CN115785871A - Heat-cured flame-retardant epoxy resin single-component adhesive and preparation method thereof - Google Patents
Heat-cured flame-retardant epoxy resin single-component adhesive and preparation method thereof Download PDFInfo
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- CN115785871A CN115785871A CN202211715030.1A CN202211715030A CN115785871A CN 115785871 A CN115785871 A CN 115785871A CN 202211715030 A CN202211715030 A CN 202211715030A CN 115785871 A CN115785871 A CN 115785871A
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- epoxy resin
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- retardant
- heat
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 50
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 50
- 239000003063 flame retardant Substances 0.000 title claims abstract description 40
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000012205 single-component adhesive Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000945 filler Substances 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 239000004593 Epoxy Substances 0.000 claims abstract description 13
- 239000003085 diluting agent Substances 0.000 claims abstract description 12
- 239000000853 adhesive Substances 0.000 claims description 13
- 230000001070 adhesive effect Effects 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 13
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 12
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical group [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 claims description 7
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 7
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 5
- -1 alkyl glycidyl ether Chemical compound 0.000 claims description 4
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims description 4
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract 1
- 238000001723 curing Methods 0.000 description 12
- 238000001035 drying Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000003292 glue Substances 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000565 sealant Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000013007 heat curing Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
Abstract
The invention discloses a heat-cured flame-retardant epoxy resin single-component adhesive and a preparation method thereof, wherein the heat-cured flame-retardant epoxy resin single-component adhesive comprises the following raw materials of 50-200 parts of epoxy resin, 10-50 parts of epoxy diluent, 80-350 parts of flame-retardant filler, 5-25 parts of latent curing agent and 1-5 parts of accelerator.
Description
Technical Field
The invention belongs to the field of epoxy resin pouring sealant, and particularly relates to a heating-cured flame-retardant epoxy resin single-component adhesive and a preparation method thereof.
Background
At present, with the rapid development of domestic and foreign electronic industries, the flame retardant requirement for products is higher and higher, and for some special metal elements, the metal material per se has good heat conduction and heat dissipation, and on glue products for encapsulating the modules, the fast curing speed and certain flame retardant property are required, and the protection property is also excellent.
The conventional two-component pouring sealant needs to mix the AB component, and sometimes has the problem of poor flame retardant property of glue.
Disclosure of Invention
In order to solve the problems, the invention provides the heating curing flame-retardant epoxy resin single-component adhesive and the preparation method thereof, the operation is simple, the performances in all aspects are excellent, the encapsulation efficiency of the product can be effectively improved, and the flame-retardant performance of the adhesive is improved to reach the grade of 94V-0 under the condition of ensuring good bonding and sealing.
The technical scheme provided by the invention is as follows:
on one hand, the heat-cured flame-retardant epoxy resin single-component adhesive comprises the following components in parts by mass:
50-200 parts of epoxy resin, 10-50 parts of epoxy diluent, 80-350 parts of flame-retardant filler, 5-25 parts of latent curing agent and 1-5 parts of accelerator;
the flame-retardant filler is aluminum hydroxide, organic phosphorus nitrogen powder and aluminum oxide.
Further, the flame-retardant filler comprises the following components in parts by mass:
50-200 parts of aluminum hydroxide, 25-100 parts of organic phosphorus nitrogen powder and 5-50 parts of aluminum oxide.
Furthermore, the grain diameter of the aluminum hydroxide is 500-3000 meshes, the grain diameter of the organic phosphorus-nitrogen powder is 500-3000 meshes, and the grain diameter of the aluminum oxide is 15-25 mu m.
Further, the epoxy resin is bisphenol A epoxy resin with an epoxy value of 0.48-0.54, and the viscosity of the epoxy resin is 5000-20000cps at 25 ℃.
Furthermore, the epoxy diluent is one or a mixture of more than two of benzyl alcohol, propylene carbonate, dimethylbenzene and C12-C14 alkyl glycidyl ether.
Furthermore, the latent curing agent is powdery dicyandiamide, and the particle size of the powdery dicyandiamide is 500-3000 meshes.
Furthermore, the accelerant is modified powdery imidazole, and the particle size of the modified powdery imidazole is 1500-3000 meshes.
On the other hand, the preparation method of the heat-cured flame-retardant epoxy resin single-component adhesive comprises the following steps:
s1: 50-200 parts of epoxy resin, 10-50 parts of epoxy diluent, 80-350 parts of flame-retardant filler, 5-25 parts of latent curing agent and 1-5 parts of accelerator are dried at high temperature, cooled to room temperature and placed in a dry place for later use;
s2: dispersing and mixing the filler in the step S1 at a high speed to obtain an epoxy resin single component;
s3: and placing the epoxy resin single component into a module, baking for 60-80min at the temperature of 100-110 ℃, taking out, and cooling to room temperature to obtain a cured rubber block.
In conclusion, the beneficial effects of the invention are as follows:
the epoxy resin, the diluent, the filler and the like are uniformly mixed and dispersed, and then are mixed with the modified amine curing agent, so that the amine curing agent and the epoxy resin are subjected to a crosslinking reaction to form a three-dimensional network structure, and then the flame-retardant filler added in the system is added, so that the flame-retardant performance of the cured colloid can be improved to reach the flame-retardant grade of V-0.
Detailed Description
In order to enhance the understanding of the present invention, the present invention will be further described with reference to the following examples, which are only for the purpose of illustrating the present invention and are not to be construed as limiting the scope of the present invention.
The heat-cured flame-retardant epoxy resin single-component adhesive comprises the following components in parts by mass:
50-200 parts of epoxy resin, 10-50 parts of epoxy diluent, 80-350 parts of flame-retardant filler, 5-25 parts of latent curing agent and 1-5 parts of accelerator;
the flame-retardant filler comprises the following components in parts by mass:
50-200 parts of aluminum hydroxide with the grain diameter of 500-3000 meshes, 25-100 parts of organic phosphorus nitrogen powder with the grain diameter of 500-3000 meshes, 5-50 parts of aluminum oxide with the grain diameter of 15-25 mu m.
The epoxy resin is bisphenol A epoxy resin with an epoxy value of 0.48-0.54, and the viscosity of the epoxy resin is 5000-20000cps at 25 ℃.
The epoxy diluent is one or more of benzyl alcohol, propylene carbonate, xylene and C12-C14 alkyl glycidyl ether.
The latent curing agent is powdery dicyandiamide, and the particle size of the latent curing agent is 500-3000 meshes.
The accelerant is modified powdery imidazole, and the particle size of the accelerant is 1500-3000 meshes.
Specifically, the heat-cured flame-retardant epoxy resin single-component adhesive is formed by the cross-linking reaction of epoxy resin and a latent curing agent through an accelerator under the heating condition, and in the manufacturing process, the viscosity of the epoxy resin single-component adhesive is reduced by adding a diluent, and the flame retardance, the strength and other properties of the epoxy resin single-component adhesive are improved by adding a filler.
As for the materials and the system, the materials do not react with the materials such as metal plastic and the like, and can be applied to the materials, but the glue is often heated under the use condition, so the single-component glue is mainly used on metal modules, and the fire retardant is selected from halogen-free materials, does not release harmful gases during combustion, and meets the requirements of various aspects of environmental protection.
A preparation method of a heating-cured flame-retardant epoxy resin single-component adhesive comprises the following steps:
s1: 50-200 parts of epoxy resin, 10-50 parts of epoxy diluent, 80-350 parts of flame-retardant filler, 5-25 parts of latent curing agent and 1-5 parts of accelerator are dried at high temperature, cooled to room temperature and placed in a dry place for later use;
s2: dispersing and mixing the filler in the step S1 at a high speed to obtain an epoxy resin single component;
s3: placing the epoxy resin single component in a module, baking for 60-80min at the temperature of 100-110 ℃, then taking out, and cooling to room temperature to obtain a cured rubber block.
The invention is further illustrated by the following examples:
example 1
Taking 100 parts by mass of bisphenol A epoxy resin, 10 parts by mass of benzyl alcohol, 100 parts by mass of aluminum hydroxide, 30 parts by mass of organic phosphorus powder, 10 parts by mass of alumina powder, 10 parts by mass of dicyandiamide and 1 part by mass of accelerator, drying at high temperature, cooling to room temperature, and placing in a drying place for later use;
the filler is put into a dispersion machine and uniformly dispersed at a high speed to obtain the epoxy resin single-component adhesive;
and pouring the prepared single-component epoxy resin adhesive into a die with a specific groove depth of 3mm, baking for 60min in an environment at 100 ℃, taking out and cooling to normal temperature to obtain the cured sample adhesive sheet 1.
Example 2
Taking 100 parts by mass of bisphenol A epoxy resin, 20 parts by mass of a mixture of propylene carbonate and xylene, 120 parts by mass of aluminum hydroxide, 40 parts by mass of organic phosphorus powder, 10 parts by mass of alumina powder, 8 parts by mass of dicyandiamide and 1.1 parts by mass of accelerator, drying at high temperature, cooling to room temperature, and placing in a dry place for later use;
the filler is put into a dispersion machine and uniformly dispersed at a high speed to obtain the epoxy resin single-component adhesive;
and pouring the prepared single-component epoxy resin adhesive into a die with a specific groove depth of 3mm, baking for 70min in an environment of 110 ℃, taking out and cooling to normal temperature to obtain the cured sample adhesive sheet 2.
Example 3
Taking 90 parts by mass of bisphenol A epoxy resin, 10 parts by mass of C12-C14 alkyl glycidyl ether, 90 parts by mass of aluminum hydroxide, 40 parts by mass of organic phosphorus powder, 10 parts by mass of alumina powder, 9 parts by mass of dicyandiamide and 1.2 parts by mass of accelerator, drying at high temperature, cooling to room temperature, and placing in a drying place for later use;
the filler is put into a dispersion machine and uniformly dispersed at a high speed to obtain the epoxy resin single-component adhesive;
and pouring the prepared single-component epoxy resin adhesive into a die with a specific groove depth of 3mm, baking for 80min in an environment at 105 ℃, taking out and cooling to normal temperature to obtain a cured sample adhesive sheet 3.
The films 1, 2 and 3 obtained in the above examples were examined, and the examination results are shown in Table 1
TABLE 1
According to the detection results in the table 1, the heat curing flame retardant epoxy resin single component adhesive prepared by the components and the preparation method thereof can reach the flame retardant standard of V-0.
While the foregoing description shows and describes the preferred embodiments of the present invention, it is to be understood that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as described herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. The heat-cured flame-retardant epoxy resin single-component adhesive is characterized by comprising the following components in parts by mass:
50-200 parts of epoxy resin, 10-50 parts of epoxy diluent, 80-350 parts of flame-retardant filler, 5-25 parts of latent curing agent and 1-5 parts of accelerator;
the flame-retardant filler is aluminum hydroxide, organic phosphorus nitrogen powder and aluminum oxide.
2. The heat-curable flame-retardant epoxy resin one-component adhesive according to claim 1, wherein the flame-retardant filler comprises the following components in parts by mass:
50-200 parts of aluminum hydroxide, 25-100 parts of organic phosphorus nitrogen powder and 5-50 parts of aluminum oxide.
3. The heat-curable flame-retardant epoxy resin one-component adhesive according to claim 2, wherein the particle size of the aluminum hydroxide is 500-3000 mesh, the particle size of the organic phosphorus-nitrogen powder is 500-3000 mesh, and the particle size of the aluminum oxide is 15-25 μm.
4. The heat-curable flame-retardant epoxy resin one-component adhesive as claimed in claim 1, wherein the epoxy resin is bisphenol A epoxy resin having an epoxy value of 0.48-0.54, and the viscosity of the epoxy resin is 5000-20000cps at 25 ℃.
5. The heat curable flame retardant epoxy resin one-component adhesive according to claim 1, wherein the epoxy diluent is one or a mixture of more than two of benzyl alcohol, propylene carbonate, xylene, and C12-C14 alkyl glycidyl ether.
6. The heat-curable flame-retardant epoxy resin one-component adhesive according to claim 1, wherein the latent curing agent is powdered dicyandiamide having a particle size of 500-3000 mesh.
7. The one-component adhesive of claim 1, wherein the accelerator is modified powdered imidazole with a particle size of 1500-3000 mesh.
8. The preparation method of the heat-cured flame-retardant epoxy resin single-component adhesive is characterized by comprising the following steps of:
s1: 50-200 parts of epoxy resin, 10-50 parts of epoxy diluent, 80-350 parts of flame-retardant filler, 5-25 parts of latent curing agent and 1-5 parts of accelerator are dried at high temperature, cooled to room temperature and placed in a dry place for later use;
s2: dispersing and mixing the filler in the step S1 at a high speed to obtain an epoxy resin single component;
s3: placing the epoxy resin single component in a module, baking for 60-80min at the temperature of 100-110 ℃, then taking out, and cooling to room temperature to obtain a cured rubber block.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211715030.1A CN115785871A (en) | 2022-12-28 | 2022-12-28 | Heat-cured flame-retardant epoxy resin single-component adhesive and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211715030.1A CN115785871A (en) | 2022-12-28 | 2022-12-28 | Heat-cured flame-retardant epoxy resin single-component adhesive and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN115785871A true CN115785871A (en) | 2023-03-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211715030.1A Pending CN115785871A (en) | 2022-12-28 | 2022-12-28 | Heat-cured flame-retardant epoxy resin single-component adhesive and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102181252A (en) * | 2011-05-30 | 2011-09-14 | 烟台德邦科技有限公司 | Low-halogen single-component flame-retardant epoxy adhesive |
| CN102533192A (en) * | 2011-12-28 | 2012-07-04 | 烟台德邦电子材料有限公司 | Flame retardant high-heat-conductivity epoxy resin electronic adhesive glue |
| CN104559890A (en) * | 2015-01-21 | 2015-04-29 | 华南理工大学 | Environment-friendly flame-retardant heat-conducting glue and preparation method thereof |
-
2022
- 2022-12-28 CN CN202211715030.1A patent/CN115785871A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102181252A (en) * | 2011-05-30 | 2011-09-14 | 烟台德邦科技有限公司 | Low-halogen single-component flame-retardant epoxy adhesive |
| CN102533192A (en) * | 2011-12-28 | 2012-07-04 | 烟台德邦电子材料有限公司 | Flame retardant high-heat-conductivity epoxy resin electronic adhesive glue |
| CN104559890A (en) * | 2015-01-21 | 2015-04-29 | 华南理工大学 | Environment-friendly flame-retardant heat-conducting glue and preparation method thereof |
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