Si(CH 3 ) 3 is a vinyl long-chain alkoxysilane containing a siloxane chain segment; 将第二次保温结束后的所述第一容器升温至110℃~130℃，蒸馏去除R2OH和剩余溶剂，得到导热粉体改性剂。After the second heat preservation, the first container is heated to 110° C. to 130° C., and R 2 OH and the remaining solvent are distilled off to obtain a thermally conductive powder modifier. 2. 根据权利要求1所述的一种导热粉体改性剂，其特征在于， 所述催化剂为碱性材料。2. A thermally conductive powder modifier according to claim 1, characterized in that the catalyst is an alkaline material. 3.根据权利要求1所述的一种导热粉体改性剂，其特征在于，所述R1OH为甲醇。The thermally conductive powder modifier according to claim 1 , wherein the R 1 OH is methanol. 4.根据权利要求1所述的一种导热粉体改性剂，其特征在于，所述单羟基硅油的粘度为10cps~50cps。4. A thermally conductive powder modifier according to claim 1, characterized in that the viscosity of the monohydroxy silicone oil is 10cps~50cps. 5.一种导热灌封胶，其特征在于，应用了权利要求1所述的导热粉体改性剂。5. A thermally conductive potting adhesive, characterized in that the thermally conductive powder modifier according to claim 1 is used. 6.根据权利要求5所述的一种导热灌封胶，其特征在于，所述导热灌封胶的配方包括组分A和组分B，6. The thermally conductive potting adhesive according to claim 5, characterized in that the formula of the thermally conductive potting adhesive comprises component A and component B, 所述组分A包括45~55重量份的乙烯基硅油、540~560重量份的导热粉体、4~6重量份的所述导热粉体改性剂和1.5~2.5重量份的催化剂；The component A comprises 45 to 55 parts by weight of vinyl silicone oil, 540 to 560 parts by weight of thermally conductive powder, 4 to 6 parts by weight of the thermally conductive powder modifier and 1.5 to 2.5 parts by weight of a catalyst; 所述组分B包括45~55重量份的乙烯基硅油、5~7重量份的含氢硅油、540~560重量份的导热粉体、4~6重量份的所述导热粉体改性剂和0.8~1.2重量份的抑制剂；The component B comprises 45-55 parts by weight of vinyl silicone oil, 5-7 parts by weight of hydrogenated silicone oil, 540-560 parts by weight of thermally conductive powder, 4-6 parts by weight of the thermally conductive powder modifier and 0.8-1.2 parts by weight of an inhibitor; 所述组分A和组分B按照0.8~1.2:0.8~1.2重量比混合，在70~90℃固化30min及以上。The component A and the component B are mixed in a weight ratio of 0.8-1.2:0.8-1.2 and cured at 70-90° C. for 30 minutes or more.
CN202310123842.5A 2023-02-16 2023-02-16 A thermally conductive powder modifier and preparation method thereof and thermally conductive potting glue Active CN116253885B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310123842.5A CN116253885B (en) 2023-02-16 2023-02-16 A thermally conductive powder modifier and preparation method thereof and thermally conductive potting glue

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310123842.5A CN116253885B (en) 2023-02-16 2023-02-16 A thermally conductive powder modifier and preparation method thereof and thermally conductive potting glue

Publications (2)

Publication Number Publication Date
CN116253885A CN116253885A (en) 2023-06-13
CN116253885B true CN116253885B (en) 2024-12-10

Family

ID=86682143

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202310123842.5A Active CN116253885B (en) 2023-02-16 2023-02-16 A thermally conductive powder modifier and preparation method thereof and thermally conductive potting glue

Country Status (1)

Country Link
CN (1) CN116253885B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117986589A (en) * 2023-12-27 2024-05-07 广东鼎立森新材料有限公司 Modifier for thermally conductive powder and preparation method thereof, electronic potting glue and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103102689A (en) * 2011-11-15 2013-05-15 佛山市金戈消防材料有限公司 Organic-silicon pouring sealant composition with high thermal conductivity and application thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6011087A (en) * 1997-12-22 2000-01-04 J.M. Huber Corporation Modified mineral filler for thermosets
CN103706332B (en) * 2013-12-30 2016-04-20 同济大学 A kind of bamboo charcoal modified method that can be applicable to oiliness sewage treatment

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103102689A (en) * 2011-11-15 2013-05-15 佛山市金戈消防材料有限公司 Organic-silicon pouring sealant composition with high thermal conductivity and application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
光固化3D打印技术制备SiOC陶瓷及其衍生物;马聪;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20230215(第2期);B015-1705 *
马聪.光固化3D打印技术制备SiOC陶瓷及其衍生物.《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》.2023,(第2期),B015-1705. *

Also Published As

Publication number Publication date
CN116253885A (en) 2023-06-13

Similar Documents

Publication Publication Date Title
CN112608480B (en) Asymmetric silicone oil and preparation method and application thereof
CN116253885B (en) A thermally conductive powder modifier and preparation method thereof and thermally conductive potting glue
CN107312495A (en) A kind of tack high-temperature silicon disulfide rubber band and preparation method thereof
CN110564363A (en) low-viscosity high-heat-conductivity bonding pouring sealant and preparation method thereof
CN110982277B (en) Single-component temperature-resistant heat-conducting silicon mud composition and preparation method thereof
CN116589973B (en) High-temperature-resistant COB packaging adhesive and preparation method thereof
CN110938406A (en) Bi-component organic silicon pouring sealant and preparation method thereof
CN115322721B (en) Room-temperature-cured epoxy heat-conducting adhesive for lithium battery, heat-conducting shell and preparation method of heat-conducting shell
CN103540289B (en) Preparation method and application of organic silicon resin adhesive
CN113185947A (en) Mixed crosslinking system two-component hollow sealant
CN113402850A (en) Low-dielectric-constant and low-warpage epoxy plastic packaging material composition, preparation and application
CN114774074A (en) UV-cured heat-conducting silica gel composition
CN116355419A (en) Low-viscosity high-heat-conductivity silicone grease and preparation method and application thereof
CN114045036B (en) Heat-conducting gel composition and preparation method thereof
JP2009249312A (en) Silane compound
CN104530713A (en) Heat-conducting silicone grease
CN113773503B (en) Boron-containing organic silicon tackifier and preparation method and application thereof
CN104558611A (en) MDTQ silicon resin, as well as preparation method and application thereof
CN111777941B (en) Curable organic silicon composition and preparation method and application thereof
CN117384584B (en) Double-component heat-conducting pouring sealant for OBC charging module and preparation method thereof
CN104530714A (en) Heat-conducting silicone grease composition
CN116355422B (en) A curable resin composition and its preparation method and application
CN115216269B (en) Single-component organic silicon pouring sealant and preparation method thereof
CN106752701A (en) A kind of electrostatic spraying coating containing modified carbon nano-tube
CN113999647B (en) Organic silicon pouring sealant and preparation method thereof

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