CN112877017A - Low-curing-shrinkage heat-conducting epoxy pouring sealant and preparation method thereof - Google Patents
Low-curing-shrinkage heat-conducting epoxy pouring sealant and preparation method thereof Download PDFInfo
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- 239000004593 Epoxy Substances 0.000 title claims abstract description 66
- 239000000565 sealant Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 82
- 239000003822 epoxy resin Substances 0.000 claims abstract description 39
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 39
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 25
- 239000007822 coupling agent Substances 0.000 claims abstract description 21
- 239000003085 diluting agent Substances 0.000 claims abstract description 21
- 239000000945 filler Substances 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 239000012753 anti-shrinkage agent Substances 0.000 claims abstract description 14
- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical compound C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920005989 resin Polymers 0.000 claims abstract description 11
- 239000011347 resin Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims description 36
- -1 alkylene glycidyl ether Chemical compound 0.000 claims description 24
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 20
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 20
- 239000006229 carbon black Substances 0.000 claims description 20
- KFUSXMDYOPXKKT-UHFFFAOYSA-N 2-[(2-methylphenoxy)methyl]oxirane Chemical compound CC1=CC=CC=C1OCC1OC1 KFUSXMDYOPXKKT-UHFFFAOYSA-N 0.000 claims description 18
- LCFVJGUPQDGYKZ-UHFFFAOYSA-N Bisphenol A diglycidyl ether Chemical compound C=1C=C(OCC2OC2)C=CC=1C(C)(C)C(C=C1)=CC=C1OCC1CO1 LCFVJGUPQDGYKZ-UHFFFAOYSA-N 0.000 claims description 18
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 16
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 14
- YSUQLAYJZDEMOT-UHFFFAOYSA-N 2-(butoxymethyl)oxirane Chemical compound CCCCOCC1CO1 YSUQLAYJZDEMOT-UHFFFAOYSA-N 0.000 claims description 14
- QNYBOILAKBSWFG-UHFFFAOYSA-N 2-(phenylmethoxymethyl)oxirane Chemical compound C1OC1COCC1=CC=CC=C1 QNYBOILAKBSWFG-UHFFFAOYSA-N 0.000 claims description 14
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 claims description 14
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 14
- 150000001412 amines Chemical class 0.000 claims description 14
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 14
- 229920000570 polyether Polymers 0.000 claims description 14
- 239000004952 Polyamide Substances 0.000 claims description 12
- 229920002647 polyamide Polymers 0.000 claims description 12
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 10
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical class [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 10
- 239000004843 novolac epoxy resin Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 239000003292 glue Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 8
- 238000005336 cracking Methods 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 24
- 239000000377 silicon dioxide Substances 0.000 description 12
- 238000003756 stirring Methods 0.000 description 11
- 239000006185 dispersion Substances 0.000 description 9
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000009471 action Effects 0.000 description 3
- 238000009775 high-speed stirring Methods 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 description 2
- NWYDEWXSKCTWMJ-UHFFFAOYSA-N 2-methylcyclohexane-1,1-diamine Chemical compound CC1CCCCC1(N)N NWYDEWXSKCTWMJ-UHFFFAOYSA-N 0.000 description 2
- KOGSPLLRMRSADR-UHFFFAOYSA-N 4-(2-aminopropan-2-yl)-1-methylcyclohexan-1-amine Chemical compound CC(C)(N)C1CCC(C)(N)CC1 KOGSPLLRMRSADR-UHFFFAOYSA-N 0.000 description 2
- KSMVBYPXNKCPAJ-UHFFFAOYSA-N 4-Methylcyclohexylamine Chemical compound CC1CCC(N)CC1 KSMVBYPXNKCPAJ-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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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
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- C09J163/04—Epoxynovolacs
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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- Chemical & Material Sciences (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The invention discloses a heat-conducting epoxy pouring sealant with low curing shrinkage and a preparation method thereof, wherein the formula comprises the following components: the anti-shrinkage coating comprises a component A and a component B, wherein the component A is prepared by mixing 5-100 parts by weight of epoxy resin, 1-25 parts by weight of diluent, 0.1-0.5 part by weight of defoaming agent, 5-15 parts by weight of coupling agent, 50-300 parts by weight of filler and 5-50 parts by weight of anti-shrinkage agent, the component B is prepared by mixing 20-50 parts by weight of curing agent A and 50-80 parts by weight of curing agent B, and the mass ratio of the component A to the component B is 100: 8-30; the benzoxazine resin with zero shrinkage is added, so that the curing shrinkage of the heat-conducting epoxy pouring sealant is reduced, the problems of deformation and cracking of the heat-conducting epoxy pouring sealant are solved, the reliability and stability of the heat-conducting epoxy pouring sealant are enhanced, the heat conductivity, hardness and mechanical properties of the heat-conducting epoxy pouring sealant are improved, and the service life of the heat-conducting epoxy pouring sealant is prolonged.
Description
Technical Field
The invention relates to the technical field of heat-conducting electric insulating materials, in particular to a heat-conducting epoxy pouring sealant with low curing shrinkage and a preparation method thereof.
Background
The heat-conducting epoxy pouring sealant has excellent heat conductivity, heat resistance, mechanical property and electrical property, is widely applied to packaging and bonding of electronic and electrical equipment, and improves the stability and reliability of the electronic and electrical equipment.
However, the conventional heat-conducting epoxy pouring sealant generally uses liquid epoxy resin, has large cross-linking density, large internal stress after curing and forming, and high volume shrinkage, so that the heat-conducting epoxy pouring sealant is easy to deform and even crack, the reliability and stability of the heat-conducting epoxy pouring sealant are affected, and the service life of the heat-conducting epoxy pouring sealant is shortened.
Disclosure of Invention
The invention aims to provide a heat-conducting epoxy pouring sealant with low curing shrinkage rate and a preparation method thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a low-curing-shrinkage heat-conducting epoxy pouring sealant comprises the following formula: the anti-shrinkage coating comprises a component A and a component B, wherein the component A is prepared by mixing 5-100 parts by weight of epoxy resin, 1-25 parts by weight of diluent, 0.1-0.5 part by weight of defoaming agent, 5-15 parts by weight of coupling agent, 50-300 parts by weight of filler and 5-50 parts by weight of anti-shrinkage agent, the component B is prepared by mixing 20-50 parts by weight of curing agent A and 50-80 parts by weight of curing agent B, and the mass ratio of the component A to the component B is 100: 8-30.
A preparation method of a heat-conducting epoxy pouring sealant with low curing shrinkage rate comprises the following steps of selecting materials; step two, defoaming; step three, preparation; step four, preparing glue;
in the first step, 95-100 parts of epoxy resin, 1-25 parts of diluent, 0.1-0.5 part of defoaming agent, 5-15 parts of coupling agent, 50-300 parts of filler, 5-50 parts of anti-shrinkage agent, 20-50 parts of curing agent A and 50-80 parts of curing agent B are respectively weighed according to the parts by weight of the components for later use;
in the second step, the epoxy resin prepared in the first step is poured into a vacuum defoaming stirrer, the diluent, the defoaming agent, the coupling agent, the filler and the anti-shrinkage agent prepared in the first step are added, the mixture is slowly and uniformly stirred, then is stirred at a high speed, and is subjected to vacuum defoaming to prepare a component A;
in the third step, the curing agent A and the curing agent B prepared in the first step are poured into a container, and are mixed and stirred uniformly to prepare a component B;
and in the fourth step, the component A prepared in the second step is poured into a vacuum defoaming stirrer, the component B prepared in the third step is added according to the mass ratio, and the mixture is uniformly mixed and stirred and then subjected to vacuum defoaming to obtain the low-curing-shrinkage heat-conducting epoxy pouring sealant.
According to the technical scheme, the epoxy resin is any one or two of liquid bisphenol A diglycidyl ether epoxy resin and liquid novolac epoxy resin.
According to the technical scheme, the diluent is any one of alkylene glycidyl ether, butyl glycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, o-tolyl glycidyl ether and C12-14 fatty glycidyl ether.
According to the technical scheme, the coupling agent is any one of 3-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane.
According to the technical scheme, the filler is any one or more of modified aluminum hydroxide micro powder, alumina micro powder, carbon black, silicon micro powder and calcium carbonate micro powder.
According to the technical scheme, the anti-shrinking agent is liquid benzoxazine resin.
According to the technical scheme, the curing agent A is an alicyclic amine curing agent.
According to the technical scheme, the curing agent B is one or two of a polyether amine curing agent and a polyamide curing agent.
Compared with the prior art, the invention has the following beneficial effects: the benzoxazine resin with zero shrinkage is added, so that the curing shrinkage of the heat-conducting epoxy pouring sealant is remarkably reduced, the problems of deformation and cracking of the heat-conducting epoxy pouring sealant are solved, the reliability and the stability of the heat-conducting epoxy pouring sealant are enhanced, the heat conductivity, the hardness and the mechanical property of the heat-conducting epoxy pouring sealant are improved, the service life of the heat-conducting epoxy pouring sealant is prolonged, and the heat-conducting epoxy pouring sealant is suitable for packaging and bonding electronic and electrical products with high requirements on the curing shrinkage and the heat conductivity.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a flow chart of the method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution:
example 1:
a low-curing-shrinkage heat-conducting epoxy pouring sealant comprises the following formula: the adhesive comprises a component A and a component B, wherein the component A is prepared by mixing 5-100 parts by weight of epoxy resin, 1-25 parts by weight of diluent, 0.1-0.5 part by weight of defoaming agent, 5-15 parts by weight of coupling agent, 50-300 parts by weight of filler and 5-50 parts by weight of anti-shrinking agent, the component B is prepared by mixing 20-50 parts by weight of curing agent A and 50-80 parts by weight of curing agent B, the mass ratio of the component A to the component B is 100: 8-30, the epoxy resin is any one or two of liquid bisphenol A diglycidyl ether epoxy resin and liquid novolac epoxy resin, the diluent is any one of alkylene glycidyl ether, butyl glycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, o-tolyl glycidyl ether and C12-14 fatty glycidyl ether, and the coupling agent is 3-aminopropyltrimethoxysilane, butyl glycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, o-tolyl glycidyl ether and C12-14 fatty glycidyl ether, The anti-shrinkage coating comprises gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, wherein the filler is one or more of modified aluminum hydroxide micropowder, alumina micropowder, carbon black, silica micropowder and calcium carbonate micropowder, the anti-shrinkage agent is liquid benzoxazine resin, the curing agent A is alicyclic amine curing agent, and the curing agent B is one or two of polyether amine curing agent and polyamide curing agent.
A preparation method of a heat-conducting epoxy pouring sealant with low curing shrinkage rate comprises the following steps of selecting materials; step two, defoaming; step three, preparation; step four, preparing glue;
in the first step, 120 parts of liquid bisphenol A diglycidyl ether epoxy resin with the epoxy equivalent of 170-190 g/ep, 10 parts of alkylene glycidyl ether, 0.5 part of defoaming agent, 5 parts of gamma-aminopropyltriethoxysilane, 5 parts of carbon black, 200 parts of alumina micropowder, 50 parts of silica micropowder, 10 parts of anti-shrinkage agent, 40 parts of isophorone diamine and 60 parts of D400 polyether amine are respectively weighed according to the parts by weight of the components for later use;
pouring the liquid bisphenol A diglycidyl ether epoxy resin prepared in the step one into a vacuum defoaming stirrer, adding the alkylene glycidyl ether, the defoaming agent, the gamma-aminopropyltriethoxysilane, the carbon black and the anti-shrinking agent prepared in the step one, slowly stirring while adding the alumina micropowder and the silica micropowder after uniformly dispersing, stirring at a high speed for 30min after completely dispersing, and defoaming for 15min after completely dispersing to prepare a component A;
in the third step, the isophorone diamine and the D400 polyether amine prepared in the first step are poured into a container, and are mixed and stirred uniformly to prepare a component B;
and in the fourth step, the component A prepared in the second step is poured into a vacuum defoaming stirrer, the component B prepared in the third step is added according to the mass ratio of 100: 12, and the mixture is uniformly mixed and stirred and then is subjected to vacuum defoaming for 5min, so that the low-curing-shrinkage heat-conducting epoxy pouring sealant is obtained.
Example 2:
a low-curing-shrinkage heat-conducting epoxy pouring sealant comprises the following formula: the adhesive comprises a component A and a component B, wherein the component A is prepared by mixing 5-100 parts by weight of epoxy resin, 1-25 parts by weight of diluent, 0.1-0.5 part by weight of defoaming agent, 5-15 parts by weight of coupling agent, 50-300 parts by weight of filler and 5-50 parts by weight of anti-shrinking agent, the component B is prepared by mixing 20-50 parts by weight of curing agent A and 50-80 parts by weight of curing agent B, the mass ratio of the component A to the component B is 100: 8-30, the epoxy resin is any one or two of liquid bisphenol A diglycidyl ether epoxy resin and liquid novolac epoxy resin, the diluent is any one of alkylene glycidyl ether, butyl glycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, o-tolyl glycidyl ether and C12-14 fatty glycidyl ether, and the coupling agent is 3-aminopropyltrimethoxysilane, butyl glycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, o-tolyl glycidyl ether and C12-14 fatty glycidyl ether, The anti-shrinkage coating comprises gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, wherein the filler is one or more of modified aluminum hydroxide micropowder, alumina micropowder, carbon black, silica micropowder and calcium carbonate micropowder, the anti-shrinkage agent is liquid benzoxazine resin, the curing agent A is alicyclic amine curing agent, and the curing agent B is one or two of polyether amine curing agent and polyamide curing agent.
A preparation method of a heat-conducting epoxy pouring sealant with low curing shrinkage rate comprises the following steps of selecting materials; step two, defoaming; step three, preparation; step four, preparing glue;
in the first step, 120 parts of liquid bisphenol A diglycidyl ether epoxy resin with the epoxy equivalent of 190-210 g/ep, 12 parts of alkylene glycidyl ether, 0.5 part of defoaming agent, 5 parts of gamma- (2, 3-glycidoxy) propyl trimethoxy silane, 5 parts of carbon black, 200 parts of alumina micro powder, 50 parts of calcium carbonate micro powder, 10 parts of anti-shrinking agent, 40 parts of iso-bis (4-aminocyclohexyl methane) and 60 parts of YD-8140 polyamide are respectively weighed according to the parts by weight of the components for later use;
in the second step, the liquid bisphenol A diglycidyl ether epoxy resin prepared in the first step is poured into a vacuum defoaming stirrer, alkylene glycidyl ether, a defoaming agent, gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, carbon black and an anti-shrinking agent prepared in the first step are added, after uniform dispersion, alumina micropowder and calcium carbonate micropowder are added while slowly stirring, after complete dispersion, high-speed stirring is carried out for 30min, and after complete dispersion, vacuum defoaming is carried out for 15min, so as to prepare a component A;
in the third step, the prepared iso-bis (4-aminocyclohexyl methane) and YD-8140 polyamide in the first step are poured into a container, and are mixed and stirred uniformly to prepare a component B;
and in the fourth step, the component A prepared in the second step is poured into a vacuum defoaming stirrer, the component B prepared in the third step is added according to the mass ratio of 100: 12, and the mixture is uniformly mixed and stirred and then is subjected to vacuum defoaming for 5min, so that the low-curing-shrinkage heat-conducting epoxy pouring sealant is obtained.
Example 3:
a low-curing-shrinkage heat-conducting epoxy pouring sealant comprises the following formula: the adhesive comprises a component A and a component B, wherein the component A is prepared by mixing 5-100 parts by weight of epoxy resin, 1-25 parts by weight of diluent, 0.1-0.5 part by weight of defoaming agent, 5-15 parts by weight of coupling agent, 50-300 parts by weight of filler and 5-50 parts by weight of anti-shrinking agent, the component B is prepared by mixing 20-50 parts by weight of curing agent A and 50-80 parts by weight of curing agent B, the mass ratio of the component A to the component B is 100: 8-30, the epoxy resin is any one or two of liquid bisphenol A diglycidyl ether epoxy resin and liquid novolac epoxy resin, the diluent is any one of alkylene glycidyl ether, butyl glycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, o-tolyl glycidyl ether and C12-14 fatty glycidyl ether, and the coupling agent is 3-aminopropyltrimethoxysilane, butyl glycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, o-tolyl glycidyl ether and C12-14 fatty glycidyl ether, The anti-shrinkage coating comprises gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, wherein the filler is one or more of modified aluminum hydroxide micropowder, alumina micropowder, carbon black, silica micropowder and calcium carbonate micropowder, the anti-shrinkage agent is liquid benzoxazine resin, the curing agent A is alicyclic amine curing agent, and the curing agent B is one or two of polyether amine curing agent and polyamide curing agent.
A preparation method of a heat-conducting epoxy pouring sealant with low curing shrinkage rate comprises the following steps of selecting materials; step two, defoaming; step three, preparation; step four, preparing glue;
in the first step, 120 parts of liquid bisphenol A diglycidyl ether epoxy resin with the epoxy equivalent of 220-240 g/ep, 15 parts of o-tolyl glycidyl ether, 0.5 part of a defoaming agent, 5 parts of gamma-glycidyl ether oxypropyltrimethoxysilane, 5 parts of carbon black, 200 parts of alumina micropowder, 45 parts of aluminum hydroxide micropowder, 10 parts of a shrinkage resistant agent, 30 parts of methylcyclohexanediamine and 70 parts of D400 polyetheramine are respectively weighed according to the parts by weight of the components for later use;
in the second step, the liquid bisphenol A diglycidyl ether epoxy resin prepared in the first step is poured into a vacuum defoaming stirrer, the o-tolyl glycidyl ether prepared in the first step, a defoaming agent, gamma-glycidyl ether oxypropyltrimethoxysilane, carbon black and an anti-shrinking agent are added, after uniform dispersion, alumina micropowder and aluminum hydroxide micropowder are added while slowly stirring, after complete dispersion, high-speed stirring is carried out for 30min, and after complete dispersion, vacuum defoaming is carried out for 15min to prepare a component A;
in the third step, the methylcyclohexanediamine and the D400 polyetheramine prepared in the first step are poured into a container, and are mixed and stirred uniformly to prepare a component B;
and in the fourth step, the component A prepared in the second step is poured into a vacuum defoaming stirrer, the component B prepared in the third step is added according to the mass ratio of 100: 13, and the mixture is uniformly mixed and stirred and then is subjected to vacuum defoaming for 5min, so that the low-curing-shrinkage heat-conducting epoxy pouring sealant is obtained.
Example 4:
a low-curing-shrinkage heat-conducting epoxy pouring sealant comprises the following formula: the adhesive comprises a component A and a component B, wherein the component A is prepared by mixing 5-100 parts by weight of epoxy resin, 1-25 parts by weight of diluent, 0.1-0.5 part by weight of defoaming agent, 5-15 parts by weight of coupling agent, 50-300 parts by weight of filler and 5-50 parts by weight of anti-shrinking agent, the component B is prepared by mixing 20-50 parts by weight of curing agent A and 50-80 parts by weight of curing agent B, the mass ratio of the component A to the component B is 100: 8-30, the epoxy resin is any one or two of liquid bisphenol A diglycidyl ether epoxy resin and liquid novolac epoxy resin, the diluent is any one of alkylene glycidyl ether, butyl glycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, o-tolyl glycidyl ether and C12-14 fatty glycidyl ether, and the coupling agent is 3-aminopropyltrimethoxysilane, butyl glycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, o-tolyl glycidyl ether and C12-14 fatty glycidyl ether, The anti-shrinkage coating comprises gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, wherein the filler is one or more of modified aluminum hydroxide micropowder, alumina micropowder, carbon black, silica micropowder and calcium carbonate micropowder, the anti-shrinkage agent is liquid benzoxazine resin, the curing agent A is alicyclic amine curing agent, and the curing agent B is one or two of polyether amine curing agent and polyamide curing agent.
A preparation method of a heat-conducting epoxy pouring sealant with low curing shrinkage rate comprises the following steps of selecting materials; step two, defoaming; step three, preparation; step four, preparing glue;
in the first step, 120 parts of liquid novolac epoxy resin with the epoxy equivalent of 190-210 g/ep, 15 parts of o-tolyl glycidyl ether, 0.5 part of defoaming agent, 5 parts of 3-aminopropyltrimethoxysilane, 5 parts of carbon black, 245 parts of alumina micropowder, 10 parts of anti-shrinkage agent, 40 parts of menthane diamine and 60 parts of 650-type polyamide are weighed according to the parts by weight of the components for later use;
pouring the liquid novolac epoxy resin prepared in the step one into a vacuum defoaming stirrer, adding the o-tolyl glycidyl ether prepared in the step one, a defoaming agent, 3-aminopropyl trimethoxysilane, carbon black and an anti-shrinking agent, uniformly dispersing, slowly stirring while adding alumina micropowder, completely dispersing, stirring at a high speed for 30min, completely dispersing, and then defoaming in vacuum for 15min to obtain a component A;
in the third step, the menthane diamine prepared in the first step and 650 type polyamide are poured into a container, and are mixed and stirred uniformly to prepare a component B;
and in the fourth step, the component A prepared in the second step is poured into a vacuum defoaming stirrer, the component B prepared in the third step is added according to the mass ratio of 100: 16, and the mixture is uniformly mixed and stirred and then is subjected to vacuum defoaming for 5min, so that the low-curing-shrinkage heat-conducting epoxy pouring sealant is obtained.
Comparative example 1:
a low-curing-shrinkage heat-conducting epoxy pouring sealant comprises the following formula: the adhesive comprises a component A and a component B, wherein the component A is prepared by mixing 5-100 parts by weight of epoxy resin, 1-25 parts by weight of diluent, 0.1-0.5 part by weight of defoaming agent, 5-15 parts by weight of coupling agent, 50-300 parts by weight of filler and 5-50 parts by weight of anti-shrinking agent, the component B is prepared by mixing 20-50 parts by weight of curing agent A and 50-80 parts by weight of curing agent B, the mass ratio of the component A to the component B is 100: 8-30, the epoxy resin is any one or two of liquid bisphenol A diglycidyl ether epoxy resin and liquid novolac epoxy resin, the diluent is any one of alkylene glycidyl ether, butyl glycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, o-tolyl glycidyl ether and C12-14 fatty glycidyl ether, and the coupling agent is 3-aminopropyltrimethoxysilane, butyl glycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, o-tolyl glycidyl ether and C12-14 fatty glycidyl ether, The anti-shrinkage coating comprises gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, wherein the filler is one or more of modified aluminum hydroxide micropowder, alumina micropowder, carbon black, silica micropowder and calcium carbonate micropowder, the anti-shrinkage agent is liquid benzoxazine resin, the curing agent A is alicyclic amine curing agent, and the curing agent B is one or two of polyether amine curing agent and polyamide curing agent.
A preparation method of a heat-conducting epoxy pouring sealant with low curing shrinkage rate comprises the following steps of selecting materials; step two, defoaming; step three, preparation; step four, preparing glue;
in the first step, 120 parts of liquid bisphenol A diglycidyl ether epoxy resin with the epoxy equivalent of 190-210 g/ep, 12 parts of alkylene glycidyl ether, 0.5 part of defoaming agent, 5 parts of gamma-aminopropyltriethoxysilane, 5 parts of carbon black, 200 parts of alumina micropowder, 60 parts of silica micropowder, 40 parts of isophorone diamine and 60 parts of D400 polyether amine are respectively weighed according to the parts by weight of the components for later use;
in the second step, the liquid bisphenol A diglycidyl ether epoxy resin prepared in the first step is poured into a vacuum defoaming stirrer, the alkylene glycidyl ether, the defoaming agent, the gamma-aminopropyltriethoxysilane and the carbon black prepared in the first step are added, after uniform dispersion, alumina micropowder and silica micropowder are added while slowly stirring, after complete dispersion, high-speed stirring is carried out for 30min, and after complete dispersion, vacuum defoaming is carried out for 15min to prepare a component A;
in the third step, the isophorone diamine and the D400 polyether amine prepared in the first step are poured into a container, and are mixed and stirred uniformly to prepare a component B;
and in the fourth step, pouring the component A prepared in the second step into a vacuum defoaming stirrer, adding a corresponding amount of the component B prepared in the third step according to the mass ratio of 100: 11, uniformly mixing and stirring, and performing vacuum defoaming for 5min to obtain the heat-conducting epoxy pouring sealant.
Comparative example 2:
a low-curing-shrinkage heat-conducting epoxy pouring sealant comprises the following formula: the adhesive comprises a component A and a component B, wherein the component A is prepared by mixing 5-100 parts by weight of epoxy resin, 1-25 parts by weight of diluent, 0.1-0.5 part by weight of defoaming agent, 5-15 parts by weight of coupling agent, 50-300 parts by weight of filler and 5-50 parts by weight of anti-shrinking agent, the component B is prepared by mixing 20-50 parts by weight of curing agent A and 50-80 parts by weight of curing agent B, the mass ratio of the component A to the component B is 100: 8-30, the epoxy resin is any one or two of liquid bisphenol A diglycidyl ether epoxy resin and liquid novolac epoxy resin, the diluent is any one of alkylene glycidyl ether, butyl glycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, o-tolyl glycidyl ether and C12-14 fatty glycidyl ether, and the coupling agent is 3-aminopropyltrimethoxysilane, butyl glycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, o-tolyl glycidyl ether and C12-14 fatty glycidyl ether, The anti-shrinkage coating comprises gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, wherein the filler is one or more of modified aluminum hydroxide micropowder, alumina micropowder, carbon black, silica micropowder and calcium carbonate micropowder, the anti-shrinkage agent is liquid benzoxazine resin, the curing agent A is alicyclic amine curing agent, and the curing agent B is one or two of polyether amine curing agent and polyamide curing agent.
A preparation method of a heat-conducting epoxy pouring sealant with low curing shrinkage rate comprises the following steps of selecting materials; step two, defoaming; step three, preparation; step four, preparing glue;
in the first step, 120 parts of liquid bisphenol A diglycidyl ether epoxy resin with the epoxy equivalent of 190-210 g/ep, 30 parts of alkylene glycidyl ether, 0.5 part of defoaming agent, 5 parts of gamma-aminopropyltriethoxysilane, 5 parts of carbon black, 200 parts of alumina micropowder, 40 parts of silica micropowder, 40 parts of isophorone diamine and 60 parts of D400 polyether amine are respectively weighed according to the parts by weight of the components for later use;
pouring the liquid bisphenol A diglycidyl ether epoxy resin prepared in the step one into a vacuum defoaming stirrer, adding the alkylene glycidyl ether, the defoaming agent, the gamma-aminopropyltriethoxysilane, the carbon black and the anti-shrinking agent prepared in the step one, slowly stirring while adding the alumina micropowder and the silica micropowder after uniformly dispersing, stirring at a high speed for 30min after completely dispersing, and defoaming for 15min after completely dispersing to prepare a component A;
in the third step, the isophorone diamine and the D400 polyether amine prepared in the first step are poured into a container, and are mixed and stirred uniformly to prepare a component B;
and in the fourth step, pouring the component A prepared in the second step into a vacuum defoaming stirrer, adding a corresponding amount of the component B prepared in the third step according to the mass ratio of 100: 11, uniformly mixing and stirring, and performing vacuum defoaming for 5min to obtain the heat-conducting epoxy pouring sealant.
The low curing shrinkage rate heat-conducting epoxy pouring sealant obtained in the above embodiment and the heat-conducting epoxy pouring sealant obtained in the comparative example are subjected to curing shrinkage rate, heat conductivity, hardness, bending strength and impact strength item detection, and the detection results are as follows:
curing shrinkage | Thermal conductivity | Hardness of | Bending strength | Impact strength | |
Example 1 | 0.49% | 0.95W/m.K | 90 | 91MPa | 15.2kJ/m2 |
Example 2 | 0.45% | 0.91W/m.K | 89 | 87MPa | 14.3kJ/m2 |
Example 3 | 0.46% | 0.89W/m.K | 88 | 82MPa | 13.8kJ/m2 |
Example 4 | 0.42% | 0.88W/m.K | 86 | 78MPa | 14.2kJ/m2 |
Comparative example 1 | 1.13% | 0.96W/m.K | 89 | 88MPa | 14.9kJ/m2 |
Comparative example 2 | 0.95% | 0.90W/m.K | 81 | 55MPa | 9.8kJ/m2 |
Compared with the prior art, the invention has the following beneficial effects: the benzoxazine resin with zero shrinkage is added, so that the curing shrinkage of the heat-conducting epoxy pouring sealant is remarkably reduced, the problems of deformation and cracking of the heat-conducting epoxy pouring sealant are solved, the reliability and the stability of the heat-conducting epoxy pouring sealant are enhanced, the heat conductivity, the hardness and the mechanical property of the heat-conducting epoxy pouring sealant are improved, the service life of the heat-conducting epoxy pouring sealant is prolonged, and the heat-conducting epoxy pouring sealant is suitable for packaging and bonding electronic and electrical products with high requirements on the curing shrinkage and the heat conductivity.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A low-curing-shrinkage heat-conducting epoxy pouring sealant comprises the following formula: the component A and the component B are characterized in that: the component A is prepared by mixing 5-100 parts by weight of epoxy resin, 1-25 parts by weight of diluent, 0.1-0.5 part by weight of defoaming agent, 5-15 parts by weight of coupling agent, 50-300 parts by weight of filler and 5-50 parts by weight of anti-shrinking agent, the component B is prepared by mixing 20-50 parts by weight of curing agent A and 50-80 parts by weight of curing agent B, and the mass ratio of the component A to the component B is 100: 8-30.
2. A preparation method of a heat-conducting epoxy pouring sealant with low curing shrinkage rate comprises the following steps of selecting materials; step two, defoaming; step three, preparation; step four, preparing glue; the method is characterized in that:
in the first step, 95-100 parts of epoxy resin, 1-25 parts of diluent, 0.1-0.5 part of defoaming agent, 5-15 parts of coupling agent, 50-300 parts of filler, 5-50 parts of anti-shrinkage agent, 20-50 parts of curing agent A and 50-80 parts of curing agent B are respectively weighed according to the parts by weight of the components for later use;
in the second step, the epoxy resin prepared in the first step is poured into a vacuum defoaming stirrer, the diluent, the defoaming agent, the coupling agent, the filler and the anti-shrinkage agent prepared in the first step are added, the mixture is slowly and uniformly stirred, then is stirred at a high speed, and is subjected to vacuum defoaming to prepare a component A;
in the third step, the curing agent A and the curing agent B prepared in the first step are poured into a container, and are mixed and stirred uniformly to prepare a component B;
and in the fourth step, the component A prepared in the second step is poured into a vacuum defoaming stirrer, the component B prepared in the third step is added according to the mass ratio, and the mixture is uniformly mixed and stirred and then subjected to vacuum defoaming to obtain the low-curing-shrinkage heat-conducting epoxy pouring sealant.
3. The low curing shrinkage rate heat-conducting epoxy pouring sealant as claimed in claim 1, wherein: the epoxy resin is any one or two of liquid bisphenol A diglycidyl ether epoxy resin and liquid novolac epoxy resin.
4. The low curing shrinkage rate heat-conducting epoxy pouring sealant as claimed in claim 1, wherein: the diluent is any one of alkylene glycidyl ether, butyl glycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, o-tolyl glycidyl ether and C12-14 fatty glycidyl ether.
5. The low curing shrinkage rate heat-conducting epoxy pouring sealant as claimed in claim 1, wherein: the coupling agent is any one of 3-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane.
6. The low curing shrinkage rate heat-conducting epoxy pouring sealant as claimed in claim 1, wherein: the filler is any one or more of modified aluminum hydroxide micro powder, alumina micro powder, carbon black, silicon micro powder and calcium carbonate micro powder.
7. The low curing shrinkage rate heat-conducting epoxy pouring sealant as claimed in claim 1, wherein: the anti-shrinking agent is liquid benzoxazine resin.
8. The low curing shrinkage rate heat-conducting epoxy pouring sealant as claimed in claim 1, wherein: the curing agent A is alicyclic amine curing agent.
9. The low curing shrinkage rate heat-conducting epoxy pouring sealant as claimed in claim 1, wherein: the curing agent B is one or two of polyether amine curing agent and polyamide curing agent.
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