CN110305365B - Epoxy glass fiber wet winding prepreg - Google Patents

Epoxy glass fiber wet winding prepreg Download PDF

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Publication number
CN110305365B
CN110305365B CN201910530282.9A CN201910530282A CN110305365B CN 110305365 B CN110305365 B CN 110305365B CN 201910530282 A CN201910530282 A CN 201910530282A CN 110305365 B CN110305365 B CN 110305365B
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parts
epoxy
glass fiber
flame retardant
epoxy glass
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CN201910530282.9A
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CN110305365A (en
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朱汉峥
朱文远
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Sichuan Huisen Science And Technology Co ltd
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Sichuan Huisen Science And Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • 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
    • C08K3/2279—Oxides; Hydroxides of metals of antimony
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/32—Phosphorus-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/05—Alcohols; Metal alcoholates
    • C08K5/053—Polyhydroxylic alcohols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/34—Heterocyclic compounds having nitrogen in the ring
    • C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
    • C08K5/3477—Six-membered rings
    • C08K5/3492—Triazines
    • C08K5/34924—Triazines containing cyanurate groups; Tautomers thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/14—Glass
    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • 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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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Reinforced Plastic Materials (AREA)

Abstract

The invention discloses an epoxy glass fiber wet winding prepreg which comprises, by weight, 100 parts of epoxy resin, 70-83 parts of an epoxy curing agent, 12-15 parts of a toughening agent, 0.3-0.5 part of an accelerator, 3-8 parts of pentaerythritol, 8-13 parts of ammonium polyphosphate, 10-15 parts of melamine cyanurate and 18-23 parts of antimony trioxide. The epoxy glass fiber wet-process winding prepreg provided by the invention has good flame retardant property which can reach UL 94V 0 level, and can enhance the mechanical property and dielectric strength of products.

Description

Epoxy glass fiber wet winding prepreg
Technical Field
The invention relates to an epoxy glass fiber wet winding prepreg, and belongs to the technical field of epoxy glass fiber wet winding flame retardance.
Background
With the development of composite materials, the application range, the process method and the material selection of the composite materials are wider and wider. People have higher and higher demands on materials, and the environmental protection requirement is continuously improved. In the past, most of flame retardants of composite materials adopt halogen elements for flame retarding, the flame retarding effect is excellent, but a large amount of halides are generated in the flame retarding process, the pollution and the damage to the environment and human bodies are large, and residues are not easy to eliminate. So the concept of halogen-free flame retardant is proposed.
Epoxy resin is a commonly used resin material and has good physical and chemical properties. Has intentional bonding strength to the surfaces of metal and non-metal materials, and is practical and convenient. In addition, the epoxy resin has the characteristics of good dielectric property, small shrinkage rate, high hardness, good flexibility, stability to alkali and most solvents and the like, is widely applied to various fields of national defense and national economy, and has wide market prospect because the epoxy resin is widely used in the industries of composite materials in airplanes and spacecrafts, packaging materials of large-scale integrated circuits, generator insulating materials, coatings and the like. However, the limited oxygen index of common epoxy resin is low (about 19.8 parts), and the flammability and the continuous spontaneous combustion after leaving the fire easily cause fire, easily cause the risk of life and property loss, and are difficult to meet the requirement of flame retardant performance.
Epoxy resin prepreg has been widely used in the field of electronic and electrical appliances, and epoxy resin glass fiber wet winding has adopted a halogen flame-retardant gas phase mechanism in the past, and has been effective in increasing hydrogen halide reaction through the action of metal ion active components and halogen flame retardants, and releasing more effective flame retardant-metal halide. The flame retardant effect is more obvious. However, in the reaction process, a large amount of hydrogen halide gas is generated, so that the environmental pollution is serious, and the production and living environment of people are seriously influenced.
The eu countries require that all products entering the eu countries must employ halogen-free flame retardant materials to control accidental combustion. In practical use, common flame retardants, such as aluminum (aluminum hydroxide) flame retardants, phosphorus (red phosphorus, organic phosphorus salts, etc.) flame retardants have very good flame retardant effects in other systems, such as PVC, PP, PC, PS, PA, and also have very good flame retardant properties in processes such as epoxy molding, laminating, casting, etc., but have poor flame retardant properties in epoxy wet winding processes.
Disclosure of Invention
The invention aims to: aiming at the existing problems, the invention provides the epoxy glass fiber wet winding prepreg which can effectively improve the flame retardant property of an epoxy glass fiber wet winding product.
The technical scheme adopted by the invention is as follows:
the wet-process winding halogen-free epoxy glass fiber flame retardant includes polyol, ammonium polyphosphate, nitrogen-containing polycarbon compound and inorganic flame retardant.
Preferably, the polyol is pentaerythritol.
Preferably, the nitrogen-containing polycarbon compound is melamine cyanurate.
Preferably, the inorganic flame retardant is antimony trioxide.
Preferably, the cleaning agent comprises 3-8 parts of pentaerythritol, 8-13 parts of ammonium polyphosphate, 10-15 parts of melamine cyanurate and 18-23 parts of antimony trioxide by weight.
The invention also discloses an epoxy glass fiber wet-process winding prepreg which is added with the epoxy glass fiber wet-process winding halogen-free flame retardant.
Preferably, the flame retardant comprises 100 parts by weight of epoxy resin, 70-83 parts by weight of epoxy curing agent, 12-15 parts by weight of toughening agent, 0.3-0.5 part by weight of accelerator, 21-38 parts by weight of intumescent flame retardant and 18-23 parts by weight of inorganic flame retardant.
Preferably, the coating comprises 100 parts of epoxy resin, 70-83 parts of epoxy curing agent, 12-15 parts of flexibilizer, 0.3-0.5 part of accelerator, 3-8 parts of pentaerythritol, 8-13 parts of ammonium polyphosphate, 10-15 parts of melamine cyanurate and 18-23 parts of antimony trioxide.
Preferably, the epoxy curing agent is methyl tetrahydrophthalic anhydride.
Preferably, the accelerator is benzylamine.
Preferably, the toughening agent is DH 410.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that: the flame retardance can reach UL94 certification V0 level in the wet winding of the epoxy glass fiber; and can enhance the mechanical properties and dielectric strength of the product.
Detailed Description
All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive.
Any feature disclosed in this specification may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.
Example 1
The wet-process winding halogen-free epoxy glass fiber flame retardant comprises, by weight, 3 parts of pentaerythritol, 8 parts of ammonium polyphosphate, 10 parts of melamine cyanurate and 18 parts of antimony trioxide.
An epoxy glass fiber wet winding prepreg comprises, by weight, 100 parts of epoxy resin, 70 parts of an epoxy curing agent, 12 parts of a toughening agent, 0.3 part of an accelerator, 3 parts of pentaerythritol, 8 parts of ammonium polyphosphate, 10 parts of melamine cyanurate and 18 parts of antimony trioxide.
Example 2
The wet-process winding halogen-free flame retardant for epoxy glass fiber comprises 8 parts by weight of pentaerythritol, 13 parts by weight of ammonium polyphosphate, 15 parts by weight of melamine cyanurate and 23 parts by weight of antimony trioxide.
An epoxy glass fiber wet winding prepreg comprises, by weight, 100 parts of epoxy resin, 83 parts of an epoxy curing agent, 15 parts of a toughening agent, 0.5 part of an accelerator, 8 parts of pentaerythritol, 13 parts of ammonium polyphosphate, 15 parts of melamine cyanurate and 23 parts of antimony trioxide.
Example 3
The wet-process winding halogen-free flame retardant for epoxy glass fiber comprises, by weight, 5 parts of pentaerythritol, 10 parts of ammonium polyphosphate, 12 parts of melamine cyanurate and 20 parts of antimony trioxide.
An epoxy glass fiber wet winding prepreg comprises, by weight, 100 parts of epoxy resin, 76 parts of an epoxy curing agent, 13 parts of a toughening agent, 0.4 part of an accelerator, 4 parts of pentaerythritol, 10 parts of ammonium polyphosphate, 12 parts of melamine cyanurate and 20 parts of antimony trioxide.
Comparative example 1
The wet-process epoxy glass fiber winding prepreg comprises, by weight, 100 parts of epoxy resin, 76 parts of epoxy curing agent, 13 parts of toughening agent and 0.4 part of accelerator.
Comparative example 2
The wet-process epoxy glass fiber winding prepreg comprises, by weight, 100 parts of epoxy resin, 76 parts of an epoxy curing agent, 13 parts of a toughening agent, 0.4 part of an accelerator, 8 parts of pentaerythritol, 20 parts of ammonium polyphosphate and 24 parts of melamine cyanurate.
Comparative example 3
The wet-process winding prepreg of epoxy glass fiber comprises, by weight, 100 parts of epoxy resin, 76 parts of epoxy curing agent, 13 parts of toughening agent, 0.4 part of accelerator and 15 parts of antimony trioxide.
Preferably, in another embodiment, the antimony trioxide is 20 parts;
preferably, in another embodiment, the antimony trioxide is 25 parts.
Comparative example 4
The wet-process epoxy glass fiber winding prepreg comprises, by weight, 100 parts of epoxy resin, 76 parts of an epoxy curing agent, 13 parts of a toughening agent, 0.4 part of an accelerator and 15 parts of ammonium polyphosphate.
Preferably, in another embodiment, the ammonium polyphosphate is 20 parts;
preferably, in another embodiment, the ammonium polyphosphate is 25 parts.
Comparative example 5
The wet-process epoxy glass fiber winding prepreg comprises, by weight, 100 parts of epoxy resin, 76 parts of epoxy curing agent, 13 parts of toughening agent, 0.4 part of accelerator and 5 parts of melamine cyanurate.
Preferably, in another embodiment, the melamine cyanurate is 10 parts;
preferably, in another embodiment, the melamine cyanurate is 15 parts;
preferably, in another embodiment, the melamine cyanurate is 20 parts;
preferably, in another embodiment, the melamine cyanurate is 25 parts;
comparative example 6
The wet-process epoxy glass fiber winding prepreg comprises, by weight, 100 parts of epoxy resin, 76 parts of epoxy curing agent, 13 parts of toughening agent, 0.4 part of accelerator and 5 parts of pentaerythritol.
Preferably, in another embodiment, the pentaerythritol is 10 parts;
preferably, in another embodiment, the pentaerythritol is 15 parts;
preferably, in another embodiment, the pentaerythritol is 20 parts;
preferably, in another embodiment, the pentaerythritol is 25 parts.
Comparative example 7
The wet-process epoxy glass fiber winding prepreg comprises, by weight, 100 parts of epoxy resin, 76 parts of epoxy curing agent, 13 parts of toughening agent, 0.4 part of accelerator and 30 parts of aluminum hydroxide.
Preferably, in another embodiment, the aluminum hydroxide is 35 parts;
preferably, in another embodiment, the aluminum hydroxide is 40 parts;
preferably, in another embodiment, the aluminum hydroxide is 45 parts.
The epoxy glass fiber wet-process winding prepreg is used for manufacturing an epoxy wet-process winding product, and the flame retardant property is compared as follows:
example 1 Example 2 Example 3 Comparative example 1 Comparative example 2
Flame retardant grade (UL 94) V0 V0 V0 Without hierarchy V1
The following table shows the flame retardant properties of comparative examples 3-6:
5 portions of 10 portions of 15 portions of 20 portions of 25 portions of
Antimony trioxide - - V2 V2 V2
Ammonium polyphosphate - - V2 V2 V2
Trimerization of cyanuric acidCyanamide V2 V2 V2 V2 V1
Pentaerythritol V2 V2 V2 V2 V2
The following table shows the flame retardant properties of comparative example 7
Aluminum hydroxide content 30 portions of 35 portions of 40 portions of 45 portions of
Flame retardant grade (UL 94) V2 V2 V2 V2
The following table shows the properties of the wet-wound products obtained in examples 1 to 3 and comparative examples 1 to 7 (comparative examples 3 to 7 used the highest ratio):
example 1 Example 2 Example 3 Comparative example 1 Comparative example 2
Dielectric loss factor 0.006 0.0059 0.0057 0.223 0.042
Compressive strength MPa 171 168 166 89 101
Elongation at break% 58 58 57 38 43
Comparative example 3 Comparative example 4 Comparative example 5 Comparative example 6 Comparative example 7
Dielectric loss factor 0.058 0.092 0.113 0.124 0.143
Compressive strength MPa 112 123 125 132 118
Elongation at break% 45 46 46 48 42
In conclusion, in the wet winding process of the epoxy glass fiber, the flame retardant properties of pure antimony trioxide, ammonium polyphosphate, melamine cyanurate, pentaerythritol and aluminum hydroxide are poor and can only reach UL94 certification V2 level; the combined use of ammonium polyphosphate, melamine cyanurate and pentaerythritol can only reach UL94 approved V1 level, and the flame retardant property can not meet the requirement. However, when antimony trioxide, ammonium polyphosphate, melamine cyanurate and pentaerythritol are used in combination, the flame retardant property is very good and can reach UL94 certification V0 level, which shows that the antimony trioxide, the ammonium polyphosphate, the melamine cyanurate and the pentaerythritol can generate a synergistic effect in the wet winding process of the epoxy glass fiber, thereby enhancing the flame retardant property in the wet winding process of the epoxy glass fiber.
It should be noted that, when the flame retardants such as aluminum hydroxide, antimony trioxide, ammonium polyphosphate, melamine cyanurate, pentaerythritol are used in PVC, PP, PC, PS, and PA systems, the flame retardant properties are excellent and can reach UL94 certified V0 level, but in the epoxy wet winding process, the flame retardant properties are poor and cannot reach the flame retardant requirements.
Because the epoxy wet winding process is special, the flame retardance of the epoxy system in other epoxy processes such as die pressing, laminating, pouring and the like is relatively easy to achieve, but the halogen-free flame retardance of the epoxy system in the epoxy wet winding process hardly reaches the UL94 certification V0 level; for example, the flame retardant such as aluminum hydroxide, antimony trioxide, ammonium polyphosphate, melamine cyanurate, pentaerythritol and the like has flame retardant performance reaching UL94 certified V0 grade in the implementation of other epoxy processes such as die pressing, laminating, casting and the like, but has poor flame retardant performance only reaching UL94 certified V2 grade in the wet winding process of epoxy glass fiber.
In conclusion, compared with other products, the wet-process winding product prepared by winding the prepreg by the epoxy glass fiber wet process of the epoxy glass fiber wet process winding halogen-free flame retardant is obviously enhanced in compressive strength and breaking tensile rate and enhanced in dielectric strength.
In conclusion, the prepreg wound by the epoxy glass fiber wet method has good flame retardant property in the wet winding of the epoxy glass fiber, and can reach UL 94V 0 level; the mechanical properties and dielectric strength of the product can be enhanced.
The invention is not limited to the foregoing embodiments. The invention extends to any novel feature or any novel combination of features disclosed in this specification, and to any novel method or process steps or any novel group of steps disclosed.

Claims (3)

1. The utility model provides an epoxy glass fiber wet process winding prepreg which characterized in that: the flame retardant comprises, by weight, 100 parts of epoxy resin, 70-83 parts of an epoxy curing agent, 12-15 parts of a toughening agent, 0.3-0.5 part of an accelerator, 3-8 parts of pentaerythritol, 8-13 parts of ammonium polyphosphate, 10-15 parts of melamine cyanurate and 18-23 parts of antimony trioxide, achieves UL 94V 0-level flame retardance, and enhances the mechanical property and the dielectric strength of a product.
2. The epoxy glass fiber wet wound prepreg of claim 1, wherein: the epoxy curing agent is methyl tetrahydrophthalic anhydride.
3. The epoxy glass fiber wet wound prepreg of claim 1, wherein: the accelerator is benzylamine.
CN201910530282.9A 2019-06-19 2019-06-19 Epoxy glass fiber wet winding prepreg Active CN110305365B (en)

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Application Number Priority Date Filing Date Title
CN201910530282.9A CN110305365B (en) 2019-06-19 2019-06-19 Epoxy glass fiber wet winding prepreg

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CN110305365B true CN110305365B (en) 2021-03-30

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002241559A (en) * 2001-02-20 2002-08-28 Kanegafuchi Chem Ind Co Ltd Styrenic resin composition, foamed material and method for producing the same
CN101293984B (en) * 2007-04-28 2010-10-27 中国石油化工股份有限公司 Expanded carbon flame-proof polypropelene composition and preparation method thereof
CN101293983B (en) * 2007-04-28 2011-01-26 中国石油化工股份有限公司 Expansion flame-proof polypropelene composition and preparation method thereof
CN102719022B (en) * 2012-07-06 2015-06-03 上海日之升新技术发展有限公司 Anti-aging halogen-free flame retardant polypropylene composite material and preparation method thereof
CN103044762A (en) * 2012-12-06 2013-04-17 上海日之升新技术发展有限公司 Mineral reinforced halogen-free flame-retardant polypropylene composite material and preparation method thereof
CN104327511A (en) * 2014-10-30 2015-02-04 济南泰星精细化工有限公司 Low-smoke halogen-free flame retardant composition for silicone rubber and application thereof
CN107383613A (en) * 2017-08-22 2017-11-24 南宁学院 A kind of flame-retardant polypropylene composite material and preparation method

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