CN110317562B - Organic silicon modified epoxy pouring sealant - Google Patents
Organic silicon modified epoxy pouring sealant Download PDFInfo
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- CN110317562B CN110317562B CN201910537062.9A CN201910537062A CN110317562B CN 110317562 B CN110317562 B CN 110317562B CN 201910537062 A CN201910537062 A CN 201910537062A CN 110317562 B CN110317562 B CN 110317562B
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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
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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
- 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
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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
- 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)
- Epoxy Resins (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention relates to an organic silicon modified epoxy pouring sealant, which is modified by adopting heat-conducting silicone oil and hydroxyl-containing silicone rubber aiming at two types of resins with relatively low relative viscosity, namely epoxy resin CGY-331 and epoxy resin VE-2025. The problems of poor flexibility, poor temperature resistance, poor strength of the organic silicon pouring sealant and the like of the epoxy pouring sealant are solved after the modification, and the advantages of the epoxy pouring sealant and the organic silicon pouring sealant are well combined. As the epoxy resin with lower viscosity is selected, a large amount of compounded heat-conducting filler can be added, so that the stacking density of the pouring sealant product is high, a heat-conducting network can be effectively increased, and the heat conductivity is further improved. The modified epoxy glue can be used as a single-component heat-conducting pouring sealant and a double-component heat-conducting pouring sealant, and has a wide application range.
Description
Technical Field
The invention relates to the technical field of pouring sealant, in particular to an organic silicon modified epoxy pouring sealant.
Background
Epoxy resin potting adhesive and organosilicon potting adhesive are mostly used in domestic and foreign markets, but the two products have respective defects, the epoxy resin has excellent bonding property, electrical insulation property and fluidity, but the epoxy resin is brittle, poor in flexibility and poor in temperature resistance, and the epoxy resin used in the insulating potting adhesive in the prior art is bisphenol A series, so that the viscosity is relatively high, and more heat-conducting fillers cannot be added to improve the heat conductivity coefficient of the product. The organic silicon resin has higher temperature resistance, better flexibility and weather resistance, but is deficient in the aspect of bonding strength.
Disclosure of Invention
The invention aims to provide an organic silicon modified epoxy pouring sealant, which comprises a curing agent and a base adhesive, wherein the base adhesive is prepared from the following raw materials in parts by weight:
the two epoxy resins selected by the invention have relatively low viscosity, can be better mixed with modified silicone oil, can realize the addition of more fillers such as 200-240 parts of hexagonal boron nitride, and is beneficial to improving the thermal conductivity. In addition, the invention uses the compounded heat-conducting filler, such as hexagonal boron nitride, ZnO crystal whisker and carbon nano tube which are mixed for use, so that the pouring sealant product has high stacking density, a heat-conducting network can be effectively increased, and the heat conductivity is further improved. The base adhesive of the formula has good cohesiveness, toughness and temperature resistance, and can be used for preparing the pouring sealant, heat-conducting adhesive, magnetic-conducting adhesive, conductive adhesive and the like.
Preferably, the heat-conducting silicone oil is low-viscosity hydroxyl-terminated polydimethylsiloxane;
further preferably, the viscosity of the silicone oil is 80 to 1000 mPa.s.
Preferably, the hydroxyl-containing silicone rubber is low-viscosity 107 silicone rubber;
more preferably, the viscosity of the silicone rubber is 1800-2200 mPa.s.
Preferably, the base glue is prepared by the following method:
1) adding epoxy resin CGY-331 and epoxy resin VE-2025 into a reaction kettle, uniformly mixing heat-conducting silicone oil and hydroxyl-containing silicone rubber, adding the mixture into the reaction kettle, filling nitrogen into the reaction kettle, displacing air in the reaction kettle, heating the reaction kettle to 115-125 ℃, and carrying out dehydration reaction to obtain a prepolymer;
2) and adding hexagonal boron nitride, ZnO whiskers and carbon nanotubes into the prepolymer, and dispersing at a high speed in a high-speed dispersion machine to ensure that the filler is dispersed uniformly enough to obtain the base adhesive.
The reaction mechanism of the organosilicon modified epoxy resin is as follows:
preferably, the application also provides a single-component pouring sealant comprising the base glue, namely, a latent curing agent is directly added into the base glue;
further preferably, the latent solid agent comprises 15-20 parts by weight of dicyandiamide and 6-10 parts by weight of ZJ-1 accelerator. The ZJ-1 accelerant has excellent performance, can be cured at different temperatures, and can well control the curing time and the curing temperature. Dicyandiamide is a latent curing agent, has low activity at normal temperature, does not generate crosslinking reaction with epoxy resin, and can improve the activity at high temperature to realize curing through the crosslinking reaction with the epoxy resin.
Further preferably, the ZJ-1 accelerator is prepared by mixing DMP-30 and dimethyl imidazole according to the mass ratio of 1: 1.
Preferably, the application also provides a using method of the single-component pouring sealant, which comprises the following steps: and (3) placing the pouring sealant at 115-125 ℃ to finish curing within 1-3 h.
Preferably, the application also provides a two-component pouring sealant comprising the basic sealant, namely a curing agent which is independently used with the basic sealant,
further preferably, the independently used curing agent comprises 100-120 parts by weight of modified curing agent and 5-10 parts by weight of coupling agent KH-550.
Further preferably, the modified curing agent is prepared by the following method.
1) Heating triethylene tetramine to 35 ℃, and then dropwise adding an epoxy 660 diluent, wherein the temperature is not higher than 60 ℃ in the dropwise adding process, and the dropwise adding is completed within 2-3 hours;
2) cooling to 48-52 ℃, adding dimethyl imidazole, mixing and stirring until the mixture is clear and transparent, adding DMP-30, mixing and stirring uniformly to obtain the product;
preferably, the addition amount of the triethylene tetramine is 20-25 parts, the addition amount of the epoxy 660 diluent is 72-28 parts, the addition amount of the DMP-30 is 3-5 parts, and the addition amount of 4.28g of dimethyl imidazole is 5-6 parts by weight.
Preferably, the application also provides a use method of the two-component pouring sealant, which comprises the following steps: and (3) mixing the base adhesive and the independently used curing agent according to a mass ratio of 3:1, uniformly mixing, and realizing primary curing at normal temperature for 4-6 h.
The epoxy pouring sealant disclosed by the invention has the following beneficial effects:
1) the invention solves the problems of poor flexibility, poor temperature resistance, poor strength of the organic silicon pouring sealant and the like of the epoxy pouring sealant, and well combines the advantages of the epoxy pouring sealant and the organic silicon pouring sealant;
2) the base adhesive carries out vacuum heating treatment on epoxy and organic silicon resin in the preparation process, the process can carry out modified chemical reaction, volatile matters in the resin can be removed, and a cured film layer is more compact, so that the base adhesive has good heat conduction and insulation effects, can better combine the advantages of two materials, and has better comprehensive performance.
3) The invention selects the compounding of several heat-conducting fillers (ZnO crystal whisker, boron nitride and carbon nano tube are all in micron-sized grain size), so that the pouring sealant has large bulk density and large specific gravity, and can further improve the heat conductivity and mechanical strength of the product.
4) The invention adopts the compounding of nano materials and micron materials (ZnO whiskers, boron nitride and carbon nanotubes are all in micron-sized particle size) for improvement, and the obtained base adhesive can be used as a single-component heat-conducting pouring sealant or a double-component heat-conducting pouring sealant.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
The embodiment relates to a base adhesive, which is prepared from the following raw materials:
the preparation method comprises the following steps:
1) adding epoxy resin CGY-331 and epoxy resin VE-2025 into a reaction kettle, uniformly mixing heat-conducting silicone oil and hydroxyl-containing silicone rubber, adding the mixture into the reaction kettle, filling nitrogen into the reaction kettle, displacing air in the reaction kettle, heating the reaction kettle to 120 ℃, and carrying out glue reaction for 4-5 hours to obtain a prepolymer;
2) and adding hexagonal boron nitride, ZnO whiskers and carbon nanotubes into the prepolymer at normal temperature, and dispersing at high speed to obtain the base adhesive.
Example 2
The embodiment relates to a base adhesive, which is prepared from the following raw materials:
the preparation method comprises the following steps:
1) adding epoxy resin CGY-331 and epoxy resin VE-2025 into a reaction kettle, uniformly mixing heat-conducting silicone oil and hydroxyl-containing silicone rubber, adding the mixture into the reaction kettle, filling nitrogen into the reaction kettle, displacing air in the reaction kettle, heating the reaction kettle to 120 ℃, and carrying out polymerization reaction for 4-5 hours to obtain a prepolymer;
2) adding hexagonal boron nitride, ZnO whiskers and carbon nanotubes into the prepolymer, and dispersing at a high speed to obtain a base adhesive;
example 3
The embodiment relates to a base adhesive, which is prepared from the following raw materials:
the preparation method comprises the following steps:
1) adding epoxy resin CGY-331 and epoxy resin VE-2025 into a reaction kettle, uniformly mixing heat-conducting silicone oil and hydroxyl-containing silicone rubber, adding the mixture into the reaction kettle, filling nitrogen into the reaction kettle, displacing air in the reaction kettle, heating the reaction kettle to 120 ℃, and carrying out polymerization reaction for 4-5 hours to obtain a prepolymer;
2) and adding hexagonal boron nitride, ZnO whiskers and carbon nanotubes into the prepolymer, and dispersing at a high speed to obtain the base adhesive.
Example 4
The embodiment relates to a single-component pouring sealant, wherein a latent curing agent is added into a base adhesive in the embodiment 3: 20g of dicyandiamide and 8g of ZJ-1 accelerator.
The use method of the single-component pouring sealant comprises the following steps: and heating the pouring sealant to 120 ℃, and finishing curing within 1-3 h.
Example 5
The embodiment relates to a single-component pouring sealant, wherein a latent curing agent is added into the basic sealant in the embodiment 1: 20g of dicyandiamide and 10g of ZJ-1 accelerator.
The use method of the single-component pouring sealant comprises the following steps: and heating the pouring sealant to 120 ℃, and finishing curing within 1-3 h.
Example 6
The embodiment relates to a single-component pouring sealant, wherein a latent curing agent is added into the basic sealant in the embodiment 2: 20g of dicyandiamide and 6g of ZJ-1 accelerator.
The use method of the single-component pouring sealant comprises the following steps: and heating the pouring sealant to 120 ℃, and finishing curing within 1-3 h.
Example 7
The embodiment relates to a two-component pouring sealant, which comprises the following independently used curing agents: 100g of modified curing agent and KH-5505 g of coupling agent.
The use method of the two-component pouring sealant comprises the following steps:
when the adhesive is used, the base adhesive in the embodiment 3 and the independently used curing agent in the embodiment are uniformly mixed according to the mass ratio of 3:1, and primary curing is realized at normal temperature for 4-6 h.
Example 8
The embodiment relates to a two-component pouring sealant, which comprises the following independently used curing agents: 100g of modified curing agent and KH-55010 g of coupling agent.
The use method of the two-component pouring sealant comprises the following steps:
when the adhesive is used, the base adhesive in the embodiment 1 and the independently used curing agent in the embodiment are uniformly mixed according to the mass ratio of 3:1, and primary curing is realized at normal temperature for 4-6 h.
Example 9
The embodiment relates to a two-component pouring sealant, which comprises the following independently used curing agents: 100g of modified curing agent and KH-55010 g of coupling agent.
The use method of the two-component pouring sealant comprises the following steps:
when the adhesive is used, the basic adhesive in the embodiment 2 and the independently used curing agent in the embodiment are uniformly mixed according to the mass ratio of 3:1, and primary curing is realized at normal temperature for 4-6 h.
Comparative example 1
Compared with the example 4, the difference is that the base glue does not use organic silicon to modify epoxy, and the dosage of epoxy resin and other raw materials is kept unchanged.
Comparative example 2
The difference compared to example 4 is that the filler is Al2O3Is a heat conductive filler. The heat conduction network of the product finally formed by the embodiment is not compact, the heat conduction coefficient is correspondingly reduced, and the corresponding shear strength is also reduced.
Comparative example 3
The difference compared to example 4 is that example 3 directly mixes the raw materials during the process of preparing the base gum. In the mixing process of the embodiment, the compatibility of the heat-conducting silicone oil, the silicone rubber and the epoxy resin is poor, the phenomenon of non-uniformity is easy to occur, the advantages of the epoxy and the silicone oil and the silicone rubber cannot be well combined, and the product performance is greatly influenced.
Examples of the experiments
The performance of the potting adhesive is shown in the following table:
although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. The organic silicon modified epoxy pouring sealant is characterized by comprising a base adhesive, wherein the base adhesive is prepared from the following raw materials in parts by weight:
epoxy resin CGY-33180-100 parts
Epoxy resin VE-202580-100 parts
10-20 parts of heat-conducting silicone oil
3-5 parts of silicon rubber containing hydroxyl
200-240 parts of hexagonal boron nitride
2-4 parts of ZnO whisker
2-4 parts of carbon nanotubes;
the epoxy pouring sealant is prepared by the following method:
1) adding epoxy resin CGY-331 and epoxy resin VE-2025 into a reaction kettle, uniformly mixing heat-conducting silicone oil and hydroxyl-containing silicone rubber, adding the mixture into the reaction kettle, filling nitrogen into the reaction kettle, displacing air in the reaction kettle, heating the reaction kettle to 115-125 ℃, and carrying out dehydration reaction to obtain a prepolymer;
2) adding hexagonal boron nitride, ZnO whiskers and carbon nanotubes into the prepolymer, and dispersing at a high speed in a high-speed dispersion machine to ensure that the filler is dispersed uniformly enough to obtain a base adhesive;
the heat-conducting silicone oil is low-viscosity hydroxyl-terminated polydimethylsiloxane, and the viscosity of the heat-conducting silicone oil is 80-1000 mPa.s;
the hydroxyl-containing silicone rubber is low-viscosity 107 silicone rubber, and the viscosity of the low-viscosity 107 silicone rubber is 1800-2200 mPa.s.
2. The potting adhesive of claim 1, further comprising a latent curing agent used in direct admixture with the base adhesive.
3. The pouring sealant according to claim 2, wherein the latent solid agent comprises 15 to 20 parts by weight of dicyandiamide and 6 to 10 parts by weight of ZJ-1 accelerator.
4. The pouring sealant as claimed in claim 1, wherein the ZJ-1 accelerator is prepared by mixing DMP-30 and dimethylimidazole in a mass ratio of 1: 1.
5. The method for using the pouring sealant as claimed in claim 4, wherein the pouring sealant is cured within 1-3 hours at 115-125 ℃.
6. The potting adhesive of claim 1, further comprising a curing agent used independently of the base adhesive.
7. The pouring sealant according to claim 6, wherein the independently used curing agent comprises 100-120 parts by weight of modified curing agent and 5-10 parts by weight of coupling agent KH-550.
8. The pouring sealant according to claim 7, wherein the modified curing agent is prepared by the following method:
1) heating triethylene tetramine to 35 ℃, and then dropwise adding an epoxy 660 diluent, wherein the temperature is not higher than 60 ℃ in the dropwise adding process, and the dropwise adding is completed within 2-3 hours;
2) and cooling to 48-52 ℃, adding dimethyl imidazole, mixing and stirring until the mixture is clear and transparent, adding DMP-30, mixing and stirring uniformly to obtain the color-changing material.
9. The pouring sealant according to claim 8, wherein the amount of the triethylene tetramine is 20 to 25 parts, the amount of the epoxy 660 diluent is 72 to 28 parts, the amount of the DMP-30 is 3 to 5 parts, and the amount of the dimethyl imidazole is 5 to 6 parts by weight.
10. The use method of the pouring sealant as claimed in claim 8 or 9, characterized in that the base glue and the independently used curing agent are mixed according to the mass ratio of 3:1, uniformly mixing, and realizing primary curing at normal temperature for 4-6 h.
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| 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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| CN110317562B true CN110317562B (en) | 2021-11-19 |
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| 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 |
| 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 |
| 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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