CN102276793B - High-temperature-resistant liquid anhydride curing agent and preparation method thereof - Google Patents
High-temperature-resistant liquid anhydride curing agent and preparation method thereof Download PDFInfo
- Publication number
- CN102276793B CN102276793B CN2011101972416A CN201110197241A CN102276793B CN 102276793 B CN102276793 B CN 102276793B CN 2011101972416 A CN2011101972416 A CN 2011101972416A CN 201110197241 A CN201110197241 A CN 201110197241A CN 102276793 B CN102276793 B CN 102276793B
- Authority
- CN
- China
- Prior art keywords
- curing agent
- parts
- epoxy resin
- temperature
- maleic anhydride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Epoxy Resins (AREA)
Abstract
The invention discloses a high-temperature-resistant liquid anhydride curing agent, comprising the following components in parts by weight: 45-55 parts of maleic anhydride, 5-15 parts of phenyl hydroxide, 33-35 parts of diethylene glycol, 4-6 parts of triethanolamine and 1-1.2 parts of concentrated sulphuric acid. The raw materials are mixed according to requirements and react to generate the curing agent disclosed by the invention, then the curing agent disclosed by the invention can cure epoxy resin at the high temperature of 150 DEG C after being subjected to glue mixing with epoxy resin, the cured epoxy resin has high toughness and excellent mechanical strength, working temperature can resist 200 DEG C, insulation resistance is more than 1012 Omega, and the curing agent is applicable to filling and sealing constructions on a dry type transformer, a mutual inductor, a relay, a temperature sensor and various integrated circuits.
Description
Technical field
The present invention relates to a kind of solidifying agent, definite a kind of novel epoxy curing agent of saying so is specially a kind of high temperature resistant liquid anhydride curing agent.
Background technology
In the epoxy resin field, using maximum acid anhydride type curing agents both at home and abroad is Tetra hydro Phthalic anhydride and MALEIC ANHYDRIDE.647 liquid anhydride have been produced afterwards again, 70 and 80 liquid anhydride.Above-mentioned all acid anhydride type curing agents are after joining glue with epoxy resin and solidifying; 200 ℃ of high temperature of ability not; Though and toughness increases than the epoxy resin of self-vulcanizing; But not ideal enough, can not satisfy electronic enterprises to perfusion sealing material H.T. low-stress, and want resistant to elevated temperatures particular requirement.
Summary of the invention
The invention provides a kind of high temperature resistant liquid anhydride curing agent.This solidifying agent and epoxy resin join glue and solidify after material have the characteristics of high temperature resistant, H.T., low-stress.
The technical scheme that adopts for the present invention of realization above-mentioned purpose is following:
A kind of high temperature resistant liquid anhydride curing agent is characterized in that the weight part of its each component is:
MALEIC ANHYDRIDE 45-55
Phenol 5-15
Glycol ether 33-35
Trolamine 4-6
Vitriol oil 1-1.2.
Described liquid anhydride solidifying agent is characterized in that, the weight part of its each component is:
MALEIC ANHYDRIDE 50
Phenol 10
Glycol ether 34
Trolamine 5
The vitriol oil 1.
The preparation method of described high temperature resistant liquid anhydride curing agent is characterized in that, concrete operations are following:
(1) takes by weighing starting material by formula rate;
(2) add in the reaction kettle glycol ether that takes by weighing and trolamine and stirring earlier;
(3) with pouring in the reaction kettle after the phenol heating and melting, mix with glycol ether and trolamine in the still, stir;
(4) mixture of step (3) stirs after 30 minutes and to add after the vitriol oil continues to stir half a hour, and MALEIC ANHYDRIDE is added wherein in batches, constantly stirs;
(5), MALEIC ANHYDRIDE begins system is heated after all adding; When treating that material is warming up to 80 ℃, stop heating, treat that MALEIC ANHYDRIDE all melts back restir half a hour; Vacuumize and remove moisture content, treat to go out still by blowing when material is cooled to 50 ℃ of left and right sides naturally.
Beneficial effect of the present invention:
This solidifying agent has the pyritous characteristics, and this solidifying agent mixes with epoxy resin, and the epoxy resin after the curing has high temperature resistant, and working temperature can be anti-200 ℃; Has H.T. simultaneously; Low internal stress, physical strength is good, the characteristics that insulation resistivity is high; Can be applicable in the perfusion seal construction of rly., wave filter, TP and unicircuit; Also can be applied in the non-electron trade simultaneously, as making the epoxy resin technology article, metal or nonmetallic high temperature resistant bonding are repaired.
Embodiment
A kind of high temperature resistant liquid anhydride curing agent, the weight part of its each component is:
MALEIC ANHYDRIDE 50
Phenol 10
Glycol ether 34
Trolamine 5
The vitriol oil 1.
The preparation method of liquid anhydride solidifying agent is following:
(1) takes by weighing starting material by formula rate;
(2) add in the reaction kettle glycol ether that takes by weighing and trolamine and stirring earlier;
(3) with pouring in the reaction kettle after the phenol heating and melting, mix with glycol ether and trolamine in the still, stir;
(4) mixture of step (3) stirs after 30 minutes and to add after the vitriol oil continues to stir half a hour, and MALEIC ANHYDRIDE is added wherein in batches, constantly stirs;
(5), MALEIC ANHYDRIDE begins system is heated after all adding; When treating that material is warming up to 80 ℃, stop heating, treat that MALEIC ANHYDRIDE all melts back restir half a hour; Vacuumize and remove moisture content, treat to go out still by blowing when material is cooled to 50 ℃ of left and right sides naturally.
Application examples: during use, with epoxy resin E
44Or E
51With the epoxy curing agent of the present invention ratio batching of 100:60～90 by weight; Can be poured in the electronic product after mixing, and insert in the electrothermostat, 150 ℃ of heating were completely solidified in 5～7 hours; Working temperature can be anti-200 ℃, and insulation resistance is greater than 10
12Ω.
Epoxy resin after the curing has very high toughness, and physical strength is excellent, and working temperature can be anti-200 ℃, and insulation resistance is greater than 10
12Ω, the perfusion seal construction of suitable dry type transformer, mutual inductor, rly., TP and each adhesive integrated circuit.
High and new technology industrial development zone, Hefei City three brilliant electronics corporations successfully make resistant to elevated temperatures TP with epoxy curing agent of the present invention, have obtained good effect, have produced in batches and steady quality.
The concrete prescription that three brilliant electronics corporations use is following:
E
4480 parts in 100 parts of liquid anhydride solidifying agent of the present invention of 100 parts of ferric oxide red powder of epoxy resin
The TP that perfusion finishes is inserted in 150 ℃ of electrothermostats, after heating in 6 hours, is completely solidified.
Need the user of high temperature resistant high-toughness epoxy resin to construct with reference to the prescription and the curing process of three brilliant electronics corporations.
In non-electron trade, also can vigorously promote the use.Especially to metal or the repairing of nonmetallic high temperature resistant H.T. bonding etc., can both reach the ideal effect.
Claims (3)
1. high temperature resistant liquid anhydride curing agent is characterized in that the weight part of its each component is:
2. liquid anhydride solidifying agent according to claim 1 is characterized in that, the weight part of its each component is:
3. the preparation method of high temperature resistant liquid anhydride curing agent as claimed in claim 1 is characterized in that, concrete operations are following:
(1) takes by weighing starting material by formula rate;
(2) add in the reaction kettle glycol ether that takes by weighing and trolamine and stirring earlier;
(3) with pouring in the reaction kettle after the phenol heating and melting, mix with glycol ether and trolamine in the still, stir;
(4) mixture of step (3) stirs after 30 minutes and to add after the vitriol oil continues to stir half a hour, and MALEIC ANHYDRIDE is added wherein in batches, constantly stirs;
(5), MALEIC ANHYDRIDE begins system is heated after all adding; When treating that material is warming up to 80 ℃, stop heating, treat that MALEIC ANHYDRIDE all melts back restir half a hour; Vacuumize and remove moisture content, treat to go out still by blowing when material is cooled to 50 ℃ naturally.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101972416A CN102276793B (en) | 2011-07-14 | 2011-07-14 | High-temperature-resistant liquid anhydride curing agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101972416A CN102276793B (en) | 2011-07-14 | 2011-07-14 | High-temperature-resistant liquid anhydride curing agent and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102276793A CN102276793A (en) | 2011-12-14 |
| CN102276793B true CN102276793B (en) | 2012-11-28 |
Family
ID=45102566
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101972416A Expired - Fee Related CN102276793B (en) | 2011-07-14 | 2011-07-14 | High-temperature-resistant liquid anhydride curing agent and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102276793B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106881445B (en) * | 2017-02-08 | 2019-08-06 | 宁夏共享化工有限公司 | A kind of furan resin casting is with applying curing agent and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2807094B2 (en) * | 1990-12-27 | 1998-09-30 | 住友ベークライト株式会社 | Epoxy resin composition for optical semiconductor encapsulation |
-
2011
- 2011-07-14 CN CN2011101972416A patent/CN102276793B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| JP特开平4-363054A 1992.12.15 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102276793A (en) | 2011-12-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104726045B (en) | A kind of heat-resistant fireproof epoxy glue and preparation method thereof | |
| CN103979985B (en) | Environment-friendly converter bedding-face repairing material and preparation method thereof | |
| CN101735560B (en) | Casting mixture for epoxy casting transformer and preparation method thereof | |
| CN103113544B (en) | Phenolic aldehyde modified amine curing agent and preparation method thereof | |
| CN103570259A (en) | Geopolymer dry powder material as well as preparation method thereof | |
| WO2019015654A1 (en) | Epoxy resin and functional graphene integrated filtering ic and preparation method therefor | |
| CN104726047A (en) | Room-temperature cured high-temperature-resistant epoxy resin plugging material and preparation method thereof | |
| CN101358121A (en) | Preparation method of high temperature resistant epoxy adhesive capable of room temperature curing | |
| CN103694889B (en) | A kind of fire-resistant anticorrosion paint for wide variety of substrates and preparation method thereof | |
| CN107779147A (en) | A kind of high-strength epoxy honeycomb adhesive and preparation method thereof | |
| CN106280278A (en) | Dry-type transformer or dry type mutual inductor speed cured epoxy resin castable and preparation and application thereof | |
| CN102276792B (en) | Liquid anhydride curing agent capable of rapidly curing while heating and preparation method thereof | |
| CN102276793B (en) | High-temperature-resistant liquid anhydride curing agent and preparation method thereof | |
| CN109108213A (en) | Curing agent is used in a kind of casting | |
| CN103980669A (en) | Preparation method for epoxy resin board | |
| CN105504688B (en) | A kind of F grades of motor embedding composite ceramics/epoxy resin composite material and preparation method thereof | |
| CN105251938B (en) | Production technology for precoated sand | |
| CN105001825A (en) | Low temperature resisting epoxy resin adhesive and preparation method thereof | |
| CN105001818B (en) | Phenolic resin adhesive method is prepared using cresols production accessory substance | |
| CN105062390A (en) | Preparation method of adhesive for metal material packaging | |
| CN103911116A (en) | Adhesive for tile or steel brick | |
| CN103613359B (en) | Inorganic high-temperature adhesive for casting aluminum and aluminum alloy | |
| CN104356989A (en) | DMD (Dacron/Mylar/Dacron) flexible composite material adhesive | |
| CN102344545B (en) | Medium-temperature and quickly-cured colorless transparent epoxy resin curing agent and preparation method thereof | |
| CN106554746A (en) | A kind of wavy metal pipe binder being modified based on sodium silicate and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20121128 Termination date: 20130714 |