CN116715877A - Fiber reinforced composite material and preparation method and application thereof - Google Patents

Fiber reinforced composite material and preparation method and application thereof Download PDF

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Publication number
CN116715877A
CN116715877A CN202310616461.0A CN202310616461A CN116715877A CN 116715877 A CN116715877 A CN 116715877A CN 202310616461 A CN202310616461 A CN 202310616461A CN 116715877 A CN116715877 A CN 116715877A
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Prior art keywords
curing agent
reinforced composite
fiber reinforced
spraying
weight
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CN202310616461.0A
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Chinese (zh)
Inventor
张萍
聂长海
姜鹏程
蔡亦文
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Outmet Transportation Technology Co Ltd
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Outmet Transportation Technology Co Ltd
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Priority to CN202310616461.0A priority Critical patent/CN116715877A/en
Publication of CN116715877A publication Critical patent/CN116715877A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/28—Shaping operations therefor
    • B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/28—Shaping operations therefor
    • B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
    • 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
    • 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
    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/06—Unsaturated polyesters
    • 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
    • C08J2481/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
    • C08J2481/06—Polysulfones; Polyethersulfones
    • 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
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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

Abstract

The invention discloses a fiber reinforced composite material, a preparation method and application thereof. The invention comprises a surface layer and a reinforcing layer, wherein the surface layer comprises a gel coat and a curing agent A, and the gel coat comprises the following components: 8-10% of styrene, 35-45% of dihydric alcohol, 35-45% of dibasic acid, 1-2% of auxiliary agent and 8-10% of pigment and filler; the enhancement layer comprises the following components: 100% of unsaturated polyester resin, 10-35% of composite flame retardant, 0.3-0.5% of defoamer, 0.6-1.2% of accelerator, 1-2% of curing agent B, 20-35% of jet yarn and 10-15% of check fabric. The fiber reinforced composite material is prepared by an injection molding process and is used for manufacturing interior parts of vehicles. The components in the invention are scientifically selected, reasonably matched, synergistically promoted, and interacted with the surface layer and the reinforcing layer, so that the comprehensive performance of the fiber reinforced composite material is greatly improved, and the requirements of special industries such as vehicles and the like are met.

Description

Fiber reinforced composite material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a fiber reinforced composite material, and a preparation method and application thereof.
Background
The interior components of vehicles in the transportation industry are generally made of fiber reinforced composite materials, and currently, the fiber reinforced composite materials are increasingly used in vehicles in the transportation industry due to their excellent properties. The main forming method of the fiber reinforced composite material comprises hand lay-up forming, vacuum diversion forming, compression molding, injection forming and the like. The manual paste forming has the advantages of high dependence on the skills of operators, low production efficiency, poor reproducibility of products, difficulty in ensuring consistency of quality and high requirements of the production process on occupational health and environmental protection. The auxiliary materials needed by the vacuum diversion molding are more, the production cost is higher, and the auxiliary materials are disposable, so that great waste is caused. The automatic production degree of compression molding is very high, the equipment investment is very large, the cost of the steel mould required for production is relatively high, and the method is not suitable for the production of products with small quantity. The spray forming can reduce the dependence on manpower, has certain mechanization degree, high labor efficiency, small equipment investment, no auxiliary material loss and no need of expensive dies; however, the existing injection molding process cannot meet the requirements of special industries such as vehicles due to the fact that the formula design of raw materials is unreasonable and the selection of injection molding parameters is improper.
Disclosure of Invention
The invention aims to provide a fiber reinforced composite material, a preparation method and application thereof, and aims to solve the problems that the fiber reinforced composite material produced by adopting a spray molding process in the prior art cannot meet the requirements of special industries such as vehicles and the like due to unreasonable formula design of raw materials and improper selection of spray molding parameters.
In order to solve the technical problems, the invention is mainly realized by the following technical scheme:
in one aspect, the invention provides a fiber reinforced composite comprising a surface layer and a reinforcing layer, the surface layer and the reinforcing layer having a thickness ratio of 1:8-12; the surface layer comprises a gel coat and a curing agent A, wherein the adding amount of the curing agent A in the gel coat is 1-2%, and the gel coat comprises the following components in percentage by weight: 8-10% of styrene, 35-45% of dihydric alcohol, 35-45% of dibasic acid, 1-2% of auxiliary agent and 8-10% of pigment and filler; the reinforcing layer comprises the following components in percentage by weight: 100% of unsaturated polyester resin, 10-35% of composite flame retardant, 0.3-0.5% of defoamer, 0.6-1.2% of accelerator, 1-2% of curing agent B, 20-35% of jet yarn and 10-15% of check fabric; the composite flame retardant consists of aluminum hypophosphite and nano boehmite according to the weight ratio of 20-40:1-3, or consists of aluminum hypophosphite, nano boehmite and diphenyl sulfone polyphenyl phosphonate according to the weight ratio of 20-40:1-3:10-30.
The fiber reinforced composite material forms a surface layer by using the gel coat and the curing agent A, forms a reinforcing layer by using the unsaturated polyester resin, the composite flame retardant, the defoaming agent, the accelerator, the curing agent B, the jet yarn and the square cloth, has scientific component selection, reasonable matching and synergistic promotion, and the surface layer and the reinforcing layer interact, so that the obtained fiber reinforced composite material has the advantages of high Babbitt hardness, small water absorption, high bending strength and tensile strength, proper resin content, greatly improved comprehensive performance of the fiber reinforced composite material, particularly the use of the composite flame retardant, greatly improved fireproof performance of the fiber reinforced composite material, and meets the requirements of special industries such as interior parts of vehicles.
As a preferred embodiment, the unsaturated polyester resin comprises the following components in weight percent: 15-20% of styrene, 30-40% of dihydric alcohol, 30-40% of dibasic acid, 1-2% of auxiliary agent and 6-8% of pigment and filler. The unsaturated polyester resin is prepared by polycondensation of dihydric alcohol and dibasic acid, and the polycondensation is conventional; the polycondensation reaction product is diluted by styrene, and the auxiliary agent and pigment filler are added, so that the structure of the unsaturated polyester resin is enriched, and the comprehensive performance of the unsaturated polyester resin is improved. Typically, the auxiliary agent is an anti-settling agent, an accelerator or the like, preferably the accelerator is 0.6 to 1.2% by weight.
As a preferred embodiment, the defoamer is BYK-A515 defoamer. The invention adopts BYK-A515 defoamer to perform defoaming treatment on the mixture formed by unsaturated polyester resin, composite flame retardant and accelerator, and the defoamer has strong defoaming capability and good use effect.
As a preferred embodiment, the promoter is cobalt iso-octoate. According to the invention, cobalt iso-octoate is used as an accelerator, has a catalytic effect, is matched with the curing agent B, can promote the curing of unsaturated polyester resin, and has a good use effect.
As a preferred embodiment, both the curing agent a and the curing agent B are methyl ethyl ketone peroxide. The gel coat is cured by the methyl ethyl ketone peroxide curing agent, and the unsaturated polyester resin is also cured by the methyl ethyl ketone peroxide curing agent, so that the curing agent has good performance and is convenient to use.
As a preferred embodiment, the tarpaulin has a density of 400-800g/m 2 . The reinforcing layer is also provided with the check cloth, and the check cloth is arranged in the middle of the reinforcing layer, so that the structure of the reinforcing layer is further enriched, the hardness and the strength of the reinforcing layer are stabilized, and the comprehensive performance of the fiber reinforced composite material is improved.
In another aspect, the invention provides a method of making a fiber reinforced composite comprising the steps of: 1) Taking gel coats and a curing agent A, uniformly mixing, spraying the mixture onto a mold, and curing the mixture until the mixture is cured to a state of sticking hands and not dirtying hands to obtain a surface layer; 2) Taking unsaturated polyester resin, a composite flame retardant, a defoaming agent and an accelerator, uniformly mixing to obtain a polyester mixture, taking a curing agent B, firstly spraying the polyester mixture and the curing agent B onto a surface layer for 40-60s, uniformly coating, then spraying the polyester mixture, the curing agent B and sprayed yarns onto the polyester mixture layer at the same time, compacting by a press roller, paving square cloth, flattening by the press roller again, and finally continuously spraying the polyester mixture, the curing agent B and the sprayed yarns, compacting by the press roller, curing and demolding to obtain the fiber reinforced composite material.
In the preparation method of the fiber reinforced composite material, firstly, spraying a layer of thin polyester mixture on a surface layer by using spraying equipment, thereby improving the adhesive force of sprayed yarns; then, the polyester mixture and the jet yarn are simultaneously sprayed on the polyester mixture layer, the R angle can be sprayed firstly according to the shape of an actual product, and then other flat positions are sprayed, so that the spraying thickness is uniform all the positions; then, the loose sprayed yarn and polyester mixture layer are rolled and compacted back and forth by using a compression roller, and the corners are flattened by adopting a hairbrush, so that no bubbles are generated; paving check cloth and compacting; finally, spraying the polyester mixture and spraying yarn continuously, and compacting. After the spraying is finished, adopting a detection tool to measure whether the thickness meets the requirement, and adjusting the height from the tip of the detection tool to a measurement plane to meet the requirement of the thickness of the product; if the product has no indentation, the product has insufficient thickness, and a part of the mixture of the sprayed yarn and the polyester is required to be sprayed; after the detection tool is pulled out, the sprayed yarns on the surface of the product can possibly be raised by external force, and the product is flattened by adopting a pressing roller. The preparation method of the fiber reinforced composite material strictly controls each process step, so that each component fully interacts, and the preparation method is convenient to operate and high in production efficiency.
As a preferred embodiment, in the step 2), before laying the square cloth, the spray gun for spraying the polyester mixture and the curing agent B and spraying the yarn walks at a constant speed for two times; after laying the square cloth, the spray gun spraying the polyester mixture and the curing agent B and spraying the yarn again walks back and forth at a constant speed. According to the invention, the check cloth is paved in the middle of the reinforcing layer, and the spraying amount of the polyester mixture and the spraying yarn is controlled through the travelling stroke of the spray gun, so that the control method is convenient to control and easy to operate for workers.
As a preferred embodiment, in said step 2), the polyester mixture and hardener B outlet of the spray gun is at an angle of 45 degrees to the spray yarn outlet. The spray yarn sprayed at the angle is fully wetted by the polyester mixture sprayed at the same time, and the spray yarn and the polyester mixture are uniformly mixed, so that the uniformity of a reinforcing layer in the fiber reinforced composite material is improved, and the comprehensive performance of the fiber reinforced composite material is improved.
In yet another aspect, the invention is a use of a fiber-reinforced composite for making an interior component of a vehicle. The fiber reinforced composite material has the advantages of good comprehensive performance, large Babbitt hardness, small water absorption, high bending strength and tensile strength, proper resin content and excellent fireproof performance, is particularly suitable for manufacturing interior parts of vehicles, and meets the requirements of special industries such as vehicles and the like.
Compared with the prior art, the invention has the beneficial effects that: the fiber reinforced composite material forms a surface layer by using the gel coat and the curing agent A, forms a reinforcing layer by using the unsaturated polyester resin, the composite flame retardant, the defoaming agent, the accelerator, the curing agent B, the jet yarn and the square cloth, has scientific component selection, reasonable matching and synergistic promotion, and the surface layer and the reinforcing layer interact, so that the obtained fiber reinforced composite material has the advantages of high Babbitt hardness, small water absorption, high bending strength and tensile strength, proper resin content, greatly improved comprehensive performance of the fiber reinforced composite material, particularly the use of the composite flame retardant, greatly improved fireproof performance of the fiber reinforced composite material, and meets the requirements of special industries such as interior parts of vehicles.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with specific embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The fiber reinforced composite material comprises a surface layer and a reinforcing layer, wherein the thickness ratio of the surface layer to the reinforcing layer is 1:8-12; the surface layer comprises a gel coat and a curing agent A, wherein the adding amount of the curing agent A in the gel coat is 1-2%, and the gel coat comprises the following components in percentage by weight: 8-10% of styrene, 35-45% of dihydric alcohol, 35-45% of dibasic acid, 1-2% of auxiliary agent and 8-10% of pigment and filler; the reinforcing layer comprises the following components in percentage by weight: 100% of unsaturated polyester resin, 10-35% of composite flame retardant, 0.3-0.5% of defoamer, 0.6-1.2% of accelerator, 1-2% of curing agent B, 20-35% of jet yarn and 10-15% of check fabric; the composite flame retardant consists of aluminum hypophosphite and nano boehmite according to the weight ratio of 20-40:1-3, or consists of aluminum hypophosphite, nano boehmite and diphenyl sulfone polyphenyl phosphonate according to the weight ratio of 20-40:1-3:10-30.
Preferably, the unsaturated polyester resin comprises the following components in percentage by weight: 15-20% of styrene, 30-40% of dihydric alcohol, 30-40% of dibasic acid, 1-2% of auxiliary agent and 6-8% of pigment and filler.
Preferably, the defoamer is a BYK-A515 defoamer.
Preferably, the promoter is cobalt iso-octoate.
Preferably, the curing agent a and the curing agent B are both methyl ethyl ketone peroxide.
Preferably, the density of the square cloth is 400-800g/m 2 。
The invention relates to a preparation method of a fiber reinforced composite material, which comprises the following steps:
1) Taking gel coats and a curing agent A, uniformly mixing, spraying the mixture onto a mold, and curing the mixture until the mixture is cured to a state of sticking hands and not dirtying hands to obtain a surface layer;
2) Taking unsaturated polyester resin, a composite flame retardant, a defoaming agent and an accelerator, uniformly mixing to obtain a polyester mixture, taking a curing agent B, firstly spraying the polyester mixture and the curing agent B onto a surface layer for 40-60s, uniformly coating to obtain a polyester mixture layer, then simultaneously spraying the polyester mixture, the curing agent B and sprayed yarns onto the polyester mixture layer, compacting by a compression roller, paving check cloth, flattening by the compression roller again, and finally continuously spraying the polyester mixture, the curing agent B and the sprayed yarns, compacting by the compression roller, curing and demolding to obtain the fiber reinforced composite material.
Preferably, in the step 2), before laying the square cloth, a spray gun for spraying the polyester mixture, the curing agent B and the sprayed yarn walks at a constant speed for two times; after laying the square cloth, the spray gun spraying the polyester mixture and the curing agent B and spraying the yarn again walks back and forth at a constant speed.
Preferably, in said step 2), the polyester mixture and hardener B outlet of the spray gun is at an angle of 45 degrees to the spray yarn outlet.
The use of a fiber-reinforced composite material according to the invention for producing interior components of vehicles.
Example 1
The invention relates to a preparation method of a fiber reinforced composite material, which comprises the following steps:
1) Taking 10 parts by weight of gel coat, wherein the gel coat is an unsaturated polyester mixture prepared from 1.0 part by weight of styrene, 4.5 parts by weight of dihydric alcohol, 3.5 parts by weight of dibasic acid, 0.08 part by weight of anti-settling agent, 0.12 part by weight of accelerator and 0.8 part by weight of pigment and filler;
2) Taking 0.1 part by weight of curing agent A, namely methyl ethyl ketone peroxide, uniformly mixing the curing agent A and gel coat, pouring the mixture into a spray can, uniformly spraying the mixture formed by the gel coat and the curing agent A onto a mold by adopting a spray gun, curing, and obtaining a surface layer when the mixture is cured to a state of sticking hands but not dirtying hands;
3) Taking 100 parts by weight of unsaturated polyester resin, 35 parts by weight of composite flame retardant, 0.3 part by weight of BYK-A515 defoamer, 1.2 parts by weight of accelerator cobalt isooctanoate, 2 parts by weight of curing agent B methyl ethyl ketone peroxide, 35 parts by weight of jet yarn and 15 parts by weight of check cloth;
the unsaturated polyester resin is prepared from 20 parts by weight of styrene, 30 parts by weight of dihydric alcohol, 40 parts by weight of dibasic acid, 2 parts by weight of anti-settling agent and 8 parts by weight of pigment and filler;
the composite flame retardant consists of 34.1 parts by weight of aluminum hypophosphite and 0.9 parts by weight of nano boehmite;
the density of the square cloth is 400g/m 2 ；
4) Taking unsaturated polyester resin, a composite flame retardant, a BYK-A515 defoamer and an accelerator cobalt iso-octoate, and uniformly mixing to obtain a polyester mixture;
5) And (3) taking a curing agent B, namely methyl ethyl ketone peroxide, firstly spraying a polyester mixture and the curing agent B onto a surface layer, wherein the spraying pressure is 0.25MPa, the spraying time is 40s, uniformly coating the polyester mixture and the curing agent B by adopting a hairbrush to obtain a polyester mixture layer, then simultaneously spraying the polyester mixture, the curing agent B and spraying yarns onto the polyester mixture layer, wherein the spraying pressure is 0.25MPa, a spraying gun spraying the polyester mixture, the curing agent B and the spraying yarns walks at a constant speed for two times, the outlet of the polyester mixture and the curing agent B of the spraying gun forms a 45-degree angle with the outlet of the spraying yarns, compacting by adopting a pressing roller, paving square cloth, flattening by adopting the pressing roller again, and finally continuously spraying the polyester mixture, the curing agent B and the spraying yarns according to the process, compacting by the pressing roller, curing and demolding to obtain the fiber reinforced composite material.
In the fiber-reinforced composite material obtained in this example, the thickness of the surface layer was 0.35mm, and the thickness of the reinforcing layer was 2.8mm.
Example two
The invention relates to a preparation method of a fiber reinforced composite material, which comprises the following steps:
1) Taking 10 parts by weight of gel coat, wherein the gel coat is an unsaturated polyester mixture prepared from 0.8 part by weight of styrene, 3.5 parts by weight of dihydric alcohol, 4.5 parts by weight of dibasic acid, 0.12 part by weight of anti-settling agent, 0.08 part by weight of accelerator and 1.0 part by weight of pigment and filler;
2) Taking 0.2 part by weight of curing agent A, namely methyl ethyl ketone peroxide, uniformly mixing the curing agent A and gel coat, pouring the mixture into a spray can, uniformly spraying the mixture formed by the gel coat and the curing agent A onto a mold by adopting a spray gun, curing, and obtaining a surface layer when the mixture is cured to a state of sticking hands but not dirtying hands;
3) 120 parts of unsaturated polyester resin, 12 parts of composite flame retardant, 0.6 part of BYK-A515 defoamer, 0.72 part of accelerator cobalt iso-octoate, 1.2 parts of curing agent B methyl ethyl ketone peroxide, 24 parts of jet yarn and 12 parts of check cloth are taken;
the unsaturated polyester resin is prepared from 18 parts by weight of styrene, 48 parts by weight of dihydric alcohol, 45.6 parts by weight of dibasic acid, 1.2 parts by weight of anti-settling agent and 7.2 parts by weight of pigment and filler;
the composite flame retardant consists of 10.4 parts by weight of aluminum hypophosphite and 1.6 parts by weight of nano boehmite;
the density of the square cloth is 600g/m 2 ；
4) Taking unsaturated polyester resin, a composite flame retardant, a BYK-A515 defoamer and an accelerator cobalt iso-octoate, and uniformly mixing to obtain a polyester mixture;
5) And (3) taking a curing agent B, namely methyl ethyl ketone peroxide, firstly spraying a polyester mixture and the curing agent B onto a surface layer, wherein the spraying pressure is 0.30MPa, the spraying time is 60s, uniformly coating the polyester mixture and the curing agent B by adopting a hairbrush to obtain a polyester mixture layer, then simultaneously spraying the polyester mixture, the curing agent B and spraying yarns onto the polyester mixture layer, wherein the spraying pressure is 0.30MPa, a spraying gun spraying the polyester mixture, the curing agent B and the spraying yarns walks at a constant speed for two times, the outlet of the polyester mixture and the curing agent B of the spraying gun forms a 45-degree angle with the outlet of the spraying yarns, compacting by adopting a pressing roller, paving square cloth, flattening by adopting the pressing roller again, and finally continuously spraying the polyester mixture, the curing agent B and the spraying yarns according to the process, compacting by the pressing roller, curing and demolding to obtain the fiber reinforced composite material.
In the fiber-reinforced composite material obtained in this example, the thickness of the surface layer was 0.36mm, and the thickness of the reinforcing layer was 4.32mm.
Example III
The invention relates to a preparation method of a fiber reinforced composite material, which comprises the following steps:
1) Taking 10 parts by weight of gel coat, wherein the gel coat is an unsaturated polyester mixture prepared from 1.0 part by weight of styrene, 4.0 parts by weight of dihydric alcohol, 4.0 parts by weight of dibasic acid, 0.04 part by weight of anti-settling agent, 0.06 part by weight of accelerator and 0.9 part by weight of pigment and filler;
2) Taking 0.15 part by weight of curing agent A, namely methyl ethyl ketone peroxide, uniformly mixing the curing agent A and gel coat, pouring the mixture into a spray can, uniformly spraying the mixture formed by the gel coat and the curing agent A onto a mold by adopting a spray gun, curing, and obtaining a surface layer when the mixture is cured to a state of sticking hands but not dirtying hands;
3) Taking 100 parts by weight of unsaturated polyester resin, 20 parts by weight of composite flame retardant, 0.4 part by weight of BYK-A515 defoamer, 0.9 part by weight of accelerator cobalt iso-octoate, 1.5 parts by weight of curing agent B methyl ethyl ketone peroxide, 30 parts by weight of jet yarn and 12 parts by weight of check cloth;
the unsaturated polyester resin is prepared from 20 parts by weight of styrene, 40 parts by weight of dihydric alcohol, 30 parts by weight of dibasic acid, 2 parts by weight of anti-settling agent and 8 parts by weight of pigment and filler;
the composite flame retardant consists of 11.2 parts by weight of aluminum hypophosphite, 0.3 part by weight of nano boehmite and 8.5 parts by weight of diphenyl sulfone polyphenyl phosphonate;
the density of the square cloth is 800g/m 2 ；
4) Taking unsaturated polyester resin, a composite flame retardant, a BYK-A515 defoamer and an accelerator cobalt iso-octoate, and uniformly mixing to obtain a polyester mixture;
5) And (3) taking a curing agent B, namely methyl ethyl ketone peroxide, firstly spraying a polyester mixture and the curing agent B onto a surface layer, wherein the spraying pressure is 0.28MPa, the spraying time is 50s, uniformly coating the polyester mixture and the curing agent B by adopting a hairbrush to obtain a polyester mixture layer, then simultaneously spraying the polyester mixture, the curing agent B and spraying yarns onto the polyester mixture layer, wherein the spraying pressure is 0.28MPa, a spraying gun spraying the polyester mixture, the curing agent B and the spraying yarns walks at a constant speed for two times, the outlet of the polyester mixture and the curing agent B of the spraying gun forms a 45-degree angle with the outlet of the spraying yarns, compacting by adopting a pressing roller, paving square cloth, flattening by adopting the pressing roller again, and finally continuously spraying the polyester mixture, the curing agent B and the spraying yarns according to the process, compacting by the pressing roller, curing and demolding to obtain the fiber reinforced composite material.
In the fiber-reinforced composite material obtained in this example, the thickness of the surface layer was 0.38mm, and the thickness of the reinforcing layer was 3.80mm.
Example IV
The invention relates to a preparation method of a fiber reinforced composite material, which comprises the following steps:
1) 15 parts of gel coat which is an unsaturated polyester mixture prepared from 1.35 parts of styrene, 6.0 parts of dihydric alcohol, 6.0 parts of dibasic acid, 0.15 parts of anti-settling agent, 0.15 parts of accelerator and 1.35 parts of pigment and filler;
2) Taking 0.225 weight parts of curing agent A, namely methyl ethyl ketone peroxide, uniformly mixing the curing agent A and gel coat, pouring the mixture into a spray can, uniformly spraying the mixture formed by the gel coat and the curing agent A onto a mold by adopting a spray gun, curing, and obtaining a surface layer when the mixture is cured to a state of sticking hands but not dirtying hands;
3) Taking 150 parts by weight of unsaturated polyester resin, 45 parts by weight of composite flame retardant, 0.6 part by weight of BYK-A515 defoamer, 1.5 parts by weight of accelerator cobalt iso-octoate, 2.25 parts by weight of curing agent B methyl ethyl ketone peroxide, 45 parts by weight of jet yarn and 18 parts by weight of check cloth;
the unsaturated polyester resin is prepared from 30 parts by weight of styrene, 52.5 parts by weight of dihydric alcohol, 52.5 parts by weight of dibasic acid, 3 parts by weight of anti-settling agent and 12 parts by weight of pigment and filler;
the composite flame retardant consists of 27.3 parts by weight of aluminum hypophosphite, 4.1 parts by weight of nano boehmite and 13.6 parts by weight of diphenyl sulfone polyphenyl phosphonate;
the density of the square cloth is 800g/m 2 ；
4) Uniformly mixing unsaturated polyester resin, a composite flame retardant, a BYK-A515 defoamer and an accelerator cobalt iso-octoate to obtain a polyester mixture;
5) And (3) taking a curing agent B, namely methyl ethyl ketone peroxide, firstly spraying a polyester mixture and the curing agent B onto a surface layer, wherein the spraying pressure is 0.28MPa, the spraying time is 50s, uniformly coating the polyester mixture and the curing agent B by adopting a hairbrush to obtain a polyester mixture layer, then simultaneously spraying the polyester mixture, the curing agent B and spraying yarns onto the polyester mixture layer, wherein the spraying pressure is 0.28MPa, a spraying gun spraying the polyester mixture, the curing agent B and the spraying yarns walks at a constant speed for two times, the outlet of the polyester mixture and the curing agent B of the spraying gun forms a 45-degree angle with the outlet of the spraying yarns, compacting by adopting a pressing roller, paving square cloth, flattening by adopting the pressing roller again, and finally continuously spraying the polyester mixture, the curing agent B and the spraying yarns according to the process, compacting by the pressing roller, curing and demolding to obtain the fiber reinforced composite material.
In the fiber-reinforced composite material obtained in this example, the thickness of the surface layer was 0.48mm, and the thickness of the reinforcing layer was 4.80mm.
Example five
The invention relates to a preparation method of a fiber reinforced composite material, which comprises the following steps:
1) 15 parts of gel coat which is an unsaturated polyester mixture prepared from 1.35 parts of styrene, 6.0 parts of dihydric alcohol, 6.0 parts of dibasic acid, 0.15 parts of anti-settling agent, 0.15 parts of accelerator and 1.35 parts of pigment and filler;
2) Taking 0.225 weight parts of curing agent A, namely methyl ethyl ketone peroxide, uniformly mixing the curing agent A and gel coat, pouring the mixture into a spray can, uniformly spraying the mixture formed by the gel coat and the curing agent A onto a mold by adopting a spray gun, curing, and obtaining a surface layer when the mixture is cured to a state of sticking hands but not dirtying hands;
3) Taking 150 parts by weight of unsaturated polyester resin, 45 parts by weight of composite flame retardant, 0.6 part by weight of BYK-A515 defoamer, 1.5 parts by weight of accelerator cobalt iso-octoate, 2.25 parts by weight of curing agent B methyl ethyl ketone peroxide, 45 parts by weight of jet yarn and 18 parts by weight of check cloth;
the unsaturated polyester resin is prepared from 30 parts by weight of styrene, 52.5 parts by weight of dihydric alcohol, 52.5 parts by weight of dibasic acid, 3 parts by weight of anti-settling agent and 12 parts by weight of pigment and filler;
the composite flame retardant consists of 26.0 parts by weight of aluminum hypophosphite, 1.7 parts by weight of nano boehmite and 17.3 parts by weight of diphenyl sulfone polyphenyl phosphonate;
the density of the square cloth is 800g/m 2 ；
4) Taking unsaturated polyester resin, a composite flame retardant, a BYK-A515 defoamer and an accelerator cobalt iso-octoate, and uniformly mixing to obtain a polyester mixture;
5) And (3) taking a curing agent B, namely methyl ethyl ketone peroxide, firstly spraying a polyester mixture and the curing agent B onto a surface layer, wherein the spraying pressure is 0.28MPa, the spraying time is 50s, uniformly coating the polyester mixture and the curing agent B by adopting a hairbrush to obtain a polyester mixture layer, then simultaneously spraying the polyester mixture, the curing agent B and spraying yarns onto the polyester mixture layer, wherein the spraying pressure is 0.28MPa, a spraying gun spraying the polyester mixture, the curing agent B and the spraying yarns walks at a constant speed for two times, the outlet of the polyester mixture and the curing agent B of the spraying gun forms a 45-degree angle with the outlet of the spraying yarns, compacting by adopting a pressing roller, paving square cloth, flattening by adopting the pressing roller again, and finally continuously spraying the polyester mixture, the curing agent B and the spraying yarns according to the process, compacting by the pressing roller, curing and demolding to obtain the fiber reinforced composite material.
In the fiber-reinforced composite material obtained in this example, the thickness of the surface layer was 0.48mm, and the thickness of the reinforcing layer was 4.32mm.
Comparative example one
A method for preparing a fiber reinforced composite material, comprising the steps of:
1) 15 parts of gel coat which is an unsaturated polyester mixture prepared from 1.35 parts of styrene, 6.0 parts of dihydric alcohol, 6.0 parts of dibasic acid, 0.15 parts of anti-settling agent, 0.15 parts of accelerator and 1.35 parts of pigment and filler;
2) Taking 0.225 weight parts of curing agent A, namely methyl ethyl ketone peroxide, uniformly mixing the curing agent A and gel coat, pouring the mixture into a spray can, uniformly spraying the mixture formed by the gel coat and the curing agent A onto a mold by adopting a spray gun, curing, and obtaining a surface layer when the mixture is cured to a state of sticking hands but not dirtying hands;
3) Taking 150 parts by weight of unsaturated polyester resin, 1.5 parts by weight of accelerator cobalt iso-octoate, 2.25 parts by weight of curing agent B methyl ethyl ketone peroxide and 45 parts by weight of jet yarn;
the unsaturated polyester resin is prepared from 30 parts by weight of styrene, 52.5 parts by weight of dihydric alcohol, 52.5 parts by weight of dibasic acid, 3 parts by weight of anti-settling agent and 12 parts by weight of pigment and filler;
4) Taking unsaturated polyester resin and promoter cobalt iso-octoate, and uniformly mixing to obtain a polyester mixture;
5) And (3) taking a curing agent B, namely methyl ethyl ketone peroxide, spraying the polyester mixture, the curing agent B and the spraying yarns on the surface layer at the same time, wherein the spraying pressure is 0.28MPa, and a spray gun for spraying the polyester mixture, the curing agent B and the spraying yarns walks at constant speed to five times, compacting by a compression roller, curing and demolding to obtain the fiber reinforced composite material, namely a first comparison sample.
In the fiber-reinforced composite material obtained in the first control sample, the thickness of the surface layer was 0.48mm, and the thickness of the reinforcing layer was 3.86mm.
Comparative example two
A method for preparing a fiber reinforced composite material, comprising the steps of:
1) 15 parts of gel coat which is an unsaturated polyester mixture prepared from 1.35 parts of styrene, 6.0 parts of dihydric alcohol, 6.0 parts of dibasic acid, 0.15 parts of anti-settling agent, 0.15 parts of accelerator and 1.35 parts of pigment and filler;
2) Taking 0.225 weight parts of curing agent A, namely methyl ethyl ketone peroxide, uniformly mixing the curing agent A and gel coat, pouring the mixture into a spray can, uniformly spraying the mixture formed by the gel coat and the curing agent A onto a mold by adopting a spray gun, curing, and obtaining a surface layer when the mixture is cured to a state of sticking hands but not dirtying hands;
3) Taking 150 parts by weight of unsaturated polyester resin, 45 parts by weight of composite flame retardant, 0.6 part by weight of BYK-A515 defoamer, 1.5 parts by weight of accelerator cobalt iso-octoate, 2.25 parts by weight of curing agent B methyl ethyl ketone peroxide and 45 parts by weight of jet yarn;
the unsaturated polyester resin is prepared from 30 parts by weight of styrene, 52.5 parts by weight of dihydric alcohol, 52.5 parts by weight of dibasic acid, 3 parts by weight of anti-settling agent and 12 parts by weight of pigment and filler;
the composite flame retardant consists of 26.0 parts by weight of aluminum hypophosphite, 1.7 parts by weight of nano boehmite and 17.3 parts by weight of diphenyl sulfone polyphenyl phosphonate;
4) Taking unsaturated polyester resin, a composite flame retardant, a BYK-A515 defoamer and an accelerator cobalt iso-octoate, and uniformly mixing to obtain a polyester mixture;
5) And (3) taking a curing agent B, namely methyl ethyl ketone peroxide, spraying the polyester mixture, the curing agent B and the spraying yarns on the surface layer at the same time, wherein the spraying pressure is 0.28MPa, and a spray gun for spraying the polyester mixture, the curing agent B and the spraying yarns walks at constant speed to five times, compacting by a compression roller, curing and demolding to obtain the fiber reinforced composite material, namely a second comparison sample.
In the fiber-reinforced composite material obtained in the second control sample, the thickness of the surface layer was 0.48mm, and the thickness of the reinforcing layer was 4.32mm.
Comparative example three
A method for preparing a fiber reinforced composite material, comprising the steps of:
1) 15 parts of gel coat which is an unsaturated polyester mixture prepared from 1.35 parts of styrene, 6.0 parts of dihydric alcohol, 6.0 parts of dibasic acid, 0.15 parts of anti-settling agent, 0.15 parts of accelerator and 1.35 parts of pigment and filler;
2) Taking 0.225 weight parts of curing agent A, namely methyl ethyl ketone peroxide, uniformly mixing the curing agent A and gel coat, pouring the mixture into a spray can, uniformly spraying the mixture formed by the gel coat and the curing agent A onto a mold by adopting a spray gun, curing, and obtaining a surface layer when the mixture is cured to a state of sticking hands but not dirtying hands;
3) Taking 150 parts by weight of unsaturated polyester resin, 1.5 parts by weight of accelerator cobalt iso-octoate, 2.25 parts by weight of curing agent B methyl ethyl ketone peroxide, 45 parts by weight of jet yarn and 18 parts by weight of check cloth;
the unsaturated polyester resin is prepared from 30 parts by weight of styrene, 52.5 parts by weight of dihydric alcohol, 52.5 parts by weight of dibasic acid, 3 parts by weight of anti-settling agent and 12 parts by weight of pigment and filler;
the density of the square cloth is 800g/m 2 ；
4) Taking unsaturated polyester resin and promoter cobalt iso-octoate, and uniformly mixing to obtain a polyester mixture;
5) Firstly, spraying a polyester mixture and a curing agent B onto a surface layer at the spraying pressure of 0.28MPa for 50s, uniformly coating the polyester mixture and the curing agent B by adopting a hairbrush to obtain a polyester mixture layer, then simultaneously spraying the polyester mixture, the curing agent B and spraying yarns onto the polyester mixture layer at the spraying pressure of 0.28MPa, uniformly walking the spraying guns for spraying the polyester mixture, the curing agent B and the spraying yarns to two back and forth, forming an angle of 45 degrees between the outlets of the polyester mixture and the curing agent B of the spraying guns and the outlets of the spraying yarns, compacting by adopting the pressing roller, paving square cloth, flattening by adopting the pressing roller again, finally continuously spraying the polyester mixture, the curing agent B and the spraying yarns according to the process, compacting by the pressing roller, curing and demolding to obtain the fiber reinforced composite material, namely a third comparison sample;
in the fiber-reinforced composite material obtained in the third comparative example, the thickness of the surface layer was 0.48mm, and the thickness of the reinforcing layer was 4.03mm.
Performing performance test experiments on five parts of the fiber-reinforced composite material obtained in the first embodiment to the fifth embodiment of the invention and on the first control sample obtained in the first comparative example, the second control sample obtained in the second comparative example and the third control sample obtained in the third comparative example respectively, wherein the experimental test indexes comprise Babbing hardness, water absorption, bending strength, tensile strength, resin content and flame retardance, wherein the Babbing hardness is measured by DIN EN 59 glass fiber reinforced plastic Barbary hardness, the water absorption is measured by ISO 62 plastic-water absorption, the bending strength is measured by ISO 14125 fiber reinforced plastic composite material bending property, the tensile strength is measured by DIN EN ISO 527-4 plastic tensile property, the 4 th part of homogeneous and heterogeneous reinforced fiber plastic composite material test conditions are measured by DIN EN ISO 527-4 plastic tensile property, the resin content is measured by ISO 1172 woven glass fiber reinforced plastic, prepreg, molding compound and the measurement calcination method of laminated plastic woven glass fiber and mineral filler content, the flame retardance is measured by heat release MAHE, and the heat release MAHE is measured by ISO5660-1 for the first part of heat release, yield and mass loss rate: the heat release rate (cone calorimeter) was limited according to the R1 classification in EN45545 and the experimental results are given in Table 1.
TABLE 1 results of different Performance tests
As can be seen from Table 1, the fiber reinforced composites obtained by the method of the present invention all had a Babbitt hardness of between 46.5 and 52.2, whereas the control one had a Babbitt hardness of 45.6, the control two had a Babbitt hardness of 40.2, and the control three had a Babbitt hardness of 43.5; thus, the fiber reinforced composite of the present invention has a greater Babbitt stiffness. The water absorption of the fiber reinforced composite material obtained by the method is between 0.05 and 0.07 percent, however, the water absorption of the first comparison sample is 0.09 percent, the water absorption of the second comparison sample is 0.08 percent, and the water absorption of the third comparison sample is 0.08 percent; therefore, the fiber reinforced composite material has smaller water absorption. The bending strength of the fiber reinforced composite material obtained by the method is 188.14-215.64MPa, however, the bending strength of the first comparison sample is 146.35MPa, the bending strength of the second comparison sample is 153.09MPa, and the bending strength of the third comparison sample is 162.87MPa; therefore, the fiber reinforced composite material has higher bending strength. The tensile strength of the fiber reinforced composite material obtained by the method is 164.26-175.81MPa, however, the tensile strength of the first control sample is 102.65MPa, the tensile strength of the second control sample is 133.61MPa, and the tensile strength of the third control sample is 154.28MPa; therefore, the fiber reinforced composite material has higher tensile strength. The resin content of the fiber reinforced composite material obtained by the method is 52.85-58.62%, the resin content of the first comparison sample is 48.17%, the resin content of the second comparison sample is 55.45%, and the resin content of the third comparison sample is 55.37%; therefore, the fiber reinforced composite material of the present invention has a suitable resin content. The heat release MAHE of the fiber reinforced composite material obtained by the method is between 79.4 and 89.7; control sample one had a heat release MARHE of up to 125.6 due to the absence of flame retardant; in the second control, the heat release MARHE was 93.9, even though a flame retardant was used; the third control sample does not use a flame retardant, and the heat release MAHE reaches 120.3MPa; therefore, the fiber reinforced composite material has better fireproof performance.
Therefore, compared with the prior art, the invention has the beneficial effects that: the fiber reinforced composite material forms a surface layer by using the gel coat and the curing agent A, forms a reinforcing layer by using the unsaturated polyester resin, the composite flame retardant, the defoaming agent, the accelerator, the curing agent B, the jet yarn and the square cloth, has scientific component selection, reasonable matching and synergistic promotion, and the surface layer and the reinforcing layer interact, so that the obtained fiber reinforced composite material has the advantages of high Babbitt hardness, small water absorption, high bending strength and tensile strength, proper resin content, greatly improved comprehensive performance of the fiber reinforced composite material, particularly the use of the composite flame retardant, greatly improved fireproof performance of the fiber reinforced composite material, and meets the requirements of special industries such as interior parts of vehicles.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.

Claims (10)

1. A fiber reinforced composite material characterized by: comprises a surface layer and a reinforcing layer, wherein the thickness ratio of the surface layer to the reinforcing layer is 1:8-12;
the surface layer comprises a gel coat and a curing agent A, wherein the adding amount of the curing agent A in the gel coat is 1-2%, and the gel coat comprises the following components in percentage by weight: 8-10% of styrene, 35-45% of dihydric alcohol, 35-45% of dibasic acid, 1-2% of auxiliary agent and 8-10% of pigment and filler;
the reinforcing layer comprises the following components in percentage by weight: 100% of unsaturated polyester resin, 10-35% of composite flame retardant, 0.3-0.5% of defoamer, 0.6-1.2% of accelerator, 1-2% of curing agent B, 20-35% of jet yarn and 10-15% of check fabric;
the composite flame retardant consists of aluminum hypophosphite and nano boehmite according to the weight ratio of 20-40:1-3, or consists of aluminum hypophosphite, nano boehmite and diphenyl sulfone polyphenyl phosphonate according to the weight ratio of 20-40:1-3:10-30.
2. The fiber reinforced composite of claim 1, wherein:
the unsaturated polyester resin comprises the following components in percentage by weight: 15-20% of styrene, 30-40% of dihydric alcohol, 30-40% of dibasic acid, 1-2% of auxiliary agent and 6-8% of pigment and filler.
3. The fiber reinforced composite of claim 1, wherein:
the defoaming agent is BYK-A515 defoaming agent.
4. The fiber reinforced composite of claim 1, wherein:
the promoter is cobalt iso-octoate.
5. The fiber reinforced composite of claim 1, wherein:
the curing agent A and the curing agent B are methyl ethyl ketone peroxide.
6. The fiber reinforced composite of claim 1, wherein:
the density of the square grid cloth is 400-800g/m 2 。
7. A method of preparing a fibre reinforced composite material according to any one of claims 1 to 6, comprising the steps of:
1) Taking gel coats and a curing agent A, uniformly mixing, spraying the mixture onto a mold, and curing the mixture until the mixture is cured to a state of sticking hands and not dirtying hands to obtain a surface layer;
2) Taking unsaturated polyester resin, a composite flame retardant, a defoaming agent and an accelerator, uniformly mixing to obtain a polyester mixture, taking a curing agent B, firstly spraying the polyester mixture and the curing agent B onto a surface layer for 40-60s, uniformly coating, then spraying the polyester mixture, the curing agent B and sprayed yarns onto the polyester mixture layer at the same time, compacting by a press roller, paving square cloth, flattening by the press roller again, and finally continuously spraying the polyester mixture, the curing agent B and the sprayed yarns, compacting by the press roller, curing and demolding to obtain the fiber reinforced composite material.
8. The method of preparing a fiber reinforced composite according to claim 7, wherein:
in the step 2), before square cloth is paved, a spray gun for spraying the polyester mixture, the curing agent B and the sprayed yarns walks at a constant speed for two times; after laying the square cloth, the spray gun spraying the polyester mixture and the curing agent B and spraying the yarn again walks back and forth at a constant speed.
9. The method of preparing a fiber reinforced composite according to claim 7, wherein:
in the step 2), the outlet of the polyester mixture and the curing agent B of the spray gun is at an angle of 45 degrees to the outlet of the spray yarn.
10. Use of a fiber reinforced composite material according to any one of claims 1-6, characterized in that:
the fiber reinforced composite is used to make interior components of vehicles.
CN202310616461.0A 2023-05-29 2023-05-29 Fiber reinforced composite material and preparation method and application thereof Pending CN116715877A (en)

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