CN110317562A - A kind of organic-silicon-modified epoxy pouring sealant - Google Patents
A kind of organic-silicon-modified epoxy pouring sealant Download PDFInfo
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- CN110317562A CN110317562A CN201910537062.9A CN201910537062A CN110317562A CN 110317562 A CN110317562 A CN 110317562A CN 201910537062 A CN201910537062 A CN 201910537062A CN 110317562 A CN110317562 A CN 110317562A
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- glue
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- thermally conductive
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- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/14—Polycondensates modified by chemical after-treatment
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- 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
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
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- 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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- 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
- C09J183/10—Block or graft copolymers containing polysiloxane sequences
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The present invention relates to a kind of organic-silicon-modified epoxy pouring sealants, are directed to epoxy resin CGY-331 and the lesser resin of both relative viscosities of epoxy resin VE-2025, are modified using thermally conductive silicone oil and hydroxyl silicon rubber to it.It is modified to solve the problems such as epoxy pouring sealant poor in flexibility, temperature tolerance difference and bad organic silicon potting adhesive intensity, the two advantage is combined well.Due to having selected the lesser epoxy resin of viscosity, the heat filling largely compounded can be added, keeps casting glue product itself bulk density high, heat conduction network can be effectively increased, further increase thermal conductivity.Modified epoxy glue cocoa does the thermally conductive casting glue of one-component, can also do the thermally conductive casting glue of two-component, have a wide range of application.
Description
Technical field
The present invention relates to casting glue technical fields, and in particular to a kind of organic-silicon-modified epoxy pouring sealant.
Background technique
Domestic and international market mostly uses epoxy resin embedding adhesive and organic silicon potting adhesive, but both products are each have their own
Deficiency, epoxy resin has excellent adhesion energy, electrical insulation capability and mobility, but epoxy resin is more crisp, and flexibility is poor, and
Temperature tolerance is poor, and epoxy resin used in prior art insulation encapsulated glue is bisphenol-A series, and viscosity is relatively large,
More heat fillings cannot be added to improve the thermal coefficient of product.Organic siliconresin temperature tolerance with higher and preferably
Flexibility and weatherability, but be lacking in terms of adhesive strength.
Summary of the invention
The object of the present invention is to provide a kind of organic-silicon-modified epoxy pouring sealants, and the casting glue includes curing agent and base
Plinth glue, the basis glue are prepared by the raw material of following parts by weight:
The viscosity for the above two epoxy resin that the present invention selects is relatively small, not only can be preferably mixed with modified silicon oil
It closes, can also be achieved and more filler is added, such as 200~240 parts of hexagonal boron nitrides, be conducive to improve thermal conductivity.And the present invention makes
Make casting glue product itself heap if hexagonal boron nitride, ZnO whisker and carbon nanotube are used in mixed way with the heat filling of compounding
Product density is high, can effectively increase heat conduction network, further increase thermal conductivity.The basic glue of above-mentioned formula has preferable bonding
Property, toughness and temperature tolerance, not only can be prepared into casting glue described herein, can also be further prepared into heat-conducting glue, magnetic-conductive adhesive,
Conducting resinl etc..
Preferably, the thermally conductive silicone oil is low-viscosity hydroxyl-terminated injecting two methyl siloxane；
It is further preferred that the viscosity of the silicone oil is 80~1000mPa.s.
Preferably, the hydroxyl silicon rubber is 107 silicon rubber of low-viscosity；
It is further preferred that the viscosity of the silicon rubber is 1800~2200mPa.s.
Preferably, the basic glue is prepared by the following method:
1) epoxy resin CGY-331 and epoxy resin VE-2025 is added in a kettle, is uniformly mixed, by thermally conductive silicone oil
It is uniformly mixed, and is added in reaction kettle with hydroxyl silicon rubber, nitrogen is filled with into reaction kettle, is displaced in reaction kettle
Air, reaction kettle is warming up to 115~125 DEG C, dehydration is carried out, obtains performed polymer；
2) hexagonal boron nitride, ZnO whisker and carbon nanotube are added in Xiang Suoshu performed polymer, are carried out in high speed disperser high
Speed dispersion keeps filler dispersion uniform enough, obtains basic glue.
The reaction mechanism of modifying epoxy resin by organosilicon of the present invention are as follows:
Preferably, the application also provides the one pack system casting glue including herein described basic glue, i.e., in the basic glue
In directly add latent curing agent；
It is further preferred that by weight, the resting form solid formulation includes 15~20 parts of dicyandiamide, ZJ-1 promotor
6~10 parts.ZJ-1 promotor function admirable, can solidify at different temperatures, can be good at controlling curing time and solidification temperature
Degree.Dicyandiamide is latent curing agent, and activity is small under room temperature, and the crosslinking reaction may not occur with epoxy resin, can be improved under high temperature
Activity reacts realization solidification with cross linking of epoxy resin.
It is further preferred that the ZJ-1 promotor is mixed to get by DMP-30 and methylimidazole 1:1 in mass ratio.
Preferably, the application also supplies the application method of this one pack system casting glue, the steps include: for the casting glue to be placed in
At 115~125 DEG C, solidification is completed in 1~3h.
Preferably, the application also provides the bi-component casting glue including herein described basic glue, that is, provides and the base
The curing agent that plinth glue independently uses,
It is further preferred that by weight, the curing agent independently used includes 100~120 parts of modified firming agent, idol
5~10 parts of agent KH-550 of connection.
It is further preferred that the modified firming agent is prepared by the following method.
1) 660 diluent of epoxy is added dropwise after triethylene tetramine being heated to 35 DEG C, temperature must not exceed 60 during dropwise addition
DEG C, it is added dropwise within 2~3h；
2) addition methylimidazole mixes to as clear as crystal after being cooled to 48~52 DEG C, adds DMP-30 mixing and stirs
Mix uniformly to get；
Preferably, by weight, the additive amount of the triethylene tetramine is 20~25 parts, the addition of 660 diluent of epoxy
Amount is 72~28 parts, and the additive amount of DMP-30 is 3~5 parts, and the additive amount of 4.28g methylimidazole is 5~6 parts.
Preferably, the application also provides the application method of herein described bi-component casting glue, the steps include: the base
Plinth glue and the curing agent independently used the 3:1 in mass ratio are uniformly mixed, and 4~6h realizes just solidification under room temperature.
Epoxy pouring sealant of the present invention has the following beneficial effects:
1) present invention solves epoxy pouring sealant poor in flexibility, and temperature tolerance difference and organic silicon potting adhesive intensity are bad etc. asks
Topic combines the two advantage well；
2) the basic glue of the application carries out vacuum heating treatment to epoxy and organic siliconresin during preparation, this
Modified chemical reaction can both occur for a process, can also remove the volatile matter in resin, keep film layer after solidification finer and close, thus
With good thermally conductive and insulation effect, there can be more preferably comprehensive performance preferably in conjunction with the advantages of two kinds of materials.
3) present invention selects answering for several heat filling (ZnO whisker, boron nitride and carbon nanotube being micron-level particle size)
Match, make the large bulk density of casting glue, than great, can further improve the thermal conductivity and mechanical strength of product.
4) present invention employs nano materials, and (ZnO whisker, boron nitride and carbon nanotube are micron order grain with micro materials
Diameter) it compounds and is improved, resulting basis glue can do the thermally conductive casting glue of one-component, can also do the thermally conductive casting glue of two-component.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
The present embodiment is related to basic glue described herein, prepares raw material are as follows:
Preparation method includes the following steps:
1) epoxy resin CGY-331 and epoxy resin VE-2025 is added in a kettle, is uniformly mixed, by thermally conductive silicone oil
It is uniformly mixed, and is added in reaction kettle with hydroxyl silicon rubber, nitrogen is filled with into reaction kettle, is displaced in reaction kettle
Air, reaction kettle is warming up to 120 DEG C, glue is carried out and reacts 4~5h, obtain performed polymer；
2) room temperature addition hexagonal boron nitride, ZnO whisker and carbon nanotube in Xiang Suoshu performed polymer, carry out high speed dispersion, obtain
Basic glue.
Embodiment 2
The present embodiment is related to a kind of basic glue described herein, prepares raw material are as follows:
Preparation method includes the following steps:
1) epoxy resin CGY-331 and epoxy resin VE-2025 is added in a kettle, is uniformly mixed, by thermally conductive silicone oil
It is uniformly mixed, and is added in reaction kettle with hydroxyl silicon rubber, nitrogen is filled with into reaction kettle, is displaced in reaction kettle
Air, reaction kettle is warming up to 120 DEG C, 4~5h of polymerization reaction is carried out, obtains performed polymer；
2) hexagonal boron nitride, ZnO whisker and carbon nanotube are added in Xiang Suoshu performed polymer, are carried out high speed dispersion, are obtained basic
Glue；
Embodiment 3
The present embodiment is related to a kind of basic glue described herein, prepares raw material are as follows:
Preparation method includes the following steps:
1) epoxy resin CGY-331 and epoxy resin VE-2025 is added in a kettle, is uniformly mixed, by thermally conductive silicone oil
It is uniformly mixed, and is added in reaction kettle with hydroxyl silicon rubber, nitrogen is filled with into reaction kettle, is displaced in reaction kettle
Air, reaction kettle is warming up to 120 DEG C, 4~5h of polymerization reaction is carried out, obtains performed polymer；
2) hexagonal boron nitride, ZnO whisker and carbon nanotube are added in Xiang Suoshu performed polymer, are carried out high speed dispersion, are obtained basic
Glue.
Embodiment 4
The present embodiment is related to a kind of one-component casting glue, adds latent curing agent in basic glue described in embodiment 3:
Dicyandiamide 20g, ZJ-1 promotor 8g.
The application method of this one pack system casting glue are as follows: the casting glue is warming up to 120 DEG C, is completed in 1~3h solid
Change.
Embodiment 5
The present embodiment is related to a kind of one pack system casting glue, adds latent curing agent in basic glue described in embodiment 1:
Dicyandiamide 20g, ZJ-1 promotor 10g.
The application method of this one pack system casting glue are as follows: the casting glue is warming up to 120 DEG C, is completed in 1~3h solid
Change.
Embodiment 6
The present embodiment is related to a kind of one pack system casting glue, adds latent curing agent in basic glue as described in example 2:
Dicyandiamide 20g, ZJ-1 promotor 6g.
The application method of this one pack system casting glue are as follows: the casting glue is warming up to 120 DEG C, is completed in 1~3h solid
Change.
Embodiment 7
The present embodiment is related to a kind of two-component casting glue, the curing agent independently used are as follows: modified firming agent 100g, coupling agent
KH-550 5g。
The application method of this two-component casting glue are as follows:
In use, the curing agent 3:1 in mass ratio independently used in basis glue described in embodiment 3 and the present embodiment is mixed
It closes uniformly, 4~6h realizes just solidification under room temperature.
Embodiment 8
The present embodiment is related to a kind of two-component casting glue, the curing agent independently used are as follows: modified firming agent 100g, coupling agent
KH-550 10g。
The application method of this two-component casting glue are as follows:
In use, the curing agent 3:1 in mass ratio independently used in basis glue described in embodiment 1 and the present embodiment is mixed
It closes uniformly, 4~6h realizes just solidification under room temperature.
Embodiment 9
The present embodiment is related to a kind of two-component casting glue, the curing agent independently used are as follows: modified firming agent 100g, coupling agent
KH-550 10g。
The application method of this two-component casting glue are as follows:
In use, the curing agent 3:1 in mass ratio independently used in basis glue described in embodiment 2 and the present embodiment is mixed
It closes uniformly, 4~6h realizes just solidification under room temperature.
Comparative example 1
Compared with Example 4, difference is, organosilicon is not had in the basic glue and is modified to epoxy, epoxy
The dosage of resin and other raw materials remains unchanged.
Comparative example 2
Compared with Example 4, difference is, the filler is Al2O3For heat filling.The present embodiment is finally formed
The heat conduction network of product is not fine and close, and thermal coefficient can accordingly decline, and corresponding shear strength can also decline.
Comparative example 3
Compared with Example 4, difference is, embodiment 3 is directly direct by each raw material during preparing basic glue
Mixing.In the present embodiment mixed process, the compatibility of thermally conductive silicone oil and silicon rubber and epoxy resin is poor, is easy to appear unevenness
Even phenomenon cannot have larger impact to properties of product well by epoxy in conjunction with the advantages of silicone oil silicon rubber.
Experimental example
The performance of herein described casting glue see the table below:
Although above having used general explanation, specific embodiment and test, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (10)
1. a kind of organic-silicon-modified epoxy pouring sealant, which is characterized in that including basic glue, the basis glue is by following parts by weight
Raw material be prepared:
2. casting glue according to claim 1, which is characterized in that the thermally conductive silicone oil is low-viscosity terminal hydroxy group poly dimethyl
Siloxanes, it is preferred that the viscosity of the thermally conductive silicone oil is 80~1000mPa.s.
3. casting glue according to claim 1, which is characterized in that the hydroxyl silicon rubber is 107 silicon rubber of low-viscosity,
Preferably, the viscosity of 107 silicon rubber of low-viscosity is 1800~2200mPa.s.
4. described in any item casting glues according to claim 1~3, which is characterized in that its basic glue prepare by the following method and
At:
1) epoxy resin CGY-331 and epoxy resin VE-2025 is added in a kettle, is uniformly mixed, by thermally conductive silicone oil and contains
Hydroxyl silicon rubber is uniformly mixed, and is added in reaction kettle, and nitrogen is filled with into reaction kettle, displaces the sky in reaction kettle
Reaction kettle is warming up to 115~125 DEG C, carries out dehydration, obtain performed polymer by gas；
2) hexagonal boron nitride, ZnO whisker and carbon nanotube are added in Xiang Suoshu performed polymer, and high speed point is carried out in high speed disperser
It dissipates, keeps filler dispersion uniform enough, obtain basic glue.
5. casting glue according to any one of claims 1 to 4, which is characterized in that further include directly mixed with the basic glue
Close the latent curing agent used；Preferably, by weight, the resting form solid formulation includes 15~20 parts of dicyandiamide, ZJ-
1 6~10 parts of promotor.
6. casting glue according to claim 5, which is characterized in that the ZJ-1 promotor by DMP-30 and dimethyl miaow
Azoles 1:1 in mass ratio is mixed to get.
7. the application method of the casting glue of claim 6 or 7, which is characterized in that the casting glue is placed in 115~125 DEG C
Under, solidification is completed in 1~3h.
8. casting glue according to any one of claims 1 to 4, which is characterized in that further include independently making with the basic glue
Curing agent, it is preferred that by weight, the curing agent independently used includes 100~120 parts of modified firming agent, coupling
5~10 parts of agent KH-550.
9. casting glue according to claim 8, which is characterized in that the modified firming agent is prepared by the following method:
1) 660 diluent of epoxy is added dropwise after triethylene tetramine being heated to 35 DEG C, temperature must not exceed 60 DEG C during dropwise addition, and 2
It is added dropwise within~3h；
2) addition methylimidazole mixes to as clear as crystal after being cooled to 48~52 DEG C, adds DMP-30 and is mixed
It is even to get；
Preferably, by weight, the additive amount of the triethylene tetramine is 20~25 parts, and the additive amount of 660 diluent of epoxy is
72~28 parts, the additive amount of DMP-30 is 3~5 parts, and the additive amount of 4.28g methylimidazole is 5~6 parts.
10. the application method of claim 8~9 casting glue, which is characterized in that by the basic glue and the independent use
Curing agent 3:1 in mass ratio be uniformly mixed, under room temperature 4~6h realize just solidification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910537062.9A CN110317562B (en) | 2019-06-20 | 2019-06-20 | Organic silicon modified epoxy pouring sealant |
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|---|---|---|---|
| CN201910537062.9A CN110317562B (en) | 2019-06-20 | 2019-06-20 | Organic silicon modified epoxy pouring sealant |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110776849A (en) * | 2019-10-23 | 2020-02-11 | 烟台德邦科技有限公司 | Double-component high/low temperature resistant conductive adhesive and preparation method thereof |
| CN111171771A (en) * | 2020-01-20 | 2020-05-19 | 浙江华正新材料股份有限公司 | Bonding sheet and preparation method thereof |
| CN114774045A (en) * | 2022-04-24 | 2022-07-22 | 宁波西奥东升涂料系统有限公司 | Low-temperature-resistant pouring sealant and preparation method and production equipment thereof |
| CN115960569A (en) * | 2023-02-03 | 2023-04-14 | 武汉楚辰新材料科技有限公司 | Epoxy resin pouring sealant |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110776849A (en) * | 2019-10-23 | 2020-02-11 | 烟台德邦科技有限公司 | Double-component high/low temperature resistant conductive adhesive and preparation method thereof |
| CN111171771A (en) * | 2020-01-20 | 2020-05-19 | 浙江华正新材料股份有限公司 | Bonding sheet and preparation method thereof |
| CN111171771B (en) * | 2020-01-20 | 2021-11-02 | 浙江华正新材料股份有限公司 | Bonding sheet and preparation method thereof |
| CN114774045A (en) * | 2022-04-24 | 2022-07-22 | 宁波西奥东升涂料系统有限公司 | Low-temperature-resistant pouring sealant and preparation method and production equipment thereof |
| CN114774045B (en) * | 2022-04-24 | 2023-11-07 | 宁波西奥东升涂料系统有限公司 | Low-temperature-resistant pouring sealant and preparation method and production equipment thereof |
| CN115960569A (en) * | 2023-02-03 | 2023-04-14 | 武汉楚辰新材料科技有限公司 | Epoxy resin pouring sealant |
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