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CN110577813A - Formula and preparation method of high-flexibility low-halogen epoxy resin pouring sealant - Google Patents

Formula and preparation method of high-flexibility low-halogen epoxy resin pouring sealant Download PDF

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Publication number
CN110577813A
CN110577813A CN201910955643.4A CN201910955643A CN110577813A CN 110577813 A CN110577813 A CN 110577813A CN 201910955643 A CN201910955643 A CN 201910955643A CN 110577813 A CN110577813 A CN 110577813A
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China
Prior art keywords
component
halogen
epoxy resin
low
parts
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Pending
Application number
CN201910955643.4A
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Chinese (zh)
Inventor
邹建平
翁伟君
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Intercalon Electronic Materials Co Ltd
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Shanghai Intercalon Electronic Materials Co Ltd
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Priority to CN201910955643.4A priority Critical patent/CN110577813A/en
Publication of CN110577813A publication Critical patent/CN110577813A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates 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
    • C08G59/18Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50Amines
    • C08G59/504Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Sealing Material Composition (AREA)

Abstract

the invention relates to the technical field of adhesive materials, and discloses a high-flexibility low-halogen epoxy resin pouring sealant formula and a preparation method thereof, wherein the high-flexibility low-halogen epoxy resin pouring sealant formula and the preparation method thereof are characterized in that an epoxy adhesive is formed by curing a component A and a component B according to the weight ratio of 100/50-100; wherein the component A consists of the following components: 40-100 parts of special epoxy resin; 0-15 parts of low-halogen diluent; 0.2-0.5 part by mass of a defoaming agent; 0-50 parts of filler and the balance of color paste; the component B consists of the following components: 95-100 parts of polyether amine; 0.0-5.0 parts of accelerator, low-halogen special epoxy resin and low-halogen flexible polyfunctional epoxy diluent are used to ensure the flexibility and environmental protection of the product, and polyether amine is used to ensure the high flexibility and longer service life of the product and the bonding property and flexibility of the product, so that the pouring sealant is cured at a wider temperature range of 120-150 ℃, and the application range of the adhesive is improved.

Description

formula and preparation method of high-flexibility low-halogen epoxy resin pouring sealant
Technical Field
the invention relates to the technical field of adhesive materials, in particular to a high-flexibility low-halogen epoxy resin pouring sealant formula and a preparation method thereof.
Background
at present, two types of capacitors are mainly used in various fields such as household appliances, aerospace, various electronic products and the like, namely oil-immersed capacitors and dry capacitors. The filler used for the dry capacitor is basically epoxy resin, although the epoxy resin has excellent insulating property and high temperature resistance, and the shell is not greatly influenced even if the shell is cracked due to collision in transportation or actual use. However, epoxy resins also have their limitations, being cold-resistant, brittle and inelastic. If the capacitor is operated at high temperature, the capacitor expands due to heating and is easy to crack epoxy resin; when the capacitor is operated at a low temperature, the capacitor is cooled and shrinks, and a certain gap is easily formed between the capacitor and the epoxy resin, so that the insulating property of the capacitor is affected. In order to ensure the safety and reliability of the encapsulated capacitor, the requirements on the epoxy resin encapsulating adhesive are strict, the encapsulated device and the shell are required to have good adhesion, moisture and heat aging resistance, cold and heat shock resistance and ultraviolet ray long-term irradiation resistance, and therefore a formula and a preparation method of the high-flexibility low-halogen epoxy resin encapsulating adhesive are urgently needed.
disclosure of Invention
Technical problem to be solved
aiming at the defects of the prior art, the invention provides the formula of the high-flexibility low-halogen epoxy resin pouring sealant and the preparation method thereof, the formula has the advantages of flexibility, environmental friendliness, improvement on the application range of the adhesive and the like, and the problems of poor adhesion of the pouring sealant, easiness in humid heat aging and low elongation at break are solved.
(II) technical scheme
In order to achieve the purposes of flexibility and environmental protection and improving the application range of the adhesive, the invention provides the following technical scheme: the epoxy adhesive is formed by curing a component A and a component B according to the weight ratio of 100/50-100;
Wherein the component A consists of the following components: 40-100 parts of special epoxy resin; 0-15 parts of low-halogen diluent; 0.2-0.5 part by mass of a defoaming agent; 0-50 parts of filler and the balance of color paste;
the component B consists of the following components: 95-100 parts of polyether amine; 0.0 to 5.0 parts by mass of an accelerator.
Preferably, the special epoxy resin is one or two of low-halogen polyurethane modified epoxy and polyether modified epoxy.
Preferably, the low-halogen diluent is a low-halogen flexible multifunctional epoxy diluent.
preferably, the defoamer is a silicone defoamer.
Preferably, the filler is one or more of aluminum hydroxide, silica micropowder, calcium carbonate and talcum powder.
preferably, the polyether amine is one or more of D-230, D-400 and D-2000.
preferably, the accelerator is one or two of DMP-30 and imidazole.
A preparation method of a high-flexibility low-halogen epoxy resin pouring sealant comprises the following steps,
wherein the component A is prepared by the following steps:
(a) adding special epoxy resin, a defoaming agent and color paste into a resin stirring kettle in sequence according to the mass parts of the components, starting stirring, and uniformly stirring;
(b) adding a filler, and stirring for 1-2 hours;
(c) Adding the diluent, and stirring for 0.5-1 hour;
(d) Carrying out vacuum defoaming for 120 minutes;
(e) Obtaining a viscous liquid component A;
Wherein the component B is prepared by the following steps:
(a) putting the polyether amine and the accelerant into a stirring kettle according to respective mass parts, and stirring for 30 minutes;
(b) Obtaining a viscous liquid component B;
the component A and the component B are mixed according to the mass ratio of 100:50-100, the mixture is cured at the temperature of 120-150 ℃, and the cured epoxy potting adhesive is obtained after curing.
(III) advantageous effects
compared with the prior art, the invention provides a high-flexibility low-halogen epoxy resin pouring sealant formula and a preparation method thereof, and the formula has the following beneficial effects:
1. According to the formula and the preparation method of the high-flexibility low-halogen epoxy resin pouring sealant, low-halogen special epoxy resin (polyurethane modified epoxy and polyether modified epoxy) and low-halogen flexible polyfunctional epoxy diluent are used, so that the flexibility and the environmental friendliness of the product are guaranteed.
2. according to the formula and the preparation method of the high-flexibility low-halogen epoxy resin pouring sealant, the polyether amine is used, the high flexibility and the long service life of a product are ensured, the bonding performance and the flexibility of the product are ensured, the pouring sealant is cured at a wide temperature range of 120-150 ℃, and the application range of an adhesive is improved.
3. According to the formula and the preparation method of the high-flexibility low-halogen epoxy resin pouring sealant, the defoaming agent is added into the epoxy resin adhesive, and the defoaming agent is an organic silicon defoaming agent, so that bubbles in a system are effectively reduced, and the heat-conducting property and the bonding property of a product are improved.
4. the formula and the preparation method of the high-flexibility low-halogen epoxy resin pouring sealant solve the problem of elongation at break of a product (50-100%), have high bonding strength, have high and low temperature resistance (40-150 ℃) and are wide in application range.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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.
example one
A formula of a high-flexibility low-halogen epoxy resin pouring sealant comprises the following components: the epoxy adhesive is formed by curing the component A and the component B according to the weight ratio of 100/50-100;
The component A comprises the following components in percentage by weight: 40 parts of special epoxy resin; 15 parts of low-halogen diluent; 0.5 part by mass of a defoaming agent; 40 parts of filler and the balance of color paste;
The component B comprises the following components in percentage by weight: 98 parts of polyether amine; 2.0 parts of accelerator.
Example two
a formula of a high-flexibility low-halogen epoxy resin pouring sealant comprises the following components: the epoxy adhesive is formed by curing the component A and the component B according to the weight ratio of 100/50-100;
The component A comprises the following components in percentage by weight: 60 parts of special epoxy resin; 10 parts by mass of a low-halogen diluent; 0.4 part by mass of a defoaming agent; 20 parts of filler and the balance of color paste;
the component B comprises the following components in percentage by weight: 96 parts of polyether amine; 4.0 parts of accelerator.
EXAMPLE III
a formula of a high-flexibility low-halogen epoxy resin pouring sealant comprises the following components: the epoxy adhesive is formed by curing the component A and the component B according to the weight ratio of 100/50-100;
The component A comprises the following components in percentage by weight: 80 parts of special epoxy resin; 5 parts by mass of a low-halogen diluent; 0.3 part by mass of a defoaming agent; 10 parts of filler and the balance of color paste;
the component B comprises the following components in percentage by weight: 95 parts by mass of polyetheramine; 5.0 parts by mass of an accelerator.
wherein,
the special epoxy resin is one or two of low-halogen polyurethane modified epoxy and polyether modified epoxy;
The low-halogen diluent is a low-halogen flexible polyfunctional epoxy diluent;
the defoaming agent is an organic silicon defoaming agent;
the filler is one or more of aluminum hydroxide, silicon micropowder, calcium carbonate and talcum powder;
The polyether amine is one or more of D-230, D-400 and D-2000;
The promoter is one or two of DMP-30 and imidazole.
A preparation method of a high-flexibility low-halogen epoxy resin pouring sealant comprises the following steps,
Wherein the component A is prepared by the following steps:
(a) Adding special epoxy resin, a defoaming agent and color paste into a resin stirring kettle in sequence according to the mass parts of the components, starting stirring, and uniformly stirring;
(b) adding a filler, and stirring for 1-2 hours;
(c) Adding the diluent, and stirring for 0.5-1 hour;
(d) Carrying out vacuum defoaming for 120 minutes;
(e) Obtaining a viscous liquid component A;
Wherein the component B is prepared by the following steps:
(a) putting the polyether amine and the accelerant into a stirring kettle according to respective mass parts, and stirring for 30 minutes;
(b) Obtaining a viscous liquid component B;
the component A and the component B are mixed according to the mass ratio of 100:50-100, the mixture is cured at the temperature of 120-150 ℃, and the cured epoxy potting adhesive is obtained after curing.
the cured product properties are shown below:
Item Unit of Test data Method of producing a composite material
Hardness of Shore D 25℃ 50-80 Shore D
Boiling water absorption 100℃4hr% <1.0
Dielectric strength KV/mm 25℃ >17 GB/T 15479-1995
volume resistivity Ω-m 25℃ >1015 GB/T 1410-2006
Dielectric loss 50Hz,25℃ 0.5 GB/T 1409-2006
elongation at break 25℃,% 50-100
temperature range of use -40-150℃
although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (6)

1. the formula of the high-flexibility low-halogen epoxy resin pouring sealant is characterized in that: the epoxy adhesive is formed by curing a component A and a component B according to the weight ratio of 100/50-100;
wherein the component A consists of the following components: 40-100 parts of special epoxy resin; 0-15 parts of low-halogen diluent; 0.2-0.5 part by mass of a defoaming agent; 0-50 parts of filler and the balance of color paste;
the component B consists of the following components: 95-100 parts of polyether amine; 0.0 to 5.0 parts by mass of an accelerator.
2. the formula of the high-flexibility low-halogen epoxy resin pouring sealant and the preparation method thereof according to claim 1 are characterized in that: the special epoxy resin is one or two of low-halogen polyurethane modified epoxy and polyether modified epoxy.
3. The formula of the high-flexibility low-halogen epoxy resin pouring sealant and the preparation method thereof according to claim 1 are characterized in that: the low-halogen diluent is a low-halogen flexible polyfunctional epoxy diluent.
4. the formula of the high-flexibility low-halogen epoxy resin pouring sealant and the preparation method thereof according to claim 1 are characterized in that: the polyether amine is one or more of D-230, D-400 and D-2000.
5. The preparation method of the high-flexibility low-halogen epoxy resin pouring sealant as claimed in claim 1, wherein the preparation method comprises the following steps: the method comprises the following steps:
Wherein the component A is prepared by the following steps:
(a) Adding special epoxy resin, a defoaming agent and color paste into a resin stirring kettle in sequence according to the mass parts of the components, starting stirring, and uniformly stirring;
(b) adding a filler, and stirring for 1-2 hours;
(c) Adding the diluent, and stirring for 0.5-1 hour;
(d) Carrying out vacuum defoaming for 120 minutes;
(e) obtaining a viscous liquid component A;
Wherein the component B is prepared by the following steps:
(a) putting the polyether amine and the accelerant into a stirring kettle according to respective mass parts, and stirring for 30 minutes;
(b) obtaining a viscous liquid component B;
Mixing the component A and the component B according to the corresponding proportion.
6. The formula of the high-flexibility low-halogen epoxy resin pouring sealant and the preparation method thereof according to claim 1 are characterized in that: and the component A and the component B are mixed according to the mass ratio of 100:50-100, the mixture is cured at the temperature of 120-150 ℃, and the cured product of the epoxy pouring sealant is obtained after curing.
CN201910955643.4A 2019-10-09 2019-10-09 Formula and preparation method of high-flexibility low-halogen epoxy resin pouring sealant Pending CN110577813A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111303813A (en) * 2020-04-22 2020-06-19 中国工程物理研究院电子工程研究所 Room temperature curing pouring sealant for precise electronic components and use method thereof
CN111675989A (en) * 2019-12-26 2020-09-18 上海多迪高分子材料有限公司 Low-stress epoxy pouring sealant and preparation method and use method thereof
CN112812726A (en) * 2021-01-07 2021-05-18 东莞市新懿电子材料技术有限公司 Solid filling adhesive for large-size chip bottom filling and preparation method thereof
CN113637441A (en) * 2021-08-12 2021-11-12 长春艾德斯新材料有限公司 Epoxy resin adhesive capable of being rapidly cured at room temperature and preparation method thereof

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CN108546535A (en) * 2018-04-28 2018-09-18 上海回天新材料有限公司 A kind of epoxyn of high elongation at tear

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CN107286888A (en) * 2017-07-28 2017-10-24 上海回天新材料有限公司 A kind of epoxyn of low surface tension
CN107418498A (en) * 2017-09-11 2017-12-01 杭州之江有机硅化工有限公司 A kind of elastic epoxy fire-proof potting compound and preparation method thereof
CN108546535A (en) * 2018-04-28 2018-09-18 上海回天新材料有限公司 A kind of epoxyn of high elongation at tear

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111675989A (en) * 2019-12-26 2020-09-18 上海多迪高分子材料有限公司 Low-stress epoxy pouring sealant and preparation method and use method thereof
CN111303813A (en) * 2020-04-22 2020-06-19 中国工程物理研究院电子工程研究所 Room temperature curing pouring sealant for precise electronic components and use method thereof
CN111303813B (en) * 2020-04-22 2022-02-18 中国工程物理研究院电子工程研究所 A room temperature curing potting glue for precision electronic components and using method thereof
CN112812726A (en) * 2021-01-07 2021-05-18 东莞市新懿电子材料技术有限公司 Solid filling adhesive for large-size chip bottom filling and preparation method thereof
CN113637441A (en) * 2021-08-12 2021-11-12 长春艾德斯新材料有限公司 Epoxy resin adhesive capable of being rapidly cured at room temperature and preparation method thereof

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Application publication date: 20191217