CN112358707A - Flame-retardant epoxy resin structural foam composition - Google Patents
Flame-retardant epoxy resin structural foam composition Download PDFInfo
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- CN112358707A CN112358707A CN202011280881.9A CN202011280881A CN112358707A CN 112358707 A CN112358707 A CN 112358707A CN 202011280881 A CN202011280881 A CN 202011280881A CN 112358707 A CN112358707 A CN 112358707A
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/104—Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof
- C08J9/105—Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof containing sulfur
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/26—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment
- C08J2423/28—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment by reaction with halogens or halogen-containing compounds
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- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- 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
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C08K5/00—Use of organic ingredients
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- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/45—Heterocyclic compounds having sulfur in the ring
- C08K5/46—Heterocyclic compounds having sulfur in the ring with oxygen or nitrogen in the ring
- C08K5/47—Thiazoles
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Abstract
The invention discloses a flame-retardant epoxy resin structural foam composition which is prepared from the following raw materials in parts by weight: 40-60 parts of solid epoxy resin, 5-15 parts of brominated butyl rubber, 1-5 parts of curing agent, 0.5-2 parts of curing accelerator, 1-10 parts of foaming agent, 0.1-1 part of foaming accelerator, 0.1-1 part of vulcanization accelerator and 10-40 parts of flame-retardant filler. The flame-retardant epoxy resin structural foam composition can be baked and cured at 170 ℃ for 20min, and a cured product has the advantages of low density, high strength and good flame retardance and also has good bonding strength and weather resistance on metals. The automobile body upright post is placed in an automobile body cavity, and after being baked in a coating workshop, the automobile body upright post is expanded and solidified, so that the impact force of each direction on the automobile body upright post can be effectively resisted, and the strength of the upright post is enhanced.
Description
Technical Field
The invention relates to structural foam for automobiles, in particular to a flame-retardant epoxy resin structural foam composition.
Background
In recent years, the weight reduction of automobiles is an effective measure for reducing automobile emission and improving combustion efficiency, and is also a main direction of the development of automobile materials. However, while the purpose of light weight of the whole vehicle is achieved, the safety of the whole vehicle is also a main factor which must be considered. Whether the vehicle structure can be kept intact is related to the safety of the vehicle and the lives of passengers, and in a general collision experiment, the more intact the vehicle body structure can be kept, which indicates that the safety of the vehicle is higher. When an automobile is involved in a side collision, a pillar such as an a pillar, a B pillar, or a C pillar of the automobile is one of the most important rigid structures of the automobile, and the strength thereof greatly affects the crashworthiness of the side surface of the automobile. Since a break in a collision undoubtedly carries a great life risk to the passenger compartment, most vehicle assemblies adopt different methods for resisting deformation and breakage problems of side impact in the current design of the body pillar structure. One way of reinforcement is to add a foam material such as epoxy resin to the cavity to reinforce it. However, the epoxy resin is flammable, so that the prepared foaming material is easier to burn, and hidden danger is brought to the safety of automobiles. Chinese patent CN105694363A prepares a functional structural foam material for an automobile cavity, which has good cavity reinforcing operation but no flame retardant effect.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a flame-retardant epoxy resin structural foam composition, the coating is cured and foamed at 170 ℃ for 20min, and the foam has strong rigidity, is not easy to burn and has good safety.
In order to achieve the above object, according to the flame retardant epoxy resin structural foam composition of the present invention, the epoxy resin provides rigidity to the foam, and the combustion speed of the foam can be significantly reduced by the combined action of the brominated butyl rubber and the flame retardant filler.
The invention adopts the following specific technical scheme: the flame-retardant epoxy resin structural foam composition is characterized by comprising the following raw materials in parts by weight: 40-60 parts of solid epoxy resin, 5-15 parts of brominated butyl rubber, 1-5 parts of curing agent, 0.5-2 parts of curing accelerator, 1-10 parts of foaming agent, 0.1-1 part of foaming accelerator, 0.1-1 part of vulcanization accelerator and 10-40 parts of flame-retardant filler.
The invention has the beneficial effects that: the flame-retardant epoxy resin structural foam composition can be baked and cured at 170 ℃ for 20min, and a cured product has the advantages of low density, high strength and good flame retardance and also has good bonding strength and weather resistance on metals. The automobile body upright post is placed in an automobile body cavity, and after being baked in a coating workshop, the automobile body upright post is expanded and solidified, so that the impact force of each direction on the automobile body upright post can be effectively resisted, and the strength of the upright post is enhanced.
Detailed Description
The present invention will be described in further detail with reference to examples, but the formulation of the flame retardant epoxy resin structural foam composition of the present invention is not limited to the examples.
The invention adopts the following specific technical scheme: the flame-retardant epoxy resin structural foam composition is characterized by comprising the following raw materials in parts by weight: 40-60 parts of solid epoxy resin, 5-15 parts of brominated butyl rubber, 1-5 parts of curing agent, 0.5-2 parts of curing accelerator, 1-10 parts of foaming agent, 0.1-1 part of foaming accelerator, 0.1-1 part of vulcanization accelerator and 10-40 parts of flame-retardant filler.
The flame-retardant epoxy resin structural foam composition is produced by adopting the following process: weighing 40-60 parts of solid epoxy resin and 5-15 parts of brominated butyl rubber according to a mass ratio, putting into an internal mixer at 80-120 ℃, adding 10-40 parts of flame-retardant filler for internal mixing for a period of time after the materials are molten, and finally adding 1-5 parts of curing agent, 0.5-2 parts of curing accelerator, 1-10 parts of foaming agent, 0.1-1 part of foaming accelerator and 0.1-1 part of vulcanization accelerator for mixing for a period of time and then discharging; and extruding and granulating at the temperature of 80-120 ℃ by using a granulator to obtain the flame-retardant epoxy resin structural foam composition.
Preferably, the solid epoxy resin is bisphenol A epoxy resin with the softening point of 60-120 ℃.
Preferably, the curing agent is dicyandiamide.
Preferably, the curing accelerator is either imidazole or an imidazole adduct or a combination of both.
Preferably, the foaming agent is any one of Azodicarbonamide (AC) or 4,4' -oxybis-benzenesulfonylhydrazide (OBSH).
Preferably, the foaming promoter is any one or a combination of two of zinc oxide or zinc stearate.
Preferably, the vulcanization accelerator is any one or a combination of two of thiazole vulcanization accelerators M or DM.
Preferably, the flame retardant filler is any one or a combination of two of aluminum hydroxide or magnesium hydroxide.
Example 1
Weighing 50 parts of solid epoxy resin and 10 parts of brominated butyl rubber according to the mass ratio, putting the solid epoxy resin and the brominated butyl rubber into an internal mixer at 90 ℃, adding 18 parts of aluminum hydroxide and 13.3 parts of magnesium hydroxide after melting the materials, internally mixing for a period of time, and finally adding 3 parts of dicyandiamide, 1 part of imidazole, 4 parts of OBSH, 0.2 part of zinc oxide and 0.5 part of vulcanization accelerator M, mixing for a period of time, and then discharging; and extruding and granulating at the temperature of 90 ℃ by using a granulator to obtain the flame-retardant epoxy resin structural foam composition. The coating is placed in an oven at 170 ℃ for 20 minutes, then is solidified and foamed, is cooled to room temperature and is placed for 24 hours, and then performance test is carried out.
Example 2
Weighing 60 parts of solid epoxy resin and 5 parts of brominated butyl rubber according to a mass ratio, putting the solid epoxy resin and the brominated butyl rubber into an internal mixer at 90 ℃, adding 25 parts of aluminum hydroxide for internal mixing for a period of time after the materials are molten, and finally adding 5 parts of dicyandiamide, 0.5 part of imidazole adduct, 4 parts of AC, 0.3 part of zinc oxide and 0.2 part of vulcanization accelerator DM for mixing for a period of time and then discharging; and extruding and granulating at the temperature of 90 ℃ by using a granulator to obtain the flame-retardant epoxy resin structural foam composition. The coating is placed in an oven at 170 ℃ for 20 minutes, then is solidified and foamed, is cooled to room temperature and is placed for 24 hours, and then performance test is carried out.
Example 3
Weighing 40 parts of solid epoxy resin and 15 parts of brominated butyl rubber according to the mass ratio, putting the materials into an internal mixer at the temperature of 90 ℃, adding 40 parts of magnesium hydroxide for internal mixing for a period of time after the materials are molten, and finally adding 1.5 parts of dicyandiamide; 0.5 part of an imidazole adduct; 2 parts of OBSH; 0.2 part of zinc stearate; 0.8 part of vulcanization accelerator M is mixed for a period of time and then discharged. And extruding and granulating at the temperature of 90 ℃ by using a granulator to obtain the flame-retardant epoxy resin structural foam composition. The coating is placed in an oven at 170 ℃ for 20 minutes, then is solidified and foamed, is cooled to room temperature and is placed for 24 hours, and then performance test is carried out.
Example 4
55 parts of solid epoxy resin and 7.5 parts of brominated butyl rubber are weighed according to the mass ratio and put into an internal mixer at the temperature of 90 ℃, 17.8 parts of aluminum hydroxide and 10 parts of magnesium hydroxide are added after the materials are melted and internally mixed for a period of time, and finally 3.5 parts of dicyandiamide, 0.5 part of imidazole, 5 parts of AC, 0.5 part of zinc oxide and 0.2 part of vulcanization accelerator DM are added and mixed for a period of time, and then the materials are discharged. And extruding and granulating at the temperature of 90 ℃ by using a granulator to obtain the flame-retardant epoxy resin structural foam composition. The coating is placed in an oven at 170 ℃ for 20 minutes, then is solidified and foamed, is cooled to room temperature and is placed for 24 hours, and then performance test is carried out.
Example 5
Weighing 45 parts of solid epoxy resin and 12 parts of brominated butyl rubber according to the mass ratio, putting the materials into an internal mixer at 90 ℃, adding 37 parts of aluminum hydroxide for internal mixing for a period of time after the materials are molten, and finally adding 1.5 parts of dicyandiamide, 0.5 part of imidazole adduct, 3 parts of OBSH, 0.5 part of zinc oxide and 0.5 part of vulcanization accelerator M for mixing for a period of time and then discharging. And extruding and granulating at the temperature of 90 ℃ by using a granulator to obtain the flame-retardant epoxy resin structural foam composition. The coating is placed in an oven at 170 ℃ for 20 minutes, then is solidified and foamed, is cooled to room temperature and is placed for 24 hours, and then performance test is carried out.
The flame retardant epoxy resin structural foam compositions prepared in examples 1 to 5 were tested for their performance and the results are shown in table 1 below:
TABLE 1 Performance testing of flame retardant epoxy resin structural foam compositions
The test results of the examples 1 to 5 show that the flame-retardant epoxy resin structural foam composition has the burning speed of less than or equal to 5mm/min, the shear strength of more than 5MPa, the volume change rate of 36 to 78 percent, hard foam of a cured product and uniform pores. Have fire-retardant and cavity structure additional action concurrently, promoted the security of car greatly, be worth promoting.
Claims (8)
1. The flame-retardant epoxy resin structural foam composition is characterized by comprising the following raw materials in parts by weight:
40-60 parts of solid epoxy resin
5-15 parts of brominated butyl rubber
1-5 parts of curing agent
0.5-2 parts of curing accelerator
1-10 parts of foaming agent
0.1-1 part of foaming promoter
0.1-1 part of vulcanization accelerator
10-40 parts of flame-retardant filler.
2. The flame retarded epoxy resin structural foam composition according to claim 1 wherein: the solid epoxy resin is bisphenol A epoxy resin with a softening point of 60-120 ℃.
3. The flame retarded epoxy resin structural foam composition according to claim 1 wherein: the curing agent is dicyandiamide.
4. The flame retarded epoxy resin structural foam composition according to claim 1 wherein: the curing accelerator is one or the combination of two of imidazole or imidazole addition products.
5. The flame retarded epoxy resin structural foam composition according to claim 1 wherein: the foaming agent is any one of Azodicarbonamide (AC) or 4,4' -oxo-bis-benzenesulfonyl hydrazide (OBSH).
6. The flame retarded epoxy resin structural foam composition according to claim 1 wherein: the foaming accelerant is any one or the combination of two of zinc oxide or zinc stearate.
7. The flame retarded epoxy resin structural foam composition according to claim 1 wherein: the vulcanization accelerator is one or the combination of two of thiazole vulcanization accelerators M or DM.
8. The flame retarded epoxy resin structural foam composition according to claim 1 wherein: the flame-retardant filler is any one or the combination of two of aluminum hydroxide or magnesium hydroxide.
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| CN202011280881.9A CN112358707A (en) | 2020-11-16 | 2020-11-16 | Flame-retardant epoxy resin structural foam composition |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6403668B1 (en) * | 1999-05-28 | 2002-06-11 | Neo-Ex Lab, Inc. | Foam materials and foam precursor materials |
| CN105924902A (en) * | 2016-05-16 | 2016-09-07 | 贵州省材料产业技术研究院 | Thermally-expandable solid epoxy resin microcellular foam material and preparation method thereof |
| WO2017080134A1 (en) * | 2015-11-12 | 2017-05-18 | 广东生益科技股份有限公司 | Epoxy resin composition and use thereof |
| CN108752871A (en) * | 2018-05-30 | 2018-11-06 | 中国科学院化学研究所 | A kind of epoxy foams and preparation method thereof |
| CN109957185A (en) * | 2019-03-12 | 2019-07-02 | 天津市浩迪橡塑科技有限公司 | A kind of high fire-retardance destatics type butyl rubber composite damping material and preparation method thereof |
| CN111286159A (en) * | 2020-03-25 | 2020-06-16 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of light foam core material |
-
2020
- 2020-11-16 CN CN202011280881.9A patent/CN112358707A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6403668B1 (en) * | 1999-05-28 | 2002-06-11 | Neo-Ex Lab, Inc. | Foam materials and foam precursor materials |
| WO2017080134A1 (en) * | 2015-11-12 | 2017-05-18 | 广东生益科技股份有限公司 | Epoxy resin composition and use thereof |
| CN105924902A (en) * | 2016-05-16 | 2016-09-07 | 贵州省材料产业技术研究院 | Thermally-expandable solid epoxy resin microcellular foam material and preparation method thereof |
| CN108752871A (en) * | 2018-05-30 | 2018-11-06 | 中国科学院化学研究所 | A kind of epoxy foams and preparation method thereof |
| CN109957185A (en) * | 2019-03-12 | 2019-07-02 | 天津市浩迪橡塑科技有限公司 | A kind of high fire-retardance destatics type butyl rubber composite damping material and preparation method thereof |
| CN111286159A (en) * | 2020-03-25 | 2020-06-16 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of light foam core material |
Non-Patent Citations (1)
| Title |
|---|
| 蔡永源: "《高分子材料阻燃技术手册》", 28 February 1993, 化学工业出版社 * |
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