CN107353775B - Carbon fiber reinforced resin matrix composite flame-retardant surface film and preparation method thereof - Google Patents
Carbon fiber reinforced resin matrix composite flame-retardant surface film and preparation method thereof Download PDFInfo
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- CN107353775B CN107353775B CN201710644607.7A CN201710644607A CN107353775B CN 107353775 B CN107353775 B CN 107353775B CN 201710644607 A CN201710644607 A CN 201710644607A CN 107353775 B CN107353775 B CN 107353775B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
- D06N3/0022—Glass fibres
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
- D06N3/0036—Polyester fibres
-
- 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
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- 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
-
- 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
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The invention relates to a flame-retardant surface film made of a carbon fiber reinforced resin matrix composite, which is prepared from the following raw materials in parts by weight: the preparation method comprises the following steps of (1) weighing, (2) preparing a resin mixture, (3) blending and discharging, and (4) calendering to form a film. The surface film can improve the apparent quality of a workpiece, and simultaneously solves the problem that a common epoxy resin system cannot meet the EN45545-2 flame-retardant standard.
Description
Technical Field
The invention relates to a flame-retardant surface film for a carbon fiber reinforced epoxy resin matrix composite material and a preparation method thereof, belonging to the technical field of fibers.
Background
With the vigorous advocation of energy conservation and emission reduction in China, materials and methods capable of saving energy and reducing emission are vigorously invested and researched in various fields, and the field of rail transit is no exception. As is well known, carbon fiber reinforced resin matrix composite materials are typical representatives of high-strength high-modulus materials, because the carbon fiber reinforced resin matrix composite materials are lighter in weight than aluminum alloys and not lower in mechanical strength than the aluminum alloys, the carbon fiber reinforced resin matrix composite materials become a favorite under the flag of energy conservation and emission reduction, and are widely applied to the fields of aerospace and the like. However, most of the existing flame-retardant modification is in a body addition type, and the flame-retardant modification hardly meets the flame-retardant standard of EN45545-2 on the premise of not influencing the mechanical property of the plate, so that an efficient flame-retardant method is urgently needed to be found to improve the flame-retardant level of the carbon fiber reinforced epoxy resin-based composite material, and the mechanical property of the final product plate is not influenced basically.
Disclosure of Invention
In order to solve the problems, the invention provides a flame-retardant surface film for a carbon fiber reinforced epoxy resin matrix composite material and a preparation method thereof, which can improve the apparent quality of a workpiece and solve the problem that a common epoxy resin system cannot meet the EN45545-2 flame-retardant standard.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the invention relates to a flame-retardant surface film made of a carbon fiber reinforced resin matrix composite, which is prepared from the following raw materials in parts by weight: 60-100 parts of epoxy resin, 15-25 parts of toughening agent, 4-8 parts of curing agent, 2-4 parts of accelerator, 40-0 part of flame retardant and carrier.
The invention is further improved in that: the epoxy resin is composed of low-viscosity bisphenol A epoxy resin, medium-viscosity bisphenol A epoxy resin, novolac epoxy resin and polyfunctional epoxy resin.
The invention is further improved in that: the toughening agent is composed of one or more of polysulfone, polyethersulfone, polyaryletherketone, hydroxyl-terminated nitrile rubber and carboxyl-terminated nitrile rubber.
The invention is further improved in that: the curing agent consists of one or two of dicyandiamide and 4, 4' -diaminodiphenyl sulfone.
The invention is further improved in that: the accelerant is composed of one or more of organic ureas, thioureas, imidazole compounds or Lewis acids.
The invention is further improved in that: the flame retardant consists of one or more of additive flame retardants of triphenyl phosphate, diphenyl cresyl phosphate, pentaerythritol, aluminum hydroxide, melamine phosphate, ammonium polyphosphate and zinc borate.
The invention is further improved in that: the carrier is polyester felt or glass fiber felt.
The invention relates to a preparation method of a flame-retardant surface film of a carbon fiber reinforced resin matrix composite, which comprises the following steps:
(1) weighing: weighing 60-100 parts of epoxy resin, 15-25 parts of toughening agent, 4-8 parts of curing agent, 2-4 parts of accelerator and 40-70 parts of flame retardant according to parts by weight;
(2) preparation of a resin mixture: dividing the epoxy resin weighed in the step (1) into 3 parts by mass, preparing a toughening concentrated solution or paste by hot melting the first part and a toughening agent, grinding and blending the second part and a flame retardant by a three-roll mill to prepare a flame retardant paste, and mixing the third part, a curing agent and an accelerator by a Speed Mixer to prepare a curing agent paste;
(3) blending and discharging: stirring the toughening concentrated solution or paste in the step (2) and the flame retardant paste in a 75 ℃ reaction kettle for 1h until the system is uniform, reducing the kettle temperature to below 60 ℃, adding the curing agent paste in the step (2), stirring for 15min until the system is uniform, and discharging;
(4) rolling and film forming: and (4) coating the discharged material in the step (3) by a coating machine, and then impregnating the discharged material and a carrier support on an impregnation machine to prepare the efficient flame-retardant surface film.
The invention is further improved in that: in the step (4), the coating temperature is 75-85 ℃, the impregnation temperature is 80-85 ℃, and the gram weight of the surface film is controlled to be 140-300 gsm.
The invention has the beneficial effects that: the flame-retardant surface film can form a stable and expansive flame-retardant carbon layer on the surface of the carbon fiber composite material, can effectively retard flame, insulate heat and suppress smoke, and meets the flame-retardant standard of EN 45545-2.
Detailed Description
In order to enhance the understanding of the present invention, the present invention will be described in further detail with reference to the following examples, which are provided for the purpose of illustration only and are not intended to limit the scope of the present invention.
The invention discloses a carbon fiber reinforced resin matrix composite flame-retardant surface film as shown in an embodiment, which comprises the following raw materials in parts by weight: 60-100 parts of epoxy resin, 15-25 parts of toughening agent, 4-8 parts of curing agent, 2-4 parts of accelerator, 40-0 parts of flame retardant and carrier;
wherein: the epoxy resin consists of low-viscosity bisphenol A epoxy resin, medium-viscosity bisphenol A epoxy resin, novolac epoxy resin and polyfunctional epoxy resin;
the toughening agent is composed of one or more of polysulfone, polyethersulfone, polyaryletherketone, hydroxyl-terminated nitrile rubber and carboxyl-terminated nitrile rubber;
the curing agent consists of one or two of dicyandiamide and 4, 4' -diaminodiphenyl sulfone;
the accelerant is composed of one or more of organic ureas, thioureas, imidazole compounds or Lewis acids;
the flame retardant consists of one or more of additive flame retardants of triphenyl phosphate, diphenyl cresyl phosphate, pentaerythritol, aluminum hydroxide, melamine phosphate, ammonium polyphosphate and zinc borate;
the carrier is a polyester felt or a glass fiber felt.
The invention discloses a preparation method of a flame-retardant surface film of a carbon fiber reinforced resin matrix composite, which comprises the following steps:
(1) weighing: weighing 60-100 parts of epoxy resin, 15-25 parts of toughening agent, 4-8 parts of curing agent, 2-4 parts of accelerator and 40-70 parts of flame retardant according to parts by weight;
(2) preparation of a resin mixture: dividing the epoxy resin weighed in the step (1) into 3 parts by mass, preparing a toughening concentrated solution or paste by hot melting the first part and a toughening agent, grinding and blending the second part and a flame retardant by a three-roll mill to prepare a flame retardant paste, and mixing the third part, a curing agent and an accelerator by a Speed Mixer to prepare a curing agent paste;
(3) blending and discharging: stirring the toughening concentrated solution or paste in the step (2) and the flame retardant paste in a 75 ℃ reaction kettle for 1h until the system is uniform, reducing the kettle temperature to below 60 ℃, adding the curing agent paste in the step (2), stirring for 15min until the system is uniform, and discharging;
(4) rolling and film forming: coating the discharged material in the step (3) by a coating machine, and then impregnating the discharged material and a carrier support on an impregnation machine to prepare the high-efficiency flame-retardant surface film, wherein the coating temperature is 75-85 ℃, the impregnation temperature is 80-85 ℃, and the gram weight of the surface film is controlled to be 140-300 gsm.
Example one
The invention relates to a flame-retardant surface film made of a carbon fiber reinforced resin matrix composite material, which comprises the following raw materials in parts by weight:
epoxy resin: 75 portions of
Polyether sulfone: 15 portions of
Flame retardant: 40 portions of
Curing agent and accelerator: 6 portions of
3 parts of weighed epoxy resin is divided into 3 parts by mass, the first part and polyether sulfone are subjected to hot melting to prepare toughening concentrated solution, the second part and a flame retardant are ground and blended by a three-roll mill to prepare flame retardant paste, and the third part, a curing agent and an accelerator are mixed by a Speed Mixer to prepare curing agent paste; then, uniformly stirring the toughening concentrated solution and the flame retardant paste in a 75 ℃ reaction kettle for 1h, reducing the kettle temperature to below 60 ℃, adding the curing agent paste, uniformly stirring for 15min, and discharging; finally, the discharged material is coated by a coating machine and then is impregnated with a carrier support on an impregnation machine to prepare the high-efficiency flame-retardant surface film.
Plates obtained by singly autoclave curing the EM 112-42-HFW 220T-1000 prepreg of Jiangsu Henshen company and plates obtained by co-curing the EM 112-42-HFW 220T-1000 carbon fiber prepreg and the flame-retardant surface film of Jiangsu Henshen company are respectively marked as No. 1 and No. 2, and the basic performance of the obtained surface film and the flame-retardant performance of the plates are as follows:
TABLE 1 post-curing Properties of surface film of carbon fiber composites
TABLE 2 comparison of flame retardancy of flame retardant carbon fiber composites with flame retardant surface film and without flame retardant surface film
| Test Standard/En 45545-2 | CEF/kW/m2 | MARHE/kW/m2 | Ds(4) | VOF4 |
| 1# | 5 | -- | 915 | 1430 |
| 2# | 25 | -- | 496 | 905 |
Wherein: 2# meets the flame retardant standard of HL1 in EN45545-2 (Critical radiation energy CFE value)>Smoke density Ds (4) value at 20, 4min<Smoke toxicity VOF at 600, 4min4Value of<1200）
Example two
The invention relates to a flame-retardant surface film material for a carbon fiber reinforced epoxy resin matrix composite material, which is prepared by weighing the following components in parts by mass:
epoxy resin: 80 portions
Carboxyl-terminated nitrile rubber: 10 portions of
Flame retardant: 60 portions of
Curing agent and accelerator: 7 portions of
Dividing the weighed epoxy resin into 3 parts by mass, preparing a toughening paste from the first part and carboxyl-terminated butadiene-acrylonitrile rubber, grinding and blending the second part and a flame retardant by a three-roll mill to prepare a flame retardant paste, and mixing the third part, a curing agent and an accelerator by a Speed Mixer to prepare a curing agent paste; then, uniformly stirring the toughening paste and the flame retardant paste in a 75 ℃ reaction kettle for 1h, reducing the kettle temperature to below 60 ℃, adding the curing agent paste, uniformly stirring for 15min, and discharging; finally, the discharged material is coated by a coating machine and then is impregnated with a carrier support on an impregnation machine to prepare the high-efficiency flame-retardant surface film.
A plate obtained by co-curing the EM112-42% -HFW200T-1000 carbon fiber prepreg and the flame-retardant surface film of Jiangsu Hengshen company is marked as No. 3, and the basic performance of the obtained surface film and the flame-retardant performance of the plate are as follows:
TABLE 3 post-curing Properties of surface film of carbon fiber composites
| Test items | Test condition/reference method | Test results |
| Appearance of the product | Visual inspection at 23 deg.C | Compact, smooth and flat |
| Cross scribing adhesion | 23℃，GB/T9286 | 0-stage non-debonding |
| Surface hardness (Babbitt hardness) | 23℃ | 66 |
| Glass transition temperature | Room temperature dry/ASTM D7028-07 | 108 |
TABLE 4 comparison of flame retardancy of flame retardant carbon fiber composites with flame retardant surface film without flame retardant surface film
| Test Standard/En 45545-2 | CEF/kW/m2 | MARHE/kW/m2 | Ds(4) | VOF4 |
| 1# | 5 | -- | 915 | 1430 |
| 3# | 37 | 82 | 263 | 468 |
Wherein: no. 3 meets the flame retardant standard (critical radiation energy CFE value) of HL2 in EN45545-2>20, maximum average Heat Release Rate MARHE value<Cigarette for 90, 4minDensity Ds (4) value<Smoke toxicity VOF at 300, 4min4Value of<600）。
Claims (4)
1. The flame-retardant surface film of the carbon fiber reinforced resin matrix composite is characterized in that: the surface film material consists of the following raw materials in parts by weight: 60-100 parts of epoxy resin, 15-25 parts of toughening agent, 4-8 parts of curing agent, 2-4 parts of accelerator, 40-70 parts of flame retardant and carrier,
the preparation method of the flame-retardant surface film of the carbon fiber reinforced resin matrix composite comprises the following steps:
(1) weighing: weighing 60-100 parts of epoxy resin, 15-25 parts of toughening agent, 4-8 parts of curing agent, 2-4 parts of accelerator and 40-70 parts of flame retardant according to parts by weight;
(2) preparation of a resin mixture: dividing the epoxy resin weighed in the step (1) into 3 parts by mass, preparing a toughening concentrated solution or paste by hot melting the first part and a toughening agent, grinding and blending the second part and a flame retardant by a three-roll mill to prepare a flame retardant paste, and mixing the third part, a curing agent and an accelerator by a Speed Mixer to prepare a curing agent paste;
(3) blending and discharging: stirring the toughening concentrated solution or paste in the step (2) and the flame retardant paste in a 75 ℃ reaction kettle for 1h until the system is uniform, reducing the kettle temperature to below 60 ℃, adding the curing agent paste in the step (2), stirring for 15min until the system is uniform, and discharging;
(4) rolling and film forming: coating the discharged material in the step (3) by a coating machine, and then impregnating the discharged material and a carrier support on an impregnation machine to prepare a high-efficiency flame-retardant surface film, wherein the coating temperature is 75-85 ℃, the impregnation temperature is 80-85 ℃, and the gram weight of the surface film is controlled to be 140-300 gsm;
wherein: the accelerant consists of one or more of organic ureas, thioureas, imidazole compounds or Lewis acids;
the flame retardant consists of one or more of additive flame retardants, namely triphenyl phosphate, diphenyl cresyl phosphate, pentaerythritol, aluminum hydroxide, melamine phosphate, ammonium polyphosphate and zinc borate;
the carrier is a polyester felt or a glass fiber felt.
2. The flame-retardant surface film made of carbon fiber reinforced resin matrix composite according to claim 1, wherein: the epoxy resin consists of low-viscosity bisphenol A epoxy resin, medium-viscosity bisphenol A epoxy resin, novolac epoxy resin and polyfunctional epoxy resin.
3. The flame-retardant surface film made of carbon fiber reinforced resin matrix composite according to claim 1, wherein: the toughening agent is composed of one or more of polysulfone, polyethersulfone, polyaryletherketone, hydroxyl-terminated nitrile rubber and carboxyl-terminated nitrile rubber.
4. The flame-retardant surface film made of carbon fiber reinforced resin matrix composite according to claim 1, wherein: the curing agent consists of one or two of dicyandiamide and 4, 4' -diaminodiphenyl sulfone.
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| GB2568727B (en) * | 2017-11-24 | 2020-06-24 | Gurit Uk Ltd | Fire-retardant composite materials |
| CN112625284B (en) * | 2020-12-11 | 2023-01-24 | 江苏恒神股份有限公司 | Continuous fiber reinforced thermosetting flame-retardant prepreg and preparation method thereof |
| CN114015200A (en) * | 2021-10-12 | 2022-02-08 | 许继集团有限公司 | Flame-retardant epoxy resin insulating material and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102108185A (en) * | 2010-12-29 | 2011-06-29 | 黑龙江省科学院石油化学研究院 | Epoxy matrix resin and prepreg and preparation method thereof and device for preparation thereof |
| CN105694665A (en) * | 2016-01-28 | 2016-06-22 | 浙江港流高分子科技有限公司 | Flame-retardant coiled material and preparation method thereof |
| CN106046680A (en) * | 2016-05-30 | 2016-10-26 | 中航复合材料有限责任公司 | Flame-retardant and heat-resistant epoxy resin for self-adhesive prepreg |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102108185A (en) * | 2010-12-29 | 2011-06-29 | 黑龙江省科学院石油化学研究院 | Epoxy matrix resin and prepreg and preparation method thereof and device for preparation thereof |
| CN105694665A (en) * | 2016-01-28 | 2016-06-22 | 浙江港流高分子科技有限公司 | Flame-retardant coiled material and preparation method thereof |
| CN106046680A (en) * | 2016-05-30 | 2016-10-26 | 中航复合材料有限责任公司 | Flame-retardant and heat-resistant epoxy resin for self-adhesive prepreg |
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