CN117417620A - Pultrusion resin composite material and preparation method and application thereof - Google Patents

Pultrusion resin composite material and preparation method and application thereof Download PDF

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Publication number
CN117417620A
CN117417620A CN202311369466.4A CN202311369466A CN117417620A CN 117417620 A CN117417620 A CN 117417620A CN 202311369466 A CN202311369466 A CN 202311369466A CN 117417620 A CN117417620 A CN 117417620A
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China
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component
anhydride
resin composite
parts
epoxy
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CN202311369466.4A
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Chinese (zh)
Inventor
徐晓虎
龚雨
俞孝伟
杨颖�
杨程
鉏瑞杰
季华
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Jiangsu Yangnong Kumho Chemical Co ltd
Jiangsu Yangnong Chemical Group Co Ltd
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Jiangsu Yangnong Kumho Chemical Co ltd
Jiangsu Yangnong Chemical Group Co Ltd
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Priority to CN202311369466.4A priority Critical patent/CN117417620A/en
Publication of CN117417620A publication Critical patent/CN117417620A/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • 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
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
    • C08J5/042—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with carbon fibres
    • 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
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • 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
    • C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
    • 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
    • C08K7/06—Elements

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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)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Moulding By Coating Moulds (AREA)
  • Epoxy Resins (AREA)

Abstract

The invention belongs to the technical field of epoxy resin production, and particularly relates to a pultrusion resin composite material, a preparation method and application thereof. The invention provides a pultrusion resin composite material which is a double-component resin and comprises a component A and a component B; the component A comprises 70-98 parts of epoxy resin, 3-5 parts of diluent and 5-7 parts of toughening agent by mass; the component B comprises 98-99.2 parts of anhydride curing agent and 0.8-2 parts of accelerator by mass. The acid anhydride curing agent can reduce the viscosity of the system, and is convenient for infiltrating the carbon fiber pultrusion material to lower the pultrusion resistivity; the acid anhydride curing agent and the epoxy resin are used as raw materials, so that the pultrusion resin composite material has good tensile strength, tensile modulus, bending strength and bending modulus, the problem of poor strength of the molded profile is effectively solved, and the material is simple and the cost is low.

Description

Pultrusion resin composite material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of epoxy resin production, and particularly relates to a pultrusion resin composite material, a preparation method and application thereof.
Background
The carbon fiber reinforced thermosetting epoxy resin matrix composite is a typical lightweight material, has the characteristics of high specific strength and specific rigidity, high damping, corrosion resistance and the like, can realize design and manufacturing integration, has low cost of the whole life cycle, improves the structural efficiency, and is widely applied to the manufacturing fields of aviation, aerospace, wind power, rail transit and automobiles requiring lightweight. The advanced pultrusion is a low-cost automatic manufacturing technology of composite materials, which takes carbon fiber or glass fiber coarse sand, fabrics, resin and auxiliary materials thereof as raw materials, and prepares composite material profiles with specific cross-section shapes through the steps of preforming, gum dipping or gum injection, extrusion-heating curing, traction and cutting; the process has the advantages of high production efficiency, high straightness of products, low porosity of finished products, easiness in secondary cementing and the like. However, the existing matrix resin has good performance, but is brittle after being cured under the condition of no modification, and cannot meet the requirements of the pultrusion process on the viscosity and strength of the matrix resin.
Disclosure of Invention
In view of the above, the invention aims to provide a pultrusion resin composite material, a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a pultrusion resin composite material which is a double-component resin and comprises a component A and a component B;
the component A comprises 70-98 parts of epoxy resin, 3-5 parts of diluent and 5-7 parts of toughening agent by mass;
the component B comprises 98-99.2 parts of anhydride curing agent and 0.8-2 parts of accelerator by mass.
Preferably, the mass ratio of the component A to the component B is 100 (80-120).
Preferably, the epoxy resin is epoxy resin E54 or epoxy resin E51.
Preferably, the diluent comprises one or more of a monofunctional epoxy diluent, a difunctional epoxy diluent and a multifunctional epoxy diluent.
Preferably, the anhydride curing agent comprises one or more of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride, methyl nadic anhydride, tetrahydrophthalic anhydride, hexahydrophthalic anhydride, phthalic anhydride, tung oil anhydride, succinic anhydride, dodecenyl succinic anhydride, glutaric anhydride, polyazelaic anhydride, cis-butadiene anhydride and di-maleic anhydride methyl ethylbenzene.
Preferably, the toughening agent is a polyol.
Preferably, the accelerator is an imidazole accelerator.
Preferably, the polyol comprises one or more of polyether polyol PPG800, polyether polyol PPG-1000, polyether polyol 2000 and polyester polyol.
The invention also provides a preparation method of the pultrusion resin composite material, which comprises the following steps:
firstly mixing epoxy resin, a diluent and a toughening agent to obtain a component A;
secondly mixing an anhydride curing agent and an accelerator to obtain a component B;
and thirdly mixing the component A and the component B to obtain the pultruded resin composite material.
The invention also provides the application of the pultrusion resin composite material according to the technical scheme or the pultrusion resin composite material prepared by the preparation method according to the technical scheme in the carbon fiber composite material.
The invention provides a pultrusion resin composite material which is a double-component resin and comprises a component A and a component B; the component A comprises 70-98 parts of epoxy resin, 3-5 parts of diluent and 5-7 parts of toughening agent by mass; the component B comprises 98-99.2 parts of anhydride curing agent and 0.8-2 parts of accelerator by mass.
The acid anhydride curing agent can reduce the viscosity of the system, and is convenient for infiltrating the carbon fiber pultrusion material to lower the pultrusion resistivity; the acid anhydride curing agent and the epoxy resin are used as raw materials, the acid anhydride curing agent is epoxy group, and after ring opening, etherification reaction is carried out on hydroxyl formed by acid anhydride, so that the formed cross-linking density is high, the compactness is stronger, and the pultrusion resin composite material has good tensile strength, tensile modulus, bending strength and bending modulus, so that the problem of poor strength of the formed profile is effectively solved, and the material is simple and the cost is low.
Detailed Description
The invention provides a pultrusion resin composite material which is a double-component resin and comprises a component A and a component B;
the component A comprises 70-98 parts of epoxy resin, 3-5 parts of diluent and 5-7 parts of toughening agent by mass;
the component B comprises 98-99.2 parts of anhydride curing agent and 0.8-2 parts of accelerator by mass.
The present invention is not limited to the specific source of the raw materials, and may be commercially available products known to those skilled in the art, unless otherwise specified.
The pultruded resin composite provided by the invention comprises an A component.
In the present invention, the a component includes 70 to 98 parts, preferably 80 to 95 parts, more preferably 90 parts of an epoxy resin. In the present invention, the epoxy resin is preferably an epoxy resin E54 or an epoxy resin E51, more preferably an epoxy resin E51.
The epoxy resin is a long-chain polymer, which wets the carbon fiber, can endow the composite material with better performance ratio based on the characteristics, and can ensure that the carbon fiber is better bonded when being pressed into a plate, and has better interlaminar shearing performance and pultrusion manufacturability.
The A component comprises 3 to 5 parts by weight of a diluent, preferably 3.5 to 4.5 parts by weight of the epoxy resin. In the present invention, the diluent preferably includes one or more of a monofunctional epoxy diluent, a difunctional epoxy diluent, and a multifunctional epoxy diluent, more preferably a monofunctional epoxy diluent or a difunctional epoxy diluent, and most preferably a 622 diluent and/or an AGE diluent; the monofunctional epoxy diluent preferably comprises one or more of decyl glycidyl ether, C8-C10 glycidyl ether and C12-C14 glycidyl ether, more preferably C12-C14 glycidyl ether; the difunctional epoxy diluent preferably comprises one or more of polyethylene glycol diglycidyl ether, 1, 4-butanediol diglycidyl ether and ethylene glycol diglycidyl ether, more preferably 1, 4-butanediol diglycidyl ether; the multifunctional epoxy diluent preferably comprises one or more of trimethylolpropane triglycidyl ether, glycerol triglycidyl ether, pentaerythritol triglycidyl ether, MF-3101 type trifunctional high-temperature-resistant epoxy resin and MF-4101 type tetrafunctional glycidylamine high-temperature-resistant epoxy resin, and more preferably MF-3101 type trifunctional high-temperature-resistant epoxy resin or MF-4101 type tetrafunctional glycidylamine high-temperature-resistant epoxy resin. When the number of the diluents is several, the invention has no special limitation on the proportions of the diluents of different types, and the diluents can be mixed at random.
Because of the higher viscosity of epoxy resins, diluents are needed to reduce the viscosity, while introducing different groups can increase toughness and elasticity. The molecular structures of the two diluents of the MF-3101 type trifunctional high-temperature-resistant epoxy resin and the MF-4101 type tetrafunctional glycidic amine high-temperature-resistant epoxy resin contain a plurality of epoxy groups and aromatic rings, and can form higher crosslinking density and aromatic density in the curing process, so that the cured product has the characteristics of good heat resistance, high mechanical strength, low curing shrinkage, radiation resistance, water resistance and the like.
The A component comprises 5 to 7 parts by weight of a toughening agent, preferably 5.5 to 6.5 parts by weight of the epoxy resin. In the present invention, the toughening agent is preferably a polyol; the polyol preferably comprises one or more of polyether polyol PPG800, polyether polyol PPG-1000, polyether polyol 2000 and polyester polyol, more preferably polyether polyol PPG800 or polyether polyol PPG-1000.
The polyether long-chain substance with the active end group of the toughening agent can participate in the curing reaction to ensure that the polyether long-chain structure is uniformly dispersed in the system, thereby achieving the toughening effect.
The pultruded resin composite provided by the invention comprises a component B.
The component B comprises 98 to 99.2 parts by mass, preferably 98.5 to 99 parts by mass, more preferably 98.8 parts by mass of an acid anhydride-based curing agent, based on 1 part by mass of the epoxy resin. In the present invention, the acid anhydride-based curing agent preferably includes one or more of methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, methylnadic anhydride, tetrahydrophthalic anhydride, hexahydrophthalic anhydride, phthalic anhydride, tung oil anhydride, succinic anhydride, dodecenyl succinic anhydride, glutaric anhydride, polyazelaic anhydride, cis-butadiene anhydride, and di-maleic anhydride-based methyl ethylbenzene, more preferably methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, methylnadic anhydride, tetrahydrophthalic anhydride, hexahydrophthalic anhydride, or phthalic anhydride. When the acid anhydride curing agents are the above-mentioned several kinds, the invention has no special limitation on the mixture ratio of the different kinds of acid anhydride curing agents, and the mixture ratio is arbitrary.
The invention uses the acid anhydride curing agent to reduce the viscosity of the system, and is convenient for infiltrating the carbon fiber pultrusion material to lower the pultrusion resistivity.
The component B comprises 0.8 to 2 parts by mass, preferably 1 to 1.5 parts by mass, more preferably 1.2 parts by mass of an accelerator, based on 1 part by mass of the epoxy resin. In the present invention, the accelerator is preferably an imidazole-based accelerator; the imidazole accelerator preferably comprises one or more of 1-methylimidazole, 2-methylimidazole and diethyl tetramethylimidazole, and more preferably 1-methylimidazole or 2-methylimidazole. The invention utilizes imidazole accelerator to reduce the curing reaction temperature and promote the curing of resin.
In the invention, the mass ratio of the component A to the component B is preferably 100 (80-120), more preferably 100:80.
The invention adopts anhydride curing agent and epoxy resin as raw materials, so that the pultrusion resin composite material has good tensile strength, tensile modulus, bending strength and bending modulus, effectively solves the problem of poor strength of the molded section bar, and has simple material and low cost.
In the invention, the invention also provides a preparation method of the pultrusion resin composite material, which comprises the following steps:
firstly mixing epoxy resin, a diluent and a toughening agent to obtain a component A;
secondly mixing an anhydride curing agent and an accelerator to obtain a component B;
and thirdly mixing the component A and the component B to obtain the pultruded resin composite material.
The invention mixes the epoxy resin, the thinner and the flexibilizer for the first time to obtain the component A. In the present invention, the first mixing is preferably performed at room temperature; the first mixing is preferably carried out under stirring; the stirring speed is 100-200 rpm, more preferably 120-180 rpm; the stirring time is preferably 15 to 45 minutes, more preferably 20 to 40 minutes.
In the present invention, the first mixing is preferably to add a diluent and a toughening agent to the epoxy resin.
The invention mixes anhydride curing agent and accelerator for the second time to obtain component B. In the present invention, the second mixing is preferably performed at room temperature; the second mixing is preferably carried out under stirring; the stirring speed is 100-200 rpm, more preferably 120-180 rpm; the stirring time is preferably 15 to 30 minutes, more preferably 20 to 25 minutes.
After the A component and the B component are obtained, the A component and the B component are mixed in a third way to obtain the pultruded resin composite material.
In the present invention, the third mixing is preferably performed at room temperature; the third mixing is preferably carried out under stirring; the stirring speed is 100-200 rpm, more preferably 120-180 rpm; the stirring time is preferably 15 to 45 minutes, more preferably 20 to 40 minutes.
The invention also provides the application of the pultrusion resin composite material according to the technical scheme or the pultrusion resin composite material prepared by the preparation method according to the technical scheme in the carbon fiber composite material.
The application of the pultrusion resin composite material in the carbon fiber composite material is not particularly limited, and the application mode well known in the art can be adopted.
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, but they should not be construed as limiting the scope of the present invention.
Examples and comparative examples
The raw materials used in examples and comparative examples are shown in Table 1.
Table 1 raw materials used in examples and comparative examples
The preparation method comprises the following steps: weighing epoxy resin according to the mass portion ratio at room temperature, then weighing diluent and flexibilizer with corresponding mass, adding the diluent and the flexibilizer into the epoxy resin, and stirring the mixture at 180rpm for 30min to obtain a component A;
weighing and mixing the acidoside curing agent and the accelerator in parts by weight at room temperature, and stirring for 20min at 180rpm to obtain a component B;
and mixing the component A and the component B according to a mass ratio of 100:80, and stirring at 180rpm for 20min at room temperature to obtain a pultruded resin composite.
Performance testing
(1) The viscosity of the A-component of each of the examples and comparative examples was measured at 25℃and the results are shown in Table 2.
TABLE 2 viscosity at 25℃of A component in examples and comparative examples
Project Example 1 Example 2 Example 3 Comparative example 1
Viscosity (cp. S) 3666 3207 5300 5523
(2) The 120℃gel time of the pultruded resin composites of each of the examples and comparative examples was measured and the results are shown in Table 3.
TABLE 3 120℃gel time for pultruded resin composites of examples and comparative examples
Gel time at 120 DEG C 1# 2# 3#
Example 1 413.5s 416.0s 414.3s
Example 2 417.2s 418.5s 417.8s
Example 3 412.0s 404.2s 408.5s
Comparative example 1 402.1s 403.5s 402.6s
(3) The properties of the pultruded resin composites of each example and comparative example were tested and the results are shown in Table 4.
Table 4 properties of the pultruded resin composites of the examples and comparative examples
As is clear from tables 2, 3 and 4, the tensile strength, tensile modulus, flexural strength and flexural modulus of example 3 were all more excellent. And the gel time is similar to that of the comparative example in an error range, the viscosity is lower than that of the comparative example 1, the carbon fiber can be better infiltrated, the pultrusion resistivity is lower, and the pultrusion efficiency can be improved. Therefore, the epoxy resin E51 is selected as the main material in the scheme, the use of the diluent is reduced, the viscosity reaches the standard, the price is lower, and the performance is better.
Although the foregoing embodiments have been described in some, but not all, embodiments of the invention, according to which one can obtain other embodiments without inventiveness, these embodiments are all within the scope of the invention.

Claims (10)

1. The pultrusion resin composite material is a two-component resin and is characterized by comprising a component A and a component B;
the component A comprises 70-98 parts of epoxy resin, 3-5 parts of diluent and 5-7 parts of toughening agent by mass;
the component B comprises 98-99.2 parts of anhydride curing agent and 0.8-2 parts of accelerator by mass.
2. The pultruded resin composite according to claim 1, wherein the mass ratio of the A component and the B component is 100 (80-120).
3. The pultruded resin composite of claim 1, wherein the epoxy is epoxy E54 or epoxy E51.
4. The pultruded resin composite of claim 1, wherein the diluent comprises one or more of a monofunctional epoxy diluent, a difunctional epoxy diluent, and a multifunctional epoxy diluent.
5. The pultruded resin composite of claim 1, wherein the anhydride curing agent comprises one or more of methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, methylnadic anhydride, tetrahydrophthalic anhydride, hexahydrophthalic anhydride, phthalic anhydride, tung oil anhydride, succinic anhydride, dodecenyl succinic anhydride, glutaric anhydride, polyazelaic anhydride, cis-butadiene anhydride, and di-maleic anhydride methyl ethylbenzene.
6. The pultruded resin composite according to claim 1, wherein the toughening agent is a polyol.
7. The pultruded resin composite according to claim 1, wherein the accelerator is an imidazole-based accelerator.
8. The pultruded resin composite of claim 6, wherein the polyol comprises one or more of polyether polyol PPG800, polyether polyol PPG-1000, polyether polyol 2000 and polyester polyol.
9. The method for producing a pultruded resin composite according to any of claims 1 to 8, characterized by comprising the steps of:
firstly mixing epoxy resin, a diluent and a toughening agent to obtain a component A;
secondly mixing an anhydride curing agent and an accelerator to obtain a component B;
and thirdly mixing the component A and the component B to obtain the pultruded resin composite material.
10. Use of a pultruded resin composite according to any of claims 1-8 or a pultruded resin composite prepared according to the method of preparation of claim 9 in a carbon fibre composite.
CN202311369466.4A 2023-10-23 2023-10-23 Pultrusion resin composite material and preparation method and application thereof Pending CN117417620A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202311369466.4A CN117417620A (en) 2023-10-23 2023-10-23 Pultrusion resin composite material and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202311369466.4A CN117417620A (en) 2023-10-23 2023-10-23 Pultrusion resin composite material and preparation method and application thereof

Publications (1)

Publication Number Publication Date
CN117417620A true CN117417620A (en) 2024-01-19

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