CN105315944B - A kind of environmental-protection flame-retardant epoxy resin adhesive and preparation method thereof - Google Patents
A kind of environmental-protection flame-retardant epoxy resin adhesive and preparation method thereof Download PDFInfo
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- CN105315944B CN105315944B CN201510823166.8A CN201510823166A CN105315944B CN 105315944 B CN105315944 B CN 105315944B CN 201510823166 A CN201510823166 A CN 201510823166A CN 105315944 B CN105315944 B CN 105315944B
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Abstract
The invention discloses a kind of environmental-protection flame-retardant epoxy resin adhesive, in parts by weight, including following components：50 80 parts of epoxy resin, 40 50 parts of polyamide, 5 10 parts of acrylonitrile styrene acrylic ester copolymer, 10 15 parts of (2,3 glycidyl) chlorinated isocyanurates, 25 parts of magnesium hydroxide, 13 parts of boron nitride, 5 15 parts of curing agent, 5 10 parts of diluent.The invention also discloses the preparation method of the epoxy resin adhesive.The adhesive fire resistance is good, and adhesive property is strong, nontoxic, and environmental protection, mechanical property is good, wear-resisting, high temperature resistant, and preparation method is simple, and cost is low.
Description
Technical field：
The present invention relates to adhesive technical field, is specifically related to a kind of environment-friendly epoxy Resin adhesive.
Background technology：
Epoxy resin adhesive is known as the title of " all-purpose adhesive ".It is developed since 19 beginning of the twenties in the end of the century, it is existing away from the present
The history of more than 100 years, it is a kind of preparation technology more maturation, adhesive of excellent in mechanical performance.But modern adhesive except
Beyond excellent mechanical property, good corrosion resistance, environmental protection, nontoxic it is also desirable to have, it is often more important that also need to have
There is good anti-flammability, could so ensure the security of the lives and property of people to greatest extent.
It is to add appropriate fire retardant to improve the most frequently used method of epoxide-resin glue fire resistance.The fire-retardant science in China rises
Walk it is later, and mainly with halogen system it is fire-retardant based on, account for the 80% of whole fire retardant, and the easy inorganic system of fire retardant external at present
Based on, overall 50%-60% is accounted for, mainly based on magnesium hydroxide, aluminium hydroxide.Halogen system is fire-retardant because its dosage is few, fire-retardant effect
Rate is high and has a wide range of application, and turns into the main flow in market, but it is fire-retardant while also produce substantial amounts of corrosivity and toxic gas, make
Its application is extremely limited.At present phosphonium flame retardant for the majority of ethoxyline resin antiflaming, its have low halogen, Halogen,
The characteristic of low toxicity, the characteristics of its dosage is few, efficiency high, received much concern in flame retardant area, but phosphorus flame retardant smoke amount is big
And itself is poisonous, is liquid at normal temperatures, can be leaked out from waste material, so as to be polluted to base material,
The content of the invention：
It is an object of the invention to provide a kind of environmental-protection flame-retardant epoxy resin adhesive, its fire resistance is good, adhesive property
By force, nontoxic, environmental protection, mechanical property is good, wear-resisting, high temperature resistant, and preparation method is simple, and cost is low.
It is a further object to provide the preparation method of the epoxy resin adhesive.
To achieve the above object, the present invention uses following technical scheme：
A kind of environmental-protection flame-retardant epoxy resin adhesive, in parts by weight, including following components：
Epoxy resin 50-80 parts, polyamide 40-50 parts,
Acrylonitrile-styrene-acrylic ester copolymer 5-10 parts,
(2,3- glycidyl) chlorinated isocyanurates 10-15 parts,
Magnesium hydroxide 2-5 parts, boron nitride 1-3 parts,
Curing agent 5-15 parts, diluent 5-10 parts.
As the preferred of above-mentioned technical proposal, a kind of environmental-protection flame-retardant epoxy resin adhesive, in parts by weight, including with
Lower component：
80 parts of epoxy resin, 40 parts of polyamide,
10 parts of acrylonitrile-styrene-acrylic ester copolymer,
12 parts of (2,3- glycidyl) chlorinated isocyanurates,
3 parts of magnesium hydroxide, 2 parts of boron nitride,
10 parts of curing agent, 8 parts of diluent.
As the preferred of above-mentioned technical proposal, the epoxy resin is one in nitrogen-containing epoxy thermoset, halogen-free epoxy resin
Kind or two kinds of mixing.
As the preferred of above-mentioned technical proposal, the boron nitride is hexagonal boron nitride, and its particle size is 1-2 μm.
As the preferred of above-mentioned technical proposal, the curing agent is Amino End Group dimethyl silicone polymer, diformazan two to amino
Phenyl silane, the dimethyl silicone polymer of Amino End Group positive group two, methyl tetrahydrophthalic anhydride, 4,4 '-MDA
In one or more mixing.
As the preferred of above-mentioned technical proposal, the diluent is methyl-silicone oil, tung oil, ethyl acetate, linseed oil, turpentine
One or more mixing in oil.
A kind of preparation method of environmental-protection flame-retardant epoxy resin adhesive, comprises the following steps：
(1) epoxy resin, polyamide are mixed, are added in autoclave, at 40-60 DEG C, mix 20-30min,
Boron nitride, diluent are added, under 500-1000W power, ultrasonic 1-2h, obtains mixed material；
(2) in the mixed material obtained to step (1), acrylonitrile-styrene-acrylic ester copolymer, (2,3- rings are added
Oxygen propyl group) chlorinated isocyanurates, at 50-60 DEG C, 30-60min is incubated, is cooled to room temperature, magnesium hydroxide, curing agent is added, stirs
Mix well mixed, obtain environmental-protection flame-retardant epoxy resin adhesive.
As the preferred of above-mentioned technical proposal, in step (1), the ultrasonic power is 900W, the ultrasonic time
For 1.5h.
The invention has the advantages that：
Polyamide and epoxy resin compatibility are good, and polyamide is heat-resist, and anti-wear performance is excellent, can be effective
Improve the mechanical property and physical property of epoxy resin adhesive；Under conditions of ultrasound, hexagonal boron nitride is stripped into nanometer
Piece, resin is filled up between layers, the boron nitride nanosheet thermal conductivity after stripping is good, can effectively improve the fire-retardant of adhesive
Property, boron nitride, magnesium hydroxide it is compound so that the epoxy resin adhesive anti-flammability being prepared reaches UL-94V-0 levels.
Epoxy resin adhesive prepared by the present invention, paint having no volatile substances are nontoxic, are advantageous to environmental protection, and preparation side
Method is simple, and cost is low.
Embodiment：
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
The present invention is released, any restriction will not be formed to the present invention.
Embodiment 1
A kind of environmental-protection flame-retardant epoxy resin adhesive, in parts by weight, including following components：
50 parts of epoxy resin, 40 parts of polyamide,
5 parts of acrylonitrile-styrene-acrylic ester copolymer,
10 parts of (2,3- glycidyl) chlorinated isocyanurates,
2 parts of magnesium hydroxide, 1 part of boron nitride,
5 parts of curing agent, 5 parts of diluent.
Its preparation method comprises the following steps：
(1) epoxy resin, polyamide are mixed, are added in autoclave, at 40 DEG C, mixed 20min, add nitrogen
Change boron, diluent, under 500W power, ultrasonic 1h, obtain mixed material；
(2) in the mixed material obtained to step (1), acrylonitrile-styrene-acrylic ester copolymer, (2,3- rings are added
Oxygen propyl group) chlorinated isocyanurates, at 50 DEG C, 30min is incubated, is cooled to room temperature, magnesium hydroxide, curing agent is added, is stirred
Uniformly, environmental-protection flame-retardant epoxy resin adhesive is obtained.
Embodiment 2
A kind of environmental-protection flame-retardant epoxy resin adhesive, in parts by weight, including following components：
80 parts of epoxy resin, 50 parts of polyamide,
10 parts of acrylonitrile-styrene-acrylic ester copolymer,
15 parts of (2,3- glycidyl) chlorinated isocyanurates,
5 parts of magnesium hydroxide, 3 parts of boron nitride,
15 parts of curing agent, 10 parts of diluent.
Its preparation method comprises the following steps：
(1) epoxy resin, polyamide are mixed, are added in autoclave, at 60 DEG C, mixed 30min, add nitrogen
Change boron, diluent, under 1000W power, ultrasonic 2h, obtain mixed material；
(2) in the mixed material obtained to step (1), acrylonitrile-styrene-acrylic ester copolymer, (2,3- rings are added
Oxygen propyl group) chlorinated isocyanurates, at 60 DEG C, 60min is incubated, is cooled to room temperature, magnesium hydroxide, curing agent is added, is stirred
Uniformly, environmental-protection flame-retardant epoxy resin adhesive is obtained.
Embodiment 3
A kind of environmental-protection flame-retardant epoxy resin adhesive, in parts by weight, including following components：
60 parts of epoxy resin, 42 parts of polyamide,
6 parts of acrylonitrile-styrene-acrylic ester copolymer,
11 parts of (2,3- glycidyl) chlorinated isocyanurates,
3 parts of magnesium hydroxide, 1.5 parts of boron nitride,
7 parts of curing agent, 6 parts of diluent.
Its preparation method comprises the following steps：
(1) epoxy resin, polyamide are mixed, are added in autoclave, at 45 DEG C, mixed 22min, add nitrogen
Change boron, diluent, under 600W power, ultrasonic 1.2h, obtain mixed material；
(2) in the mixed material obtained to step (1), acrylonitrile-styrene-acrylic ester copolymer, (2,3- rings are added
Oxygen propyl group) chlorinated isocyanurates, at 55 DEG C, 40min is incubated, is cooled to room temperature, magnesium hydroxide, curing agent is added, is stirred
Uniformly, environmental-protection flame-retardant epoxy resin adhesive is obtained.
Embodiment 4
A kind of environmental-protection flame-retardant epoxy resin adhesive, in parts by weight, including following components：
65 parts of epoxy resin, 44 parts of polyamide,
7 parts of acrylonitrile-styrene-acrylic ester copolymer,
12 parts of (2,3- glycidyl) chlorinated isocyanurates,
3.5 parts of magnesium hydroxide, 1.8 parts of boron nitride,
9 parts of curing agent, 7 parts of diluent.
Its preparation method comprises the following steps：
(1) epoxy resin, polyamide are mixed, are added in autoclave, at 50 DEG C, mixed 24min, add nitrogen
Change boron, diluent, under 700W power, ultrasonic 1.4h, obtain mixed material；
(2) in the mixed material obtained to step (1), acrylonitrile-styrene-acrylic ester copolymer, (2,3- rings are added
Oxygen propyl group) chlorinated isocyanurates, at 60 DEG C, 45min is incubated, is cooled to room temperature, magnesium hydroxide, curing agent is added, is stirred
Uniformly, environmental-protection flame-retardant epoxy resin adhesive is obtained.
Embodiment 5
A kind of environmental-protection flame-retardant epoxy resin adhesive, in parts by weight, including following components：
70 parts of epoxy resin, 46 parts of polyamide,
8 parts of acrylonitrile-styrene-acrylic ester copolymer,
13 parts of (2,3- glycidyl) chlorinated isocyanurates,
4 parts of magnesium hydroxide, 2 parts of boron nitride,
11 parts of curing agent, 8 parts of diluent.
Its preparation method comprises the following steps：
(1) epoxy resin, polyamide are mixed, are added in autoclave, at 55 DEG C, mixed 26min, add nitrogen
Change boron, diluent, under 800W power, ultrasonic 1.6h, obtain mixed material；
(2) in the mixed material obtained to step (1), acrylonitrile-styrene-acrylic ester copolymer, (2,3- rings are added
Oxygen propyl group) chlorinated isocyanurates, at 60 DEG C, 50min is incubated, is cooled to room temperature, magnesium hydroxide, curing agent is added, is stirred
Uniformly, environmental-protection flame-retardant epoxy resin adhesive is obtained.
Embodiment 6
A kind of environmental-protection flame-retardant epoxy resin adhesive, in parts by weight, including following components：
75 parts of epoxy resin, 48 parts of polyamide,
9 parts of acrylonitrile-styrene-acrylic ester copolymer,
13 parts of (2,3- glycidyl) chlorinated isocyanurates,
4.5 parts of magnesium hydroxide, 2.5 parts of boron nitride,
13 parts of curing agent, 9 parts of diluent.
Its preparation method comprises the following steps：
(1) epoxy resin, polyamide are mixed, are added in autoclave, at 55 DEG C, mixed 28min, add nitrogen
Change boron, diluent, under 900W power, ultrasonic 1.8h, obtain mixed material；
(2) in the mixed material obtained to step (1), acrylonitrile-styrene-acrylic ester copolymer, (2,3- rings are added
Oxygen propyl group) chlorinated isocyanurates, at 50 DEG C, 55min is incubated, is cooled to room temperature, magnesium hydroxide, curing agent is added, is stirred
Uniformly, environmental-protection flame-retardant epoxy resin adhesive is obtained.
Performance test is carried out to environmental-protection flame-retardant epoxy resin adhesive provided by the invention below.
Using the type glass cloth of alkali-free 7628 as reinforcing material, by impregnation, semi-solid preparation, suppressed in vacuum hotpressing machine, it is natural
Cooling and mould unloading, 130mm × 13mm × 1.6mm sample is obtained after cutting out, carry out performance test
(1) fire resistance
Table 1
From the point of view of table 1, epoxy resin adhesive fire resistance provided by the invention is good.
Claims (8)
- A kind of 1. environmental-protection flame-retardant epoxy resin adhesive, it is characterised in that in parts by weight, including following components：Epoxy resin 50-80 parts, polyamide 40-50 parts,Acrylonitrile-styrene-acrylic ester copolymer 5-10 parts,(2,3- glycidyl) chlorinated isocyanurates 10-15 parts,Magnesium hydroxide 2-5 parts, boron nitride 1-3 parts,Curing agent 5-15 parts, diluent 5-10 parts.
- A kind of 2. environmental-protection flame-retardant epoxy resin adhesive as claimed in claim 1, it is characterised in that in parts by weight, bag Include following components：80 parts of epoxy resin, 40 parts of polyamide,10 parts of acrylonitrile-styrene-acrylic ester copolymer,12 parts of (2,3- glycidyl) chlorinated isocyanurates,3 parts of magnesium hydroxide, 2 parts of boron nitride,10 parts of curing agent, 8 parts of diluent.
- 3. a kind of environmental-protection flame-retardant epoxy resin adhesive as claimed in claim 1, it is characterised in that the epoxy resin is One or both of nitrogen-containing epoxy thermoset, halogen-free epoxy resin mix.
- 4. a kind of environmental-protection flame-retardant epoxy resin adhesive as claimed in claim 1, it is characterised in that the boron nitride is six Square boron nitride, its particle size are 1-2 μm.
- 5. a kind of environmental-protection flame-retardant epoxy resin adhesive as claimed in claim 1, it is characterised in that the curing agent is end Amino polydimethyl siloxane, the p-aminophenyl base silane of diformazan two, the dimethyl silicone polymer of Amino End Group positive group two, methyl tetrahydrochysene are adjacent One or more mixing in phthalate anhydride, 4,4 '-MDA.
- 6. a kind of environmental-protection flame-retardant epoxy resin adhesive as claimed in claim 1, it is characterised in that the diluent is first One or more mixing in base silicone oil, tung oil, ethyl acetate, linseed oil, turpentine oil.
- 7. a kind of preparation method of environmental-protection flame-retardant epoxy resin adhesive as described in claim 1 to 6 is any, its feature exist In comprising the following steps：(1) epoxy resin, polyamide are mixed, are added in autoclave, at 40-60 DEG C, mixed 20-30min, add Boron nitride, diluent, under 500-1000W power, ultrasonic 1-2h, obtain mixed material；(2) in the mixed material obtained to step (1), acrylonitrile-styrene-acrylic ester copolymer, (2,3- epoxies third are added Base) chlorinated isocyanurates, at 50-60 DEG C, 30-60min is incubated, is cooled to room temperature, adds magnesium hydroxide, curing agent, stirring is mixed Close uniformly, obtain environmental-protection flame-retardant epoxy resin adhesive.
- A kind of 8. preparation method of environmental-protection flame-retardant epoxy resin adhesive as claimed in claim 7, it is characterised in that step (1) in, the ultrasonic power is 900W, and the ultrasonic time is 1.5h.
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| CN105925221A (en) * | 2016-05-06 | 2016-09-07 | 金宝丽科技（苏州）有限公司 | High-adhesiveness heat-conducting adhesive and preparation method thereof |
| CN105907359A (en) * | 2016-05-06 | 2016-08-31 | 金宝丽科技（苏州）有限公司 | High-power LED (light emitting diode) package heat conduction glue and preparation technology thereof |
| CN108342160A (en) * | 2018-02-05 | 2018-07-31 | 合肥市大卓电力有限责任公司 | A kind of Environment-friendlyadhesive adhesive and preparation method thereof |
| CN109355047B (en) * | 2018-09-25 | 2021-04-16 | 宿州学院 | High-flame-retardant heat-resistant epoxy resin adhesive |
| CN113025247B (en) * | 2021-03-17 | 2021-11-23 | 东莞市德聚胶接技术有限公司 | Low-water-absorption double-component thermosetting epoxy adhesive and preparation method and application thereof |
| CN113845331A (en) * | 2021-10-11 | 2021-12-28 | 镇江长江汽车内饰件有限公司 | Nanometer aerogel fire prevention felt for new energy automobile battery and processingequipment thereof |
| CN115384137A (en) * | 2022-06-15 | 2022-11-25 | 杭州汉美新材料有限公司 | Flame-retardant aluminum-plastic composite belt for coaxial cable and preparation method thereof |
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| CN102604330A (en) * | 2012-03-07 | 2012-07-25 | 天津大学 | Preparing method of epoxy resin composite material based on boron nitride nanoparticles |
| CN102791819A (en) * | 2010-03-15 | 2012-11-21 | 日本化药株式会社 | Heat-resistant adhesive |
| CN103694644A (en) * | 2013-12-30 | 2014-04-02 | 景旺电子科技(龙川)有限公司 | Epoxy resin composition, metal-based copper-clad plate and manufacturing method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102791819A (en) * | 2010-03-15 | 2012-11-21 | 日本化药株式会社 | Heat-resistant adhesive |
| CN102604330A (en) * | 2012-03-07 | 2012-07-25 | 天津大学 | Preparing method of epoxy resin composite material based on boron nitride nanoparticles |
| CN103694644A (en) * | 2013-12-30 | 2014-04-02 | 景旺电子科技(龙川)有限公司 | Epoxy resin composition, metal-based copper-clad plate and manufacturing method thereof |
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Effective date of registration: 20171207 Address after: 318000, three, 2-11 village gate, Baiyun Street, Jiaojiang District, Zhejiang, Taizhou Applicant after: Tao Zhenzhen Address before: 215000 Taishan road Jiangsu city Suzhou province high tech Zone No. 2 (Bo science and Technology Park pilot base in C district two floor) Applicant before: GUIDE (SUZHOU) FINE CHEMICAL CO., LTD. |
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Effective date of registration: 20190821 Address after: 214212 Nancaoxin Street, Wanshi Town, Yixing City, Jiangsu Province Patentee after: Yixing city Pulitai Electronic Materials Co. Ltd. Address before: 318000 No. 2-11, Santaimen Village, Baiyun Street, Jiaojiang District, Taizhou City, Zhejiang Province Patentee before: Tao Zhenzhen |