CN108411629A - A kind of surface has the carbon fiber of flame retardant coating, preparation method and applications - Google Patents
A kind of surface has the carbon fiber of flame retardant coating, preparation method and applications Download PDFInfo
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- CN108411629A CN108411629A CN201810129198.1A CN201810129198A CN108411629A CN 108411629 A CN108411629 A CN 108411629A CN 201810129198 A CN201810129198 A CN 201810129198A CN 108411629 A CN108411629 A CN 108411629A
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- carbon fiber
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Abstract
The invention discloses the carbon fiber that a kind of surface has flame retardant coating, there is the compound flame retardant coating of at least one layer of material composition by two class oppositely chargeds on surface；Preparation method is also disclosed, this method quickly constructs flame retardant coating using physical method on surface, and provides the application of this kind of carbon fiber.Its flame retardant coating of carbon fiber provided by the invention is deposited on surface, does not destroy its structure and does not influence the preparation process of composite material；Preparation method is simple and practicable, environmentally protective, and it is fast that coating constructs speed, is evenly distributed, and operating efficiency is high；Gained composite material has excellent flame retardant property and good mechanical property.This method is suitable for fibre reinforced flame-retarded resin based composites, has good application prospect and value in fields such as space flight and aviation, communications and transportation, sports equipments.
Description
Technical field
The present invention relates to a kind of surface flame-retardant modified carbon fiber, preparation method and applications more particularly to a kind of surface to cover
The surface flame-retardant modified carbon fiber for having covered compound flame retardant coating, the preparation side of the flame retardant coating is quickly constructed by physical method
Method and the carbon fiber are as enhancing, application of the fire proofing in high molecular polymer.
Background technology
Carbon fiber have small good high specific strength, high ratio modulus, resistance to low temperature, endurance, coefficient of thermal expansion, creep resistant,
A series of excellent performances such as friction coefficient is low, are widely applied in many fields.In recent years to the research master of carbon fiber
Concentrate on carbon fiber enhancement resin base (CFRP) composite material.
CFRP is since it is with a series of excellent properties such as high intensity, high-modulus, low-density, dimensionally stable, in aviation
The fields such as space flight, automobile, ship, war industry and athletic sports appliance are used widely, but high molecular polymer is fire-retardant
Performance is poor so that the application of CFRP is restricted.Therefore, the resistance of carbon fibre reinforced high-molecular polymer composites is improved
Combustion performance is of great significance.
The fire-retardant of CFRP composite materials mainly adds fire retardant in high molecular polymer matrix at present, although the method
Improve its flame retardant property, but when additive amount is higher, due to fire retardant in resin matrix dispersion problem, can in certain journey
The mechanical performance that composite material is destroyed on degree, limits its application field, it is therefore proposed that CFRP composite material resistances can either be improved
The ways and means of its mechanical performance can not be destroyed while firing performance again, are had a good application prospect and practical significance.
Invention content
In order to overcome problems of the prior art, present invention firstly provides the carbon that a kind of surface has flame retardant coating
Fiber, and provide a kind of method and the flame retardant coating for quickly constructing flame retardant coating in carbon fiber surface with physical method
Application of the carbon fiber in the reinforcing material and fire proofing as high molecular polymer.Carbon fiber provided by the present invention is made
For the reinforcing material and fire proofing of high molecular polymer so that the high molecular polymer being prepared can have excellent simultaneously
Flame retardant property and mechanical performance, solve defect existing in the prior art.
The present invention is achieved by the following technical solutions：
A kind of surface has the carbon fiber of flame retardant coating, it is characterised in that：Including carbon fiber and its surface covering it is compound
Object flame retardant coating, the compound flame retardant coating contain the substance of two class oppositely chargeds.
Further, the substance of the two class oppositely chargeds includes electrolyte and/or function nano particle.
Further, the substance in the substance of the two class oppositely chargeds is cationic polyelectrolyte, function is received
One or more solution in rice corpuscles 1；Another substance be anion electrolyte, one kind in function nano particle 2 or
A variety of solution, such as aqueous solution.
Further, the preferred chitosan of the cationic polyelectrolyte, poly-L-arginine hydrochloride, polylysine, poly- more
Bar amine, polyallylamine hydrochloride, polydimethyldiallyl ammonium chloride, polyethyleneimine, diallyl dimethyl ammoniumchloride,
Silane coupling agent, polyacrylamide, polypropylene amine, polyvinyl alcohol, 1 preferred function graphite alkene of nano-particle, the ammonia of functionalization
Base carbon nano tube, carbon nano-fiber, nano-titanium dioxide, nano silicon dioxide.
Further, the anion electrolyte is sodium alginate, tannic acid, hyaluronic acid, glutamic acid, deoxyribose
Nucleic acid, gelatin, cyclodextrin, phytic acid, functional fiber element, kayexalate, polyvinylsulfonic acid, polyacrylic acid, poly
Phosphate, melamine phosphate, function nano particle 2 are stratiform double-layered hydroxides, carboxylic carbon nano-tube, laminar silicic acid
Salt, nano-aluminium oxide.
A kind of preparation method of carbon fiber of the surface with flame retardant coating, includes the following steps：Carbon fiber is immersed in one
Can be specifically to mix the aqueous solution of two kinds of substances in the mixed solution for determining the substance of the two class oppositely chargeds of concentration
Carbon fiber is impregnated wherein again after closing, or carbon fiber is first immersed in the aqueous solution of certain density one of which substance,
Then the aqueous solution of another substance is added, is fully dipped to carbon fiber surface and forms at least one layer of compound flame retardant coating, obtain
There is the carbon fiber of compound flame retardant coating to a kind of surface；Above-mentioned steps can be with repeated several times.
Further, the pH value of the aqueous solution of two substances is 3-11.
It further, can be by adjusting the concentration of the electrolyte and/or function nano particle, Qi Shui in the above method
The number that the number and the method for solution repeat, is prepared carbon fiber surface different composite object flame retardant coating content and shape
The carbon fiber of looks.
Further, this approach includes the following steps：
(1) under room temperature, the water-soluble of the substance for the two classes oppositely charged that mass concentration is 0.1-10% is respectively configured
Liquid；
(2) carbon fiber is immersed in the mixed solution of two kinds of substances of step (1) preparation, wherein each substance is water-soluble
Liquid is 50-300 parts；
(3) carbon fiber is impregnated into 5-60min in the mixed solution of two substances；
(4) it is taken out after carbon fiber surface forms at least one layer of compound flame retardant coating, obtains a kind of surface tool
There is the carbon fiber of flame retardant coating；
Above-mentioned steps can be with repeated several times.
Further, after the carbon fiber prepares completion, 10- can be dried in 65-95 DEG C of convection oven
30min is cooled to room temperature later, you can is used.
Above-mentioned surface has the reinforcing material and fire proofing that the carbon fiber of flame retardant coating can be used as high molecular polymer, example
It such as can be adapted for enhancing flame-retardant high-molecular polymer such as polypropylene, polyurethane, makrolon, epoxy resin.
Compared with prior art, the beneficial effects of the invention are as follows：
Preparation method is simple by the present invention, and operation is efficient, is carried out in room temperature aqueous solution, environmentally protective.The present invention
Using the interaction between two substances, the compound that forms it into fast deposition and can be evenly distributed on inert carbon fiber
Dimension table face.The presence of compound flame retardant coating will not change the structure of carbon fiber, and not interfere with the preparation process of composite material,
And it can also be by changing the type of two substances, the number of two substance aqueous solutions and carbon fiber in two substance aqueous solutions
In soaking time and impregnate number and obtain the fibre reinforced high score for meeting different flame retardant properties and mechanical property requirements
Sub- polymer composites.In addition, carbon fiber surface is smooth, inertia is big, active function groups are few, make carbon fiber and resin matrix it
Between interface cohesion it is weaker, and in the compound flame retardant coating of carbon fiber surface contain a large amount of active groups, itself and resin can be passed through
Alternate interfacial reaction of interaction and two between matrix etc. improves composite material machinery performance, obtains with good flame-retardance
It can be with the carbon fibre reinforced high-molecular polymer composites of mechanical performance.Carbon fibre reinforced high-molecular prepared by the present invention is poly-
Compound composite material has broad application prospects and practical value in fields such as space flight and aviation, communications and transportation, sports equipments.
Description of the drawings
Fig. 1 is the scanning electron microscope diagram that surface does not have the carbon fiber of compound flame retardant coating to amplify 1000 times.
Fig. 2 is that the carbon fiber for being attached to 1 layer of compound flame retardant coating of gained in embodiment 2 in the present invention amplifies 1000 times
Scanning electron microscope diagram.
Fig. 3 is the carbon fiber amplification 3000 for being attached to 1 layer of compound flame retardant coating of gained in embodiment 20 in the present invention
Scanning electron microscope diagram again.
Fig. 4 is the carbon fiber amplification 2000 for being attached to 1 layer of compound flame retardant coating of gained in embodiment 22 in the present invention
Scanning electron microscope diagram again.
Fig. 5 is the carbon fiber amplification 1000 for being attached to 1 layer of compound flame retardant coating of gained in embodiment 30 in the present invention
Scanning electron microscope diagram again.
The carbon fiber surface modified from the mixed solution that can be seen that in Fig. 2-5 by two substances of oppositely charged
There is apparent flame retardant coating, illustrates that the present invention can be by compound flame retardant coating fast deposition in carbon fiber surface.
Specific implementation mode
The present invention is further explained in the light of specific embodiments, it is necessary to be pointed out that embodiment cannot manage
Solution is limiting the scope of the invention, and the person skilled in the art in the field is the present invention content according to the above invention
Some understand and adjustment should belong to the scope of protection of the present invention.
In addition, it is worth noting that：
(1) number of material used is mass parts in embodiment, and the content of compound flame retardant coating accounts for for it containing resistance
Fire the mass percent of the carbon fiber of coating.
(2) limit oxygen index gone out given in following comparative example and embodiment is to use HC-2C type oxygen index measurers, is pressed
It is obtained according to GB/T2406-1993 tests；Vertical combustion grade (vertical combustion UL-94) is to use CZF-2 type Vertical combustion instruments,
It is obtained according to GB/T2408-1996 tests, thickness of sample 3.2mm.
(3) impact strength test (notch) is newly to think carefully ZBC 1400-2 type Charpy impact machine testers using Shenzhen, is pressed
What the bioassay standard GB/T 1843-2008 tests according to cantilever beam impact strength obtained；Bending strength, bending modulus and interlayer are cut
Shearing stress is newly to think carefully that CMT Series Microcomputers control electronic universal tester using Shenzhen, respectively according to unidirectional fibre reinforced plastics
Performance test method GB3356-82 and unidirectional fibre reinforced plastics tensile strength test method GB/T 1040.5-2008 tests obtain
.
Embodiment 1
Under room temperature, it is water-soluble that a certain amount of carbon fiber is immersed in the chitosan that 50 parts of mass concentrations are 0.1%, pH value is 3
Liquid, is then added at one time that 50 parts of mass concentrations are 0.1%, pH value is 4 melamine phosphate aqueous solutions, and carbon fiber is in above-mentioned institute
It obtains after impregnating 60min in mixed solution, be drawn off and dry 20min in 80 DEG C of baking oven, obtain surface and contain fire-retardant painting
The carbon fiber of layer, flame retardant coating content are 3.2%.
Embodiment 2
Under room temperature, it is water-soluble that a certain amount of carbon fiber is immersed in the chitosan that 300 parts of mass concentrations are 2%, pH value is 4
Liquid, it is 5% polyphosphoric acids aqueous ammonium to be then added at one time 300 parts of mass concentrations, and carbon fiber is in above-mentioned gained mixed solution
After middle immersion 60min, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain the carbon fiber that flame retardant coating is contained on surface,
Flame retardant coating content is 8.2%.
Embodiment 3
Under room temperature, a certain amount of carbon fiber is immersed in the polyethyleneimine aqueous amine that 100 parts of mass concentrations are 2%, pH value is 7
Solution, it is 2% melamine phosphate aqueous solution to be then added at one time 100 parts of mass concentrations, and carbon fiber is mixed in above-mentioned gained
After impregnating 30min in solution, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain the carbon that flame retardant coating is contained on surface
Fiber, flame retardant coating content are 4.7%.
Embodiment 4
Under room temperature, it is 2% that a certain amount of carbon fiber, which is immersed in 50 parts of mass concentrations, the polyethyleneimine aqueous amine that pH value is 7
Solution aqueous solution, is then added at one time the ammonium polyphosphate aqueous solution that 50 parts of mass concentrations are 3%, and carbon fiber is mixed in above-mentioned gained
It closes after impregnating 5min in solution, be drawn off and dry 20min in 80 DEG C of baking oven, obtain the carbon that flame retardant coating is contained on surface
Fiber, flame retardant coating content are 3.9%.
Embodiment 5
Under room temperature, by a certain amount of carbon fiber be immersed in 150 parts of mass concentrations be 3%, the polyethyleneimine that pH value is 11
Aqueous solution aqueous solution, is then added at one time the deoxyribonucleotide aqueous solution that 150 parts of mass concentrations are 5%, and carbon fiber exists
After impregnating 40min in above-mentioned gained mixed solution, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain surface and contain
The carbon fiber of flame retardant coating, flame retardant coating content are 5.3%.
Embodiment 6
Under room temperature, a certain amount of carbon fiber is immersed in the polyethyleneimine aqueous amine that 150 parts of mass concentrations are 5%, pH value is 7
Solution aqueous solution, is then added at one time the phytic acid aqueous solution that 150 parts of mass concentrations are 8%, and carbon fiber is mixed in above-mentioned gained
After impregnating 20min in solution, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain the carbon that flame retardant coating is contained on surface
Fiber, flame retardant coating content are 4.7%.
Embodiment 7
Under room temperature, a certain amount of carbon fiber is immersed in the poly dimethyl allyl chlorination that 200 parts of mass concentrations are 4%
Aqueous ammonium, is then added at one time the phytic acid aqueous solution that 200 parts of mass concentrations are 7%, and carbon fiber mixes molten in above-mentioned gained
After impregnating 40min in liquid, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain the carbon fiber that flame retardant coating is contained on surface
Dimension, flame retardant coating content are 6.4%.
Embodiment 8
Under room temperature, a certain amount of carbon fiber is immersed in the polypropylene amine hydrochloric acid that 200 parts of mass concentrations are 8%, pH value is 5
Then saline solution is added at one time the melamine phosphate aqueous solution that 200 parts of mass concentrations are 8%, pH value is 5, carbon fiber
After impregnating 50min in above-mentioned gained mixed solution, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain surface and contain
It is 7.3% to have the carbon fiber of flame retardant coating, flame retardant coating content.
Embodiment 9
Under room temperature, a certain amount of carbon fiber is immersed in the poly-dopamine aqueous solution that 250 parts of mass concentrations are 10%, then
It is added at one time the polyacrylic acid aqueous solution that 250 parts of mass concentrations are 10%, carbon fiber impregnates in above-mentioned gained mixed solution
After 50min, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain the carbon fiber that flame retardant coating is contained on surface, fire-retardant painting
Layer content is 8.5%.
Embodiment 10
Under room temperature, a certain amount of carbon fiber is immersed in the gamma-aminopropyl-triethoxy silicon that 100 parts of mass concentrations are 3%
Alkane aqueous solution, is then added at one time the montmorillonite aqueous solution that 100 parts of mass concentrations are 5%, and carbon fiber is mixed in above-mentioned gained
After impregnating 40min in solution, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain the carbon that flame retardant coating is contained on surface
Fiber, flame retardant coating content are 4.5%.
Embodiment 11
Under room temperature, a certain amount of carbon fiber is immersed in the nano-titanium dioxide aqueous solution that 200 parts of mass concentrations are 1%,
Then it is added at one time the polyphosphoric acids sodium solution that 200 parts of mass concentrations are 6%, carbon fiber soaks in above-mentioned gained mixed solution
After steeping 20min, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain the carbon fiber that flame retardant coating is contained on surface, it is fire-retardant
Coating levels are 4.3%.
Embodiment 12
Under room temperature, a certain amount of carbon fiber is immersed in the chitosan aqueous solution that 150 parts of mass concentrations are 7%, then one
The nano-aluminium oxide solution that 150 parts of mass concentrations are 3% is added in secondary property, and carbon fiber impregnates in above-mentioned gained mixed solution
After 10min, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain the carbon fiber that flame retardant coating is contained on surface, fire-retardant painting
Layer content is 5.2%.
Embodiment 13
Under room temperature, a certain amount of carbon fiber is immersed in the poly-vinyl alcohol solution that 250 parts of mass concentrations are 4%, then one
The montmorillonite solution that 200 parts of mass concentrations are 4% is added in secondary property, after carbon fiber impregnates 10min in above-mentioned gained mixed solution,
It is drawn off and dries 20min in 80 DEG C of baking oven, obtain the carbon fiber that flame retardant coating is contained on surface, flame retardant coating content is
5.9%.
Embodiment 14
Under room temperature, it is water-soluble that a certain amount of carbon fiber is immersed in the L-arginine hydrochloride that 300 parts of mass concentrations are 5%
Liquid, it is 5% glutamic acid and the mixed solution of hyaluronic acid to be then added at one time 300 parts of mass concentrations, and carbon fiber is upper
It states after impregnating 30min in gained mixed solution, be drawn off and dry 20min in 80 DEG C of baking oven, obtain surface and contain resistance
The carbon fiber of coating is fired, flame retardant coating content is 6.4%.
Embodiment 15
Under room temperature, a certain amount of carbon fiber is immersed in the polyacrylamide aqueous amine that 250 parts of mass concentrations are 6%, pH value is 3
Solution, be then added at one time 250 parts of mass concentrations be 4% kayexalate and polyvinylsulfonic acid mixing it is molten
Liquid after carbon fiber impregnates 30min in above-mentioned gained mixed solution, is drawn off and dries 20min in 80 DEG C of baking oven, obtain
Contain the carbon fiber of flame retardant coating to surface, flame retardant coating content is 6.8%.
Embodiment 16
Under room temperature, a certain amount of carbon fiber is immersed in the chitosan aqueous solution that 200 parts of mass concentrations are 6%, then one
It is 3% phytic acid and the mixed solution of gelatin that 200 parts of mass concentrations, which are added, in secondary property, and carbon fiber is in above-mentioned gained mixed solution
After impregnating 20min, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain the carbon fiber that flame retardant coating is contained on surface, hinder
It is 5.6% to fire coating levels.
Embodiment 17
Under room temperature, a certain amount of carbon fiber is immersed in the polylysine aqueous solution that 300 parts of mass concentrations are 65%, then
It is 4% tannic acid and the mixed solution of sodium alginate to be added at one time 300 parts of mass concentrations, and carbon fiber is mixed in above-mentioned gained
It closes after impregnating 40min in solution, be drawn off and dry 20min in 80 DEG C of baking oven, obtain surface and contain flame retardant coating
Carbon fiber, flame retardant coating content are 6.2%.
Embodiment 18
Under room temperature, a certain amount of carbon fiber is immersed in the polylysine aqueous solution that 50 parts of mass concentrations are 1%, then one
It is 1% cyclodextrin and the aqueous solution of sodium alginate that 50 parts of mass concentrations, which are added, in secondary property, and carbon fiber mixes molten in above-mentioned gained
After impregnating 10min in liquid, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain the carbon fiber that flame retardant coating is contained on surface
Dimension, flame retardant coating content are 2.8%.
Embodiment 19
Under room temperature, a certain amount of carbon fiber is immersed in the nano silicon dioxide aqueous solution that 100 parts of mass concentrations are 1%,
Then it is added at one time the mixing that 100 parts of mass concentrations are respectively 2% and 1% melamine phosphate and sodium carboxymethylcellulose
Solution after carbon fiber impregnates 20min in above-mentioned gained mixed solution, is drawn off and is dried in 80 DEG C of baking oven 20min,
The carbon fiber that flame retardant coating is contained on surface is obtained, flame retardant coating content is 3.5%.
Embodiment 20
Under room temperature, a certain amount of carbon fiber is immersed in the polyethyleneimine aqueous amine that 300 parts of mass concentrations are 2%, pH value is 7
Then solution is added at one time ammonium polyphosphate and carboxylic carbon nano-tube that 300 parts of mass concentrations are respectively 3% and 0.1%
Mixed solution, after carbon fiber impregnates 30min in above-mentioned gained mixed solution, be drawn off and dry in 80 DEG C of baking oven
20min, obtains the carbon fiber that flame retardant coating is contained on surface, and flame retardant coating content is 6.8%.
Embodiment 21
Under room temperature, a certain amount of carbon fiber is immersed in the nanometer titanium dioxide that 300 parts of mass concentrations are respectively 1% and 6%
The mixed solution of titanium and polydimethyl diallyl ammonium chloride, be then added at one time 300 parts of mass concentrations be respectively 7% it is more
Polyphosphate sodium aqueous solution is drawn off and after carbon fiber impregnates 60min in above-mentioned gained mixed solution in 80 DEG C of baking oven
Dry 20min, obtains the carbon fiber that flame retardant coating is contained on surface, and flame retardant coating content is 8.5%.
Embodiment 22
Under room temperature, by a certain amount of carbon fiber be immersed in 50 parts of mass concentrations be respectively 1% and 2% graphene oxide and
Then the mixed solution of polyacrylamide is added at one time the polyphosphoric acids aqueous solutions of potassium that 50 parts of mass concentrations are respectively 2%, carbon
After fiber impregnates 30min in above-mentioned gained mixed solution, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain table
The carbon fiber of flame retardant coating is contained in face, and flame retardant coating content is 4.3%.
Embodiment 23
Under room temperature, a certain amount of carbon fiber is immersed in the chitosan and polylysine that 150 parts of mass concentrations are 1%
Then mixed solution is added at one time the double-layered hydroxides aqueous solution that 150 parts of mass concentrations are 0.1%, carbon fiber is above-mentioned
After impregnating 50min in gained mixed solution, be drawn off and the dry 20min in 80 DEG C of baking oven, obtain surface contain it is fire-retardant
The carbon fiber of coating, flame retardant coating content are 3.8%.
Embodiment 24
Under room temperature, a certain amount of carbon fiber is immersed in chitosan and the L-arginine salt that 100 parts of mass concentrations are 5%
Then the mixed solution of hydrochlorate is added at one time the sodium alginate aqueous solution that 100 parts of mass concentrations are 10%, carbon fiber is above-mentioned
After impregnating 30min in gained mixed solution, be drawn off and the dry 20min in 80 DEG C of baking oven, obtain surface contain it is fire-retardant
The carbon fiber of coating, flame retardant coating content are 5.8%.
Embodiment 25
Under room temperature, a certain amount of carbon fiber is immersed in the poly-dopamine that 200 parts of mass concentrations are respectively 7% and 0.1%
With the mixed solution of aminated carbon nano tube, it is then added at one time the kayexalate water that 200 parts of mass concentrations are 6%
Solution after carbon fiber impregnates 60min in above-mentioned gained mixed solution, is drawn off and is dried in 80 DEG C of baking oven 20min,
The carbon fiber that flame retardant coating is contained on surface is obtained, flame retardant coating content is 6.6%.
Embodiment 26
Under room temperature, a certain amount of carbon fiber is immersed in the nano-silica that 100 parts of mass concentrations are respectively 0.1% and 2%
Then the mixed solution of SiClx and polyethyleneimine is added at one time the montmorillonite aqueous solution that 100 parts of mass concentrations are 0.1%,
After carbon fiber impregnates 30min in above-mentioned gained mixed solution, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain
The carbon fiber of flame retardant coating is contained on surface, and flame retardant coating content is 2.3%.
Embodiment 27
Under room temperature, by a certain amount of carbon fiber be immersed in 150 parts of mass concentrations be respectively 4% and 1% polyvinyl alcohol and
Then the mixed solution of graphene oxide is added at one time the nano-aluminium oxide solution that 150 parts of mass concentrations are 4%, carbon
After fiber impregnates 60min in above-mentioned gained mixed solution, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain table
The carbon fiber of flame retardant coating is contained in face, and flame retardant coating content is 6.7%.
Embodiment 28
Under room temperature, a certain amount of carbon fiber is immersed in chitosan and the γ-that 200 parts of mass concentrations are respectively 3% and 4%
Then the mixed solution of aminopropyl triethoxysilane is added at one time the phytic acid that 200 parts of mass concentrations are respectively 4% and 3%
It is drawn off and in 80 DEG C of baking after carbon fiber impregnates 20min in above-mentioned gained mixed solution with the mixed solution of tannic acid
Dry 20min in case, obtains the carbon fiber that flame retardant coating is contained on surface, and flame retardant coating content is 6.8%.
Embodiment 29
Under room temperature, a certain amount of carbon fiber is immersed in the polyethyleneimine that 250 parts of mass concentrations are respectively 5% and 2%
With the mixed solution of polydimethyl diallyl ammonium chloride, it is respectively 7% He to be then added at one time 250 parts of mass concentrations
0.1% melamine phosphate and the mixed solution of carboxylic carbon nano-tube, carbon fiber impregnate in above-mentioned gained mixed solution
After 40min, it is drawn off and dries 20min in 80 DEG C of baking oven, obtain the carbon fiber that flame retardant coating is contained on surface, fire-retardant painting
Layer content is 7.7%.
Embodiment 30
Under room temperature, a certain amount of carbon fiber is immersed in the polypropylene amine salt that 150 parts of mass concentrations are respectively 5% and 5%
Then the mixed solution of hydrochlorate and polyacrylamide is added at one time the poly phosphorus that 150 parts of mass concentrations are respectively 9% and 1%
The mixed solution of sour ammonium and stratiform double-layered hydroxides is taken after carbon fiber impregnates 50min in above-mentioned gained mixed solution
Go out and dry 20min in 80 DEG C of baking oven, obtain the carbon fiber that flame retardant coating is contained on surface, flame retardant coating content is 7.4%.
Embodiment 31
Under room temperature, a certain amount of carbon fiber is immersed in the polyethyleneimine that 300 parts of mass concentrations are respectively 9% and 1%
With the mixed solution of carbon nano-fiber, it is then added at one time the ammonium polyphosphate that 300 parts of mass concentrations are respectively 6% and 4%
It is drawn off and in 80 DEG C of baking after carbon fiber impregnates 30min in above-mentioned gained mixed solution with the mixed solution of montmorillonite
Dry 20min in case, obtains the carbon fiber that flame retardant coating is contained on surface, and flame retardant coating content is 9.1%.
In order to which the enhancing and flame retardant effect, the present invention of investigating carbon fiber of the surface with flame retardant coating prepared by the present invention will
Prepared surface has the carbon fiber of flame retardant coating respectively at enhancing and polypropylene flame redardant, polyamides in above section embodiment
Amine, makrolon and epoxy resin, and test the limit oxygen index, vertical combustion and mechanical performance of each composite material.
Comparative example 1
First there is no 50 parts of 100 parts of the carbon fiber of flame retardant coating and polypropylene to be respectively put into double screw extruder on surface,
It is followed successively by each section of heating temperature of discharge port in feed inlet：It is melted at 190 DEG C, 210 DEG C, 220 DEG C, 220 DEG C, 220 DEG C, 210 DEG C
Blending extrusion, cuts into pellet by comminutor after being cooled by water, and injection molding obtains fibre reinforced PP composite material
(PP/CF).The LOI of the composite material is that 22%, UL-94 is stepless；Tensile strength is 195.3MPa, and stretch modulus is
7.7GPa, impact strength 4.1kJ/m2。
Comparative example 2
First there is no PA650 parts of 100 parts of the carbon fiber of flame retardant coating and polyamide to be respectively put into double screw extruder on surface
In, it is followed successively by each section of heating temperature of discharge port in feed inlet：It is melted at 235 DEG C, 250 DEG C, 260 DEG C, 260 DEG C, 260 DEG C, 240 DEG C
Melt blending extrusion, pellet is cut by comminutor after being cooled by water, injection molding obtains carbon fiber reinforced polyamide composite material
(PA6/CF).The LOI of the composite material is that 24%, UL-94 is stepless；Bending strength is 297.5MPa, and bending modulus is
21.3GPa, impact strength 8.3kJ/m2。
Comparative example 3
First there is no 50 parts of 100 parts of the carbon fiber of flame retardant coating and makrolon to be respectively put into double screw extruder on surface
In, it is followed successively by each section of heating temperature of discharge port in feed inlet：It is melted at 220 DEG C, 250 DEG C, 260 DEG C, 265 DEG C, 275 DEG C, 250 DEG C
Melt blending extrusion, pellet is cut by comminutor after being cooled by water, injection molding obtains fibre reinforced makrolon composite wood
Expect (PC/CF).The LOI of the composite material is that 26%, UL-94 is stepless；Tensile strength is 173.4MPa, and bending strength is
258.3MPa, bending modulus 18.6GP.
Comparative example 4
At 120 DEG C, impregnated with pre- mixed epoxy mixture (epoxy resin E-51 and 4,4- diaminodiphenylsulfone DDS)
Surface does not have 21 parts of the carbon cloth of flame retardant coating, is transferred them in mold after carbon fiber is sufficiently impregnated, and at 90 DEG C
Vacuum drying oven in bubble removing 30-40min, then by mold be transferred to vulcanizing press solidification, obtain not flame-retardant modified
Carbon fiber epoxy (EP/CF) composite material.Composite L OI is that 31%, UL-94 is stepless；Bending strength is
977.2MPa, bending modulus 51.4GP, impact strength 123.2kJ/m2。
Application examples 1
First using the method described in embodiment 2 to prepare surface has carbon fiber simultaneously repetitive operation 4 times of flame retardant coating, uses
Method described in comparative example 1 prepares fibre reinforced flame-retardant polypropylene composite material.The LOI of gained PP/CF composite materials is
25%, UL-94 are V-2 grades；Tensile strength is 183.7MPa, stretch modulus 7.5GPa, impact strength 5.4kJ/m2。
Application examples 2
First using the method described in embodiment 2 to prepare surface has carbon fiber simultaneously repetitive operation 5 times of flame retardant coating, uses
Method described in comparative example 2 prepares fibre reinforced Flameproof polyamide PA6 composite materials.The LOI of gained PA6/CF composite materials
It it is V-1 grades for 27%, UL-94；Bending strength is 291.3MPa, bending modulus 21.5GPa, impact strength 7.4kJ/m2。
Application examples 3
First using the method described in embodiment 2 to prepare surface has carbon fiber simultaneously repetitive operation 6 times of flame retardant coating, uses
Method described in comparative example 3 prepares fibre reinforced fire-retardant polycarbonate composite material.The LOI of gained PC/CF composite materials is
32%, UL-94 are V-0 grades；Tensile strength is 167.7MPa, bending strength 253.9MPa, bending modulus 18.1GPa.
Application examples 4
First using the method described in embodiment 2 to prepare surface has carbon fiber simultaneously repetitive operation 2 times of flame retardant coating, uses
Method described in comparative example 4 prepares fibre reinforced fire-retarding epoxy resin composite material.The LOI of gained EP/CF composite materials is
45%, UL-94 are V-0 grades；Bending strength is 983.5MPa, bending modulus 52.1GP；Impact strength 164.7kJ/m2。
Application examples 5
First using the method described in embodiment 20 to prepare surface has carbon fiber simultaneously repetitive operation 7 times of flame retardant coating, adopts
The method described in comparative example 1 prepares fibre reinforced flame-retardant polypropylene composite material.The LOI of gained PP/CF composite materials is
26%, UL-94 are V-1 grades；Tensile strength is 179.2MPa, stretch modulus 7.1GPa, impact strength 5.9kJ/m2。
Application examples 6
First using the method described in embodiment 20 to prepare surface has carbon fiber simultaneously repetitive operation 4 times of flame retardant coating, adopts
The method described in comparative example 2 prepares fibre reinforced Flameproof polyamide PA6 composite materials.Gained PA6/CF composite materials
LOI is that 27%, UL-94 is V-1 grades；Bending strength is 290.6MPa, bending modulus 20.5GPa, impact strength 8.1kJ/
m2。
Application examples 7
First using the method described in embodiment 20 to prepare surface has carbon fiber simultaneously repetitive operation 5 times of flame retardant coating, adopts
The method described in comparative example 3 prepares fibre reinforced fire-retardant polycarbonate composite material.The LOI of gained PC/CF composite materials
It it is V-1 grades for 31%, UL-94；Tensile strength is 169.3MPa, bending strength 256.6MPa, bending modulus 18.2GPa.
Application examples 8
First using the method described in embodiment 20 to prepare surface has carbon fiber simultaneously repetitive operation 2 times of flame retardant coating, adopts
The method described in comparative example 4 prepares fibre reinforced fire-retarding epoxy resin composite material.The LOI of gained EP/CF composite materials
It it is V-0 grades for 43%, UL-94；Bending strength is 965.3MPa, bending modulus 51.7GP；Impact strength 144.8kJ/m2。
Application examples 9
First using the method described in embodiment 22 to prepare surface has carbon fiber simultaneously repetitive operation 5 times of flame retardant coating, adopts
The method described in comparative example 1 prepares fibre reinforced flame-retardant polypropylene composite material.The LOI of gained PP/CF composite materials is
24%, UL-94 are V-2 grades；Tensile strength is 181.6MPa, stretch modulus 7.3GPa, impact strength 5.5kJ/m2。
Application examples 10
First using the method described in embodiment 22 to prepare surface has carbon fiber simultaneously repetitive operation 9 times of flame retardant coating, adopts
The method described in comparative example 2 prepares fibre reinforced Flameproof polyamide PA6 composite materials.Gained PA6/CF composite materials
LOI is that 29%, UL-94 is V-0 grades；Bending strength is 282.4MPa, bending modulus 20.1GPa, impact strength 8.8kJ/
m2。
Application examples 11
First using the method described in embodiment 22 to prepare surface has carbon fiber simultaneously repetitive operation 7 times of flame retardant coating, adopts
The method described in comparative example 3 prepares fibre reinforced fire-retardant polycarbonate composite material.The LOI of gained PC/CF composite materials
It it is V-0 grades for 33%, UL-94；Tensile strength is 171.8MPa, bending strength 259.5MPa, bending modulus 18.3GPa.
Application examples 12
First using the method described in embodiment 22 to prepare surface has carbon fiber simultaneously repetitive operation 2 times of flame retardant coating, adopts
The method described in comparative example 4 prepares fibre reinforced fire-retarding epoxy resin composite material.The LOI of gained EP/CF composite materials
It it is V-0 grades for 40%, UL-94；Bending strength is 948.6MPa, bending modulus 52.3GP；Impact strength 153.5kJ/m2。
Application examples 13
First using the method described in embodiment 30 to prepare surface has carbon fiber simultaneously repetitive operation 7 times of flame retardant coating, adopts
The method described in comparative example 1 prepares fibre reinforced flame-retardant polypropylene composite material.The LOI of gained PP/CF composite materials is
27%, UL-94 are V-1 grades；Tensile strength is 185.7MPa, stretch modulus 7.4GPa, impact strength 5.2kJ/m2。
Application examples 14
First using the method described in embodiment 308 to prepare surface has carbon fiber simultaneously repetitive operation 7 times of flame retardant coating, adopts
The method described in comparative example 2 prepares fibre reinforced Flameproof polyamide PA6 composite materials.Gained PA6/CF composite materials
LOI is that 28%, UL-94 is V-0 grades；Bending strength is 281.5MPa, bending modulus 20.4GPa, impact strength 9.1kJ/
m2。
Application examples 15
First using the method described in embodiment 30 to prepare surface has carbon fiber simultaneously repetitive operation 3 times of flame retardant coating, adopts
The method described in comparative example 3 prepares fibre reinforced fire-retardant polycarbonate composite material.The LOI of gained PC/CF composite materials
It it is V-2 grades for 28%, UL-94；Tensile strength is 169.4MPa, bending strength 257.2MPa, bending modulus 17.9GPa.
Application examples 16
First using the method described in embodiment 30 to prepare surface has carbon fiber simultaneously repetitive operation 2 times of flame retardant coating, adopts
The method described in comparative example 4 prepares fibre reinforced fire-retarding epoxy resin composite material.The LOI of gained EP/CF composite materials
It it is V-0 grades for 41%, UL-94；Bending strength is 954.8MPa, bending modulus 51.6GP；Impact strength 148.3kJ/m2。
From the test result of use above example can be seen that surface with flame retardant coating carbon fibre composite PP/CF,
The flame retardant property of PA6/CF, PC/CF and EP/CF are greatly improved, while also maintaining the mechanical performance of composite material.
Claims (10)
1. a kind of surface has the carbon fiber of flame retardant coating, it is characterised in that：Including carbon fiber and its compound of surface covering
Flame retardant coating, the compound flame retardant coating contain the substance of two class oppositely chargeds.
2. a kind of surface as described in claim 1 has the carbon fiber of flame retardant coating, it is characterised in that：The two class band phases
The substance of counter charges includes electrolyte and/or function nano particle.
3. a kind of surface as claimed in claim 2 has the carbon fiber of flame retardant coating, it is characterised in that：The two class band phases
A substance in the substance of counter charges is one or more solution in cationic polyelectrolyte, function nano particle 1；It is another
Substance is one or more solution in anion electrolyte, function nano particle 2.
4. a kind of surface as claimed in claim 3 has the carbon fiber of flame retardant coating, it is characterised in that：The cation electrodeposition
Solution matter is chitosan, poly-L-arginine hydrochloride, polylysine, poly-dopamine, polyallylamine hydrochloride, poly dimethyl dipropyl
Alkenyl ammonium chloride, polyethyleneimine, silane coupling agent, polyacrylamide, polyallylamine hydrochloride, polyvinyl alcohol, the work(
Energy nano-particle 1 is functionalization graphene, aminated carbon nano tube, carbon nano-fiber, nano-titanium dioxide, nanometer titanium dioxide
Silicon.
5. a kind of surface as described in claim 3 or 4 has the carbon fiber of flame retardant coating, it is characterised in that：It is described it is cloudy from
Sub- electrolyte is sodium alginate, tannic acid, hyaluronic acid, glutamic acid, DNA, gelatin, cyclodextrin, phytic acid, function
Cellulose, kayexalate, polyvinylsulfonic acid, polyacrylic acid, polyphosphate, melamine phosphate, function are received
Rice corpuscles 2 is stratiform double-layered hydroxides, carboxylic carbon nano-tube, phyllosilicate, nano-aluminium oxide.
6. there is the preparation method of the carbon fiber of flame retardant coating, feature to exist on a kind of surface according to any one of claims 1 to 5
In including the following steps：Carbon fiber is immersed in the mixed solution of the substance of the certain density two class oppositely chargeds
In, it is fully dipped to carbon fiber surface and forms at least one layer of compound flame retardant coating, obtain a kind of surface with compound
The carbon fiber of object flame retardant coating.
7. a kind of surface as claimed in claim 6 has the preparation method of the carbon fiber of flame retardant coating, it is characterised in that：Two classes
The pH value of the aqueous solution of substance is 3-11.
8. a kind of surface as claimed in claim 7 has the preparation method of the carbon fiber of flame retardant coating, it is characterised in that：It can lead to
Cross time that the concentration of the adjustment electrolyte and/or function nano particle, the number of its aqueous solution and the method repeat
Number, is prepared the carbon fiber of carbon fiber surface different composite object flame retardant coating content and pattern.
9. a kind of surface as claimed in claims 6 or 7 has the preparation method of the carbon fiber of flame retardant coating, which is characterized in that
Include the following steps：
（1）Under room temperature, the aqueous solution of the substance for the two classes oppositely charged that mass concentration is 0.1-10% is respectively configured；
（2）Carbon fiber is immersed in step（1）In the mixed solution of the two kinds of substances prepared, the aqueous solution of wherein each substance is equal
It is 50-300 parts；
（3）Carbon fiber is impregnated into 5-60min in the mixed solution of two substances；
（4）It is taken out after carbon fiber surface forms at least one layer of compound flame retardant coating, obtaining a kind of surface has resistance
Fire the carbon fiber of coating.
10. the surface as described in claim 1-9 is any has the application of the carbon fiber of flame retardant coating, it is characterised in that：The carbon
Fiber can be used as the reinforcing material and fire proofing of high molecular polymer.
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