CN113278254A - Rapid curing flame-retardant insulating resin for fiber prepreg and preparation method thereof - Google Patents
Rapid curing flame-retardant insulating resin for fiber prepreg and preparation method thereof Download PDFInfo
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- CN113278254A CN113278254A CN202110539949.9A CN202110539949A CN113278254A CN 113278254 A CN113278254 A CN 113278254A CN 202110539949 A CN202110539949 A CN 202110539949A CN 113278254 A CN113278254 A CN 113278254A
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
- C08J2463/04—Epoxynovolacs
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- 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
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C08L2201/02—Flame or fire retardant/resistant
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- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses a fast curing flame-retardant insulating resin for a fiber prepreg, which comprises the following components in parts by mass: 60-80 parts of a resin component A; 4-8 parts of curing agent component B and 2-6 parts of accelerator component C; also comprises 1-2 parts of an auxiliary agent component D; 5-10 parts of flame retardant component E and 5-10 parts of insulating material component F; the assistant component D comprises wetting dispersant BYK-9076, defoamer BYK072 and coupling agent KH 560. The rapid curing flame-retardant insulating resin for the fiber prepreg disclosed by the invention has the advantages that the curing speed, the flame retardance and the insulativity are improved, the glass transition temperature Tg is not obviously influenced, and the mechanical property is not obviously reduced; moreover, the flame retardant property and the insulating property are excellent while the rapid curing and the mechanical property are considered.
Description
Technical Field
The invention belongs to the technical field of high-performance resin-based composite materials, and particularly relates to a resin for a fiber prepreg and a preparation method thereof.
Background
The carbon fiber/epoxy resin composite material has the advantages of light weight, high strength and the like. In the carbon fiber/epoxy resin composite material, matrix resin plays a role in adhering fibers and transferring load, and the quality of the performance of the matrix resin has a decisive influence on the performance of the composite material.
The existing resin material has longer curing time, the gel time at 120 ℃ needs 600s, and the gel time at 150 ℃ needs 220s, which seriously affects the production efficiency. In addition, carbon fiber/epoxy resin composite materials are increasingly applied to the light automobile industry and the electronic 3C industry, wherein the requirements on the insulation performance and the flame retardant performance of the materials are increasingly high, and the existing resin materials are difficult to meet the requirements on insulation and flame retardant while ensuring the mechanical performance.
Therefore, the development of a resin material for prepreg which is fast in curing, insulating and flame retardant is urgently needed, and the fast curing performance can meet the requirement of mass production, improve the production efficiency and reduce the production cost.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a fast-curing flame-retardant insulating resin for a fiber prepreg and a preparation method thereof. The purpose of the invention is realized by the following technical scheme:
a fast curing flame-retardant insulating resin for a fiber prepreg comprises the following components in parts by mass: 60-80 parts of a resin component A; 4-8 parts of curing agent component B and 2-6 parts of accelerator component C; it is characterized by also comprising 1-2 parts of an auxiliary agent component D; 5-10 parts of flame retardant component E and 5-10 parts of insulating material component F; the assistant component D comprises wetting dispersant BYK-9076, defoamer BYK072 and coupling agent KH 560.
Specifically, the resin component A comprises, by mass, 10-30% of glycidyl ether type epoxy resin, 10-30% of toughening type epoxy resin, 20-40% of phenolic aldehyde type epoxy resin, and 30-50% of phosphorus-containing epoxy resin.
Specifically, the glycidyl ether type epoxy resin comprises one or a mixture of more than two of NPEL-127 epoxy resin, NPEL-128 epoxy resin, NPEL-134 epoxy resin, NPES-901 epoxy resin, NPES-902 epoxy resin and NPES-904 epoxy resin.
Specifically, the toughened epoxy resin comprises one or a mixture of more than two of phenoxy resin JER1256, phenoxy resin PKHH and polyurethane modified epoxy ERS-133.
Specifically, the phenolic epoxy resin comprises one or a mixture of more than two of NPPN-631 epoxy resin, NPPN-638S epoxy resin and NPCN-704 epoxy resin.
Specifically, the phosphorus-containing epoxy resin is synthesized by DOPO and bisphenol A epoxy resin.
Specifically, the curing agent component B comprises at least one of Dyhard 100S, Dyhard 100SF, Ecure 14 and ultra-fine dicyandiamide.
Specifically, the accelerator component C consists of a modified organic urea accelerator and an imidazole accelerator, wherein the modified organic urea accelerator comprises the following components in percentage by mass: the imidazole accelerator is 1:1-5: 1.
More specifically, the organic urea promoter includes: UR500, PN-23 and PN-40, and the imidazole accelerator is diethyl tetramethyl imidazole.
Specifically, the flame retardant component E is an organic phosphorus-containing flame retardant.
More specifically, the organic phosphorus-containing flame retardant comprises at least one of phosphazene, melamine urate and ammonium polyphosphate.
Specifically, the insulating material component F includes at least one of aluminum hydroxide and glass beads.
The preparation method of the rapid-curing flame-retardant insulating resin is characterized by comprising the following steps of:
(1) uniformly mixing the flame retardant component E and the first part of the resin component A by a high-speed dispersion machine for later use, and adding a wetting dispersant in the auxiliary component D during mixing; uniformly mixing the insulating material component F and the second part of the resin component A by a high-speed dispersion machine for later use, and adding a wetting dispersant and a coupling agent in the auxiliary agent component D during mixing;
(2) heating the residual resin component A to 130 +/-5 ℃, stirring uniformly after the resin is completely dissolved, and adding the defoaming agent and the coupling agent in the auxiliary agent component D;
(3) and cooling, adding the curing agent component B and the accelerator component C, and stirring and mixing uniformly to obtain the finished resin.
The invention has the beneficial effects that: the viscosity is greatly improved while the curing performance is improved, and the glass transition temperature Tg is not obviously influenced; meanwhile, the mechanical property is not obviously reduced; moreover, the flame retardant property is excellent while the quick curing and the mechanical property are considered; moreover, the insulation performance test standard required in the field is passed.
Drawings
Fig. 1 is a side view of a rapid-curing flame-retardant insulating resin for a fiber prepreg provided by the present invention passing an insulation performance test.
Detailed Description
The embodiment provides a fast-curing flame-retardant insulating resin for a fiber prepreg, which comprises the following components in parts by mass: 60-80 parts of a resin component A; 4-8 parts of curing agent component B and 2-6 parts of accelerator component C; 1-2 parts of an auxiliary component D; 5-10 parts of flame retardant component E and 5-10 parts of insulating material component F.
The component A comprises 10-30% of glycidyl ether type epoxy resin, 10-30% of toughened epoxy resin, 20-40% of phenolic epoxy resin and 30-50% of phosphorus-containing epoxy resin by mass. More specifically, the glycidyl ether type epoxy resin includes one or a mixture of two or more of NPEL-127 epoxy resin, NPEL-128 epoxy resin, NPEL-134 epoxy resin, NPES-901 epoxy resin, NPES-902 epoxy resin, and NPES-904 epoxy resin. The toughened epoxy resin comprises one or a mixture of more than two of phenoxy resin JER1256, phenoxy resin PKHH and polyurethane modified epoxy ERS-133. The phenolic epoxy resin comprises one or more of NPPN-631 epoxy resin, NPPN-638S epoxy resin and NPCN-704 epoxy resin. The phosphorus-containing epoxy resin is synthesized by adopting DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) and bisphenol A epoxy resin.
Wherein the curing agent component B is dicyandiamide and comprises one or a mixture of more than two of Dyhard 100S, Dyhard 100SF, Ecure 14 and superfine dicyandiamide. The accelerator component C consists of a modified organic urea accelerator and an imidazole accelerator, wherein the modified organic urea accelerator comprises the following components in percentage by mass: the imidazole accelerator is 1:1-5: 1. The organic urea promoter also comprises one or a mixture of more than two of UR500, PN-23 and PN-40, and the imidazole promoter is diethyl tetramethyl imidazole.
Wherein the assistant component D comprises wetting dispersant BYK-9076, defoamer BYK072 and coupling agent KH 560. The flame retardant component E is an organic phosphorus-containing flame retardant, and specifically comprises one or a mixture of more than two of phosphazene, melamine urate and ammonium polyphosphate. The insulating material component F comprises at least one of aluminum hydroxide and glass beads.
The following embodiments of the present invention are further described with reference to specific matching ratios:
the first embodiment is as follows: the respective material selection and proportion of the resin component A, the curing agent component B, the accelerator component C, the auxiliary agent component D, the flame retardant component E and the insulating material component F are shown in the following table 1.
TABLE 1
Example two: the respective material selection and proportion of the resin component A, the curing agent component B, the accelerator component C, the auxiliary agent component D, the flame retardant component E and the insulating material component F are shown in the following table 2.
TABLE 2
Example three: the respective material selection and proportion of the resin component A, the curing agent component B, the accelerator component C, the auxiliary agent component D, the flame retardant component E and the insulating material component F are shown in the following table 3.
TABLE 3
Example four: the respective material selection and proportion of the resin component A, the curing agent component B, the accelerator component C, the auxiliary agent component D, the flame retardant component E and the insulating material component F are shown in the following table 4.
TABLE 4
Based on the above embodiments of material selection and proportioning, the preparation method of the fast curing flame-retardant insulating resin comprises the following steps,
(1) uniformly mixing the flame retardant component E and the first part of the resin component A by a high-speed dispersion machine for later use, and adding a wetting dispersant in the auxiliary component D during mixing; uniformly mixing the insulating material component F and the second part of the resin component A by a high-speed dispersion machine for later use, and adding a wetting dispersant and a coupling agent in the auxiliary agent component D during mixing;
(2) heating the residual resin component A to 130 +/-5 ℃, stirring uniformly after the resin is completely dissolved, and adding the defoaming agent and the coupling agent in the auxiliary agent component D;
(3) and cooling, adding the curing agent component B and the accelerator component C, and stirring and mixing uniformly to obtain the finished resin. Wherein, the temperature in the step (3) is reduced to 65-75 ℃.
Compared with the common resin, the fast-curing flame-retardant insulating resin prepared by the method has shorter gel time and more excellent curing characteristics, and is detailed in the following table 5.
TABLE 5
Unexpectedly, the viscosity of the fast-curing flame-retardant insulating resin provided by the invention is greatly improved while the curing performance is improved, and the glass transition temperature Tg is not significantly influenced.
In addition, some existing resin materials often greatly lose mechanical properties while meeting the requirement of rapid curing. The mechanical properties of the fast-curing flame-retardant insulating resin prepared by the invention are not obviously reduced compared with those of common resins, and the fast-curing flame-retardant insulating resin is shown in the following table 6.
| Fast curing resins | General resin | |
| Tensile strength | 79Mpa | 85Mpa |
| Tensile modulus | 2.8Gpa | 2.7Gpa |
| Bending strength | 130Mpa | 134Mpa |
| Flexural modulus | 3.0Gpa | 3.0Gpa |
| Elongation at break | 3.7 | 4.0 |
TABLE 6
Moreover, the prepared fast curing flame-retardant insulating resin has excellent flame-retardant performance while giving consideration to fast curing and mechanical properties; furthermore, the standard of the insulation performance test which is required to be severe in the field is passed, and is shown in fig. 1.
The storage conditions and the molding process of the rapidly-cured flame-retardant insulating resin are described as follows:
storage conditions were as follows: the prepreg prepared by the resin has good bonding property and long storage period, and can still meet the requirements of a paving and forming process after being placed at room temperature for 30 days.
The molding process comprises the following steps: the prepreg prepared by the rapid curing flame-retardant resin is cured and molded as follows: the prepreg is laminated alternately according to the longitude and latitude sequence, then the preformed product is put into a hot die, the pressure is pressurized and cured for 5min, the pressure of a hot press is 0.3-2MPA, the pressure is removed after the completion, the direct hot die opening (which can effectively improve the production efficiency and reduce the production cost) is proved by tests, when the mold-entering temperature is 130 ℃, the temperature of the press is 150 ℃, the die is put into the press for timing, the molding can be completed within 4min, and the product is obtained by die opening.
The above embodiments are merely for full disclosure and not for limitation, and any replacement of equivalent technical features, which can be obtained without inventive work based on the gist of the present invention, should be construed as the scope of the present disclosure.
Claims (13)
1. A fast curing flame-retardant insulating resin for a fiber prepreg comprises the following components in parts by mass: 60-80 parts of a resin component A; 4-8 parts of curing agent component B and 2-6 parts of accelerator component C; it is characterized by also comprising 1-2 parts of an auxiliary agent component D; 5-10 parts of flame retardant component E and 5-10 parts of insulating material component F; the assistant component D comprises wetting dispersant BYK-9076, defoamer BYK072 and coupling agent KH 560.
2. The fast-curing flame-retardant insulating resin for a fiber prepreg according to claim 1, wherein the resin component A consists of 10 to 30% by mass of a glycidyl ether type epoxy resin, 10 to 30% by mass of a toughening type epoxy resin, 20 to 40% by mass of a phenol type epoxy resin, and 30 to 50% by mass of a phosphorus type epoxy resin.
3. The fast-curing flame-retardant insulating resin for a fiber prepreg according to claim 2, wherein the glycidyl ether type epoxy resin comprises one or a mixture of two or more of NPEL-127 epoxy resin, NPEL-128 epoxy resin, NPEL-134 epoxy resin, NPES-901 epoxy resin, NPES-902 epoxy resin, and NPES-904 epoxy resin.
4. The fast-curing flame-retardant insulating resin for a fiber prepreg according to claim 2, wherein the toughening epoxy resin comprises one or a mixture of two or more of a phenoxy resin JER1256, a phenoxy resin PKHH and a polyurethane-modified epoxy ERS-133.
5. The fast-curing flame-retardant insulating resin for fiber prepreg according to claim 2, wherein the phenolic epoxy resin comprises one or a mixture of two or more of NPPN-631 epoxy resin, NPPN-638S epoxy resin, and NPCN-704 epoxy resin.
6. The fast-curing flame-retardant insulating resin for fiber prepreg according to claim 2, wherein the phosphorus-containing epoxy resin is synthesized using DOPO and bisphenol A type epoxy resin.
7. The fast-curing flame-retardant insulating resin for a fiber prepreg according to claim 1, wherein the curing agent component B comprises at least one of Dyhard 100S, Dyhard 100SF, cure 14 and ultra-fine dicyandiamide.
8. The fast-curing flame-retardant insulating resin for the fiber prepreg according to claim 1, wherein the accelerator component C consists of a modified organic urea accelerator and an imidazole accelerator, and the modified organic urea accelerator comprises the following components in percentage by mass: the imidazole accelerator is 1:1-5: 1.
9. The fast curing flame retardant insulating resin for fiber prepreg according to claim 8, wherein the organic urea accelerator comprises: UR500, PN-23 and PN-40, and the imidazole accelerator is diethyl tetramethyl imidazole.
10. The rapid-curing flame-retardant insulating resin for fiber prepregs according to any one of claims 1 to 9, wherein the flame retardant component E is an organic phosphorus-containing flame retardant.
11. The fast curing flame retardant insulating resin for fiber prepreg according to claim 10, wherein the organic phosphorus-containing flame retardant comprises at least one of phosphazene, melamine urate, ammonium polyphosphate.
12. The rapid-curing flame-retardant insulating resin for fiber prepregs according to any one of claims 1 to 9, wherein the insulating material component F comprises at least one of aluminum hydroxide and glass beads.
13. A method for preparing the fast-curing flame-retardant insulating resin according to any one of claims 1 to 11, comprising the steps of:
(1) uniformly mixing the flame retardant component E and the first part of the resin component A by a high-speed dispersion machine for later use, and adding a wetting dispersant in the auxiliary component D during mixing; uniformly mixing the insulating material component F and the second part of the resin component A by a high-speed dispersion machine for later use, and adding a wetting dispersant and a coupling agent in the auxiliary agent component D during mixing;
(2) heating the residual resin component A to 130 +/-5 ℃, stirring uniformly after the resin is completely dissolved, and adding the defoaming agent and the coupling agent in the auxiliary agent component D;
(3) and cooling, adding the curing agent component B and the accelerator component C, and stirring and mixing uniformly to obtain the finished resin.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115386284A (en) * | 2022-10-12 | 2022-11-25 | 广东粤港澳大湾区国家纳米科技创新研究院 | Fireproof insulating material and coating method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033550A (en) * | 2017-03-07 | 2017-08-11 | 珠海辉帛复合材料有限公司 | A kind of fiber prepreg material fast-curing resin and preparation method thereof |
| CN109535660A (en) * | 2018-12-18 | 2019-03-29 | 深圳航天科技创新研究院 | A kind of fire-retardant prepreg resin of the rapid curing that viscosity is controllable and preparation method thereof |
| CN112625284A (en) * | 2020-12-11 | 2021-04-09 | 江苏恒神股份有限公司 | Continuous fiber reinforced thermosetting flame-retardant prepreg and preparation method thereof |
-
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- 2021-05-18 CN CN202110539949.9A patent/CN113278254A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033550A (en) * | 2017-03-07 | 2017-08-11 | 珠海辉帛复合材料有限公司 | A kind of fiber prepreg material fast-curing resin and preparation method thereof |
| CN109535660A (en) * | 2018-12-18 | 2019-03-29 | 深圳航天科技创新研究院 | A kind of fire-retardant prepreg resin of the rapid curing that viscosity is controllable and preparation method thereof |
| CN112625284A (en) * | 2020-12-11 | 2021-04-09 | 江苏恒神股份有限公司 | Continuous fiber reinforced thermosetting flame-retardant prepreg and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115386284A (en) * | 2022-10-12 | 2022-11-25 | 广东粤港澳大湾区国家纳米科技创新研究院 | Fireproof insulating material and coating method thereof |
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Application publication date: 20210820 |