CN105602000B - A kind of preparation method of titania modified carbon fiber enhancement resin base composite material - Google Patents

A kind of preparation method of titania modified carbon fiber enhancement resin base composite material Download PDF

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CN105602000B
CN105602000B CN201610077211.4A CN201610077211A CN105602000B CN 105602000 B CN105602000 B CN 105602000B CN 201610077211 A CN201610077211 A CN 201610077211A CN 105602000 B CN105602000 B CN 105602000B
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carbon fiber
modified carbon
mixed solution
titania modified
composite material
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CN105602000A (en
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费杰
张超
黄剑锋
曹丽云
罗丹
欧阳海波
段笑
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
    • C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
    • C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
    • 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
    • C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
    • C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
    • C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
    • 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
    • C08J2497/00—Characterised by the use of lignin-containing materials
    • C08J2497/02—Lignocellulosic material, e.g. wood, straw or bagasse
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/16—Fibres; Fibrils

Abstract

The invention discloses a kind of preparation method of titania modified carbon fiber enhancement resin base composite material, first carbon fiber is pre-processed with concentrated nitric acid under certain condition, by pretreated carbon fiber and titanium source hydro-thermal reaction certain time in using concentrated hydrochloric acid as the aqueous solution of acid medium, modified fibre is fully washed after the completion of reaction, drying, reinforced resin based composites are prepared using modified carbon fiber as reinforcing fiber.Modified carbon fiber reinforced resin based composites tensile strength prepared by the present invention improves 134.8%~153.1%, porosity is reduced to 19.3%~15.6% from 45.7%~40.5%, and pore-size distribution is more uniform, and reinforced resin based composites coefficient of friction is maintained at 0.12~0.14, wear extent reduces by 37.1%~50.3%, has fully demonstrated modified carbon fiber applied to anti-attrition effect excellent in Wet-type friction material.

Description

A kind of preparation method of titania modified carbon fiber enhancement resin base composite material
Technical field
The invention belongs to Wet-type friction material field, and in particular to a kind of titania modified carbon fiber enhancement resin base is answered The preparation method of condensation material.
Background technology
Carbon fiber enhancement resin base composite material is because of its high specific strength and specific modulus, antifatigue, corrosion-resistant, designability is strong It is widely used in Deng excellent properties in engineering material.But carbon fiber surface inertia is big, do not possess abundant netted branch Structure, it is not ideal enough with the interface cohesion of resin in the poor-performing in machine direction, tree is limited to a certain extent Application of the resin-based composite in harsh environment and special dimension.Therefore, physically or chemically changing for appropriateness is carried out to carbon fiber Property processing, to promote its bond strength with resin matrix, further expand its application field.
A kind of Application No. CN201310552131.6 Chinese patent " carbon fiber surface treatment method " is proposed one In the environment of individual atmospheric pressure, using nitrogen as surface treatment of carbon fibers medium, low temperature plasma is produced, to the carbon in motion Fibre bundle surface carries out Ions Bombardment, and then the method being modified to fiber.This method makes the active pole of carbon fiber surface Property functional group content increase, the groove of carbon fiber surface deepens, specific surface area increase, improves the interlayer shear of its composite Intensity.But the method that the patent proposes requires higher to experiment condition, is not suitable with industrialized production.
A kind of Application No. CN201310083719.1 Chinese patent " particle activeness and quietness resin base fibrous composite Preparation method " propose a kind of preparation method using particle activeness and quietness mechanics of fibre composites performance.Characterized in that, The parts by weight of solid particle 5~30 that particle diameter is 10~50 μm are added in the parts by weight of matrix resin 100, after being well mixed, then are entered Row vacuum imports and particle/fibre reinforced composites is made.The present invention can utilize particle to make fibre reinforced composites intensity 10%~35% is improved with mechanical properties such as toughness.The defects of this method is that particle and fiber are mixed into nothing by mechanical means Method ensures both uniformities, and both synergies do not fully demonstrate, and enhancing effect is not obvious enough.
The content of the invention
It is an object of the invention to provide a kind of preparation side of titania modified carbon fiber enhancement resin base composite material Method, the defects of to overcome above-mentioned prior art to exist, the present invention is using the carbon fiber after titania modified as reinforcement, preparation Go out coefficient of friction height, the low reinforced resin based composites of wear extent.
To reach above-mentioned purpose, the present invention adopts the following technical scheme that：
A kind of preparation method of titania modified carbon fiber enhancement resin base composite material, comprises the following steps：
Step 1：In terms of mass fraction, 20~30 parts of deionized waters are taken, concentrated hydrochloric acid is added thereto and obtains acid solution, Then 1~3 part of butyl titanate is added in acid solution and obtains mixed solution A, 0.05~0.2 part is pre-processed through concentrated nitric acid Carbon fiber afterwards adds in mixed solution A and obtains mixed solution B；
Step 2：Homogeneous hydro-thermal reaction, natural cooling after the completion of reaction are being occurred into homogeneous hydrothermograph for mixed solution B To room temperature, dried after obtained carbon fiber is washed with deionized water or ethanol, that is, obtain titania modified carbon fiber；
Step 3：By titania modified carbon fiber, bamboo fibre and Fanglun slurry cake according to 3:1:1 mass ratio is scattered in water In, fiber preform and naturally dry then is made using Vacuum filtration device, the fiber preform after drying is using modification Resin impregnating, it is hot-forming after naturally dry again, titania modified carbon fiber enhancement resin base composite material is made.
Further, concentrated hydrochloric acid is added in step 1 into deionized water to pH=-0.4~3.
Further, the method for concentrated nitric acid pretreatment carbon fiber is in step 1：By carbon fiber under the conditions of 80 DEG C of oil baths 6h is pre-processed using concentrated nitric acid condensing reflux.
Further, the temperature of homogeneous hydro-thermal reaction is 100 DEG C~200 DEG C in step 2, and the time is 5~24h.
Further, the phenol-formaldehyde resin modified used in step 3 is nbr modified phenolic resins.
Further, the temperature of hot pressing is 170 DEG C in step 3, pressure 5MPa.
A kind of preparation method of titania modified carbon fiber enhancement resin base composite material, comprises the following steps：
Step 1：In terms of mass fraction, 25 parts of deionized waters are taken, addition concentrated hydrochloric acid to pH=2 obtains acid molten thereto Liquid, then 2 parts of butyl titanates are added in acid solution and obtain mixed solution A, by 0.1 part through the pretreated carbon of concentrated nitric acid Fiber adds in mixed solution A and obtains mixed solution B, wherein, the method for concentrated nitric acid pretreatment carbon fiber is：By carbon fiber 80 Using concentrated nitric acid condensing reflux pretreatment 6h under the conditions of DEG C oil bath；
Step 2：Mixed solution B is transferred to water heating kettle liner and water heating kettle is installed in homogeneous hydrothermograph, at 150 DEG C At a temperature of homogeneous hydro-thermal reaction 6h, naturally cool to room temperature after the completion of reaction, the carbon fiber deionized water or ethanol that will be obtained Dried after washing, that is, obtain titania modified carbon fiber；
Step 3：By titania modified carbon fiber, bamboo fibre and Fanglun slurry cake according to 3:1:1 mass ratio is scattered in water In, fiber preform and naturally dry then is made using Vacuum filtration device, the fiber preform after drying is used into butyronitrile Phenol-formaldehyde resin modified impregnates, and uses vulcanizer after naturally dry again at a temperature of 170 DEG C, hot-forming under 5MPa pressure, system Obtain titania modified carbon fiber enhancement resin base composite material.
Compared with prior art, the present invention has technique effect beneficial below：
The present invention is grafted titanium dioxide as titanium source using butyl titanate in carbon fiber surface, to warp under thermal and hydric environment The pretreated carbon fiber of concentrated nitric acid is reprocessed, and enhancing is used as by the use of the titania modified carbon fiber that reprocessing obtains Body, polymer matrix composites are prepared with bamboo fibre and Fanglun slurry cake, carbon dioxide modified carbon fiber of the invention, maintain carbon fibre Excellent mechanical strength is tieed up, adds its surface roughness and specific surface area, is allowed to be combined more abundant, reinforcement with resin matrix Both mechanical bond performances, effectively improve the combination degree of composite, so as to greatly improve titania modified carbon The machinery and tribological property of fiber-reinforced resin matrix compound material.Titania modified fibre reinforced tree prepared by the present invention Resin-based composite, its tensile strength improve 134.8%~153.1%, and porosity is reduced to from 45.7%~40.5% 19.3%~15.6%, and pore-size distribution is more uniform, while its coefficient of friction is maintained at 0.12~0.14, wear extent reduces 37.1%~50.3%, embody excellent frictional behaviour.
Brief description of the drawings
Fig. 1 is titania modified carbon fiber SEM photograph prepared by the present invention, and wherein a, b, c, d, e, f are respectively to implement Carbon dioxide modified carbon fiber prepared by example 2,5,6,7,8,9；
Fig. 2 is that the present invention prepares titania modified carbon fiber XRD analysis, wherein a, b, and c is respectively that embodiment 2,5,6 is made Standby carbon dioxide modified carbon fiber；
Fig. 3 is that the present invention prepares titania modified carbon fiber XRD analysis, wherein d, e, and f is respectively that embodiment 7,8,9 is made Standby carbon dioxide modified carbon fiber；
Fig. 4 is the continuous braking comparison diagram that the present invention prepares titania modified carbon fiber enhancement resin base composite material, Wherein a, b, c, d, e are respectively original carbon fiber, pre-process carbon fiber and embodiment 2, titania modified prepared by 5,6 Carbon fiber enhancement resin base composite material；
Fig. 5 is that the present invention prepares titania modified carbon fiber enhancement resin base composite material average friction coefficient contrast Figure, wherein C0, C1, C2, C3, C4 is respectively original carbon fiber, pre-processes carbon fiber and embodiment 2, modified fine prepared by 5,6 Dimension enhancing friction material；
Fig. 6 is that the present invention prepares titania modified carbon fiber enhancement resin base composite material wear extent comparison diagram, wherein C0, C1, C2, C3, C4 are respectively original carbon fiber, pre-process carbon fiber and embodiment 2, and modified fibre prepared by 5,6 strengthens Friction material.
Embodiment
Embodiments of the present invention are described in further detail below：
A kind of preparation method of titania modified carbon fiber enhancement resin base composite material, comprises the following steps：
Step 1：In terms of mass fraction, 20~30 parts of deionized waters are taken, concentrated hydrochloric acid is added dropwise thereto, and (concentration is Acid solution 12mol/L) is obtained to pH=-0.4~3, then 1~3 part of butyl titanate is added in acid solution and mixed Solution A is closed, 0.05~0.2 part is added in mixed solution A through the pretreated carbon fiber of concentrated nitric acid and obtains mixed solution B, its In, the method for concentrated nitric acid pretreatment carbon fiber is：Carbon fiber is used under the conditions of 80 DEG C of oil baths (silicone oil) concentrated nitric acid (concentration for 16mol/L) condensing reflux pretreatment 6h；
Step 2：Mixed solution B is transferred to water heating kettle liner and water heating kettle is installed in homogeneous hydrothermograph, at 100 DEG C Homogeneous 5~24h of hydro-thermal reaction, room temperature is naturally cooled to after the completion of reaction at a temperature of~200 DEG C, by obtained carbon fiber spend from Dried after sub- water or ethanol washing, that is, obtain titania modified carbon fiber；
Step 3：By titania modified carbon fiber, bamboo fibre and Fanglun slurry cake according to 3:1:1 mass ratio is scattered in water In, fiber preform and naturally dry then is made using Vacuum filtration device, the fiber preform after drying is used into butyronitrile Phenol-formaldehyde resin modified impregnates, and uses vulcanizer after naturally dry again at a temperature of 170 DEG C, hot-forming under 5MPa pressure, system Obtain titania modified carbon fiber enhancement resin base composite material.
The present invention is described in further detail with reference to embodiment：
Embodiment 1
Step 1：In terms of mass fraction, 30 parts of deionized waters are taken, addition concentrated hydrochloric acid to pH=1 obtains acid molten thereto Liquid, then 1 part of butyl titanate is added in acid solution and obtains mixed solution A, by 0.1 part through the pretreated carbon of concentrated nitric acid Fiber adds in mixed solution A and obtains mixed solution B, wherein, the method for concentrated nitric acid pretreatment carbon fiber is：By carbon fiber 80 Using concentrated nitric acid condensing reflux pretreatment 6h under the conditions of DEG C oil bath (silicone oil)；
Step 2：Mixed solution B is transferred to water heating kettle liner and water heating kettle is installed in homogeneous hydrothermograph, at 110 DEG C At a temperature of homogeneous hydro-thermal reaction 5h, naturally cool to room temperature after the completion of reaction, the carbon fiber deionized water or ethanol that will be obtained Dried after washing, that is, obtain titania modified carbon fiber；
Step 3：By titania modified carbon fiber, bamboo fibre and Fanglun slurry cake according to 3:1:1 mass ratio is scattered in water In, fiber preform and naturally dry then is made using Vacuum filtration device, the fiber preform after drying is used into butyronitrile Phenol-formaldehyde resin modified impregnates, and uses vulcanizer after naturally dry again at a temperature of 170 DEG C, hot-forming under 5MPa pressure, system Obtain titania modified carbon fiber enhancement resin base composite material.
Embodiment 2
Step 1：In terms of mass fraction, 25 parts of deionized waters are taken, addition concentrated hydrochloric acid to pH=2 obtains acid molten thereto Liquid, then 2 parts of butyl titanates are added in acid solution and obtain mixed solution A, by 0.1 part through the pretreated carbon of concentrated nitric acid Fiber adds in mixed solution A and obtains mixed solution B, wherein, the method for concentrated nitric acid pretreatment carbon fiber is：By carbon fiber 80 Using concentrated nitric acid condensing reflux pretreatment 6h under the conditions of DEG C oil bath (silicone oil)；
Step 2：Mixed solution B is transferred to water heating kettle liner and water heating kettle is installed in homogeneous hydrothermograph, at 150 DEG C At a temperature of homogeneous hydro-thermal reaction 6h, naturally cool to room temperature after the completion of reaction, the carbon fiber deionized water or ethanol that will be obtained Dried after washing, that is, obtain titania modified carbon fiber；
Step 3：By titania modified carbon fiber, bamboo fibre and Fanglun slurry cake according to 3:1:1 mass ratio is scattered in water In, fiber preform and naturally dry then is made using Vacuum filtration device, the fiber preform after drying is used into butyronitrile Phenol-formaldehyde resin modified impregnates, and uses vulcanizer after naturally dry again at a temperature of 170 DEG C, hot-forming under 5MPa pressure, system Obtain titania modified carbon fiber enhancement resin base composite material.
Embodiment 3
Step 1：In terms of mass fraction, 20 parts of deionized waters are taken, addition concentrated hydrochloric acid to pH=3 obtains acid molten thereto Liquid, then 3 parts of butyl titanates are added in acid solution and obtain mixed solution A, by 0.1 part through the pretreated carbon of concentrated nitric acid Fiber adds in mixed solution A and obtains mixed solution B, wherein, the method for concentrated nitric acid pretreatment carbon fiber is：By carbon fiber 80 Using concentrated nitric acid condensing reflux pretreatment 6h under the conditions of DEG C oil bath (silicone oil)；
Step 2：Mixed solution B is transferred to water heating kettle liner and water heating kettle is installed in homogeneous hydrothermograph, at 150 DEG C At a temperature of homogeneous hydro-thermal reaction 6h, naturally cool to room temperature after the completion of reaction, the carbon fiber deionized water or ethanol that will be obtained Dried after washing, that is, obtain titania modified carbon fiber；
Step 3：By titania modified carbon fiber, bamboo fibre and Fanglun slurry cake according to 3:1:1 mass ratio is scattered in water In, fiber preform and naturally dry then is made using Vacuum filtration device, the fiber preform after drying is used into butyronitrile Phenol-formaldehyde resin modified impregnates, and uses vulcanizer after naturally dry again at a temperature of 170 DEG C, hot-forming under 5MPa pressure, system Obtain titania modified carbon fiber enhancement resin base composite material.
Embodiment 4
Step 1：In terms of mass fraction, 30 parts of deionized waters are taken, addition concentrated hydrochloric acid to pH=2 obtains acid molten thereto Liquid, then 2 parts of butyl titanates are added in acid solution and obtain mixed solution A, it is pretreated through concentrated nitric acid by 0.05 part Carbon fiber adds in mixed solution A and obtains mixed solution B, wherein, the method for concentrated nitric acid pretreatment carbon fiber is：Carbon fiber is existed Using concentrated nitric acid condensing reflux pretreatment 6h under the conditions of 80 DEG C of oil baths (silicone oil)；
Step 2：Mixed solution B is transferred to water heating kettle liner and water heating kettle is installed in homogeneous hydrothermograph, at 150 DEG C At a temperature of homogeneous hydro-thermal reaction 6h, naturally cool to room temperature after the completion of reaction, the carbon fiber deionized water or ethanol that will be obtained Dried after washing, that is, obtain titania modified carbon fiber；
Step 3：By titania modified carbon fiber, bamboo fibre and Fanglun slurry cake according to 3:1:1 mass ratio is scattered in water In, fiber preform and naturally dry then is made using Vacuum filtration device, the fiber preform after drying is used into butyronitrile Phenol-formaldehyde resin modified impregnates, and uses vulcanizer after naturally dry again at a temperature of 170 DEG C, hot-forming under 5MPa pressure, system Obtain titania modified carbon fiber enhancement resin base composite material.
Embodiment 5
Step 1：In terms of mass fraction, 30 parts of deionized waters are taken, addition concentrated hydrochloric acid to pH=2 obtains acid molten thereto Liquid, then 3 parts of butyl titanates are added in acid solution and obtain mixed solution A, by 0.1 part through the pretreated carbon of concentrated nitric acid Fiber adds in mixed solution A and obtains mixed solution B, wherein, the method for concentrated nitric acid pretreatment carbon fiber is：By carbon fiber 80 Using concentrated nitric acid condensing reflux pretreatment 6h under the conditions of DEG C oil bath (silicone oil)；
Step 2：Mixed solution B is transferred to water heating kettle liner and water heating kettle is installed in homogeneous hydrothermograph, at 140 DEG C At a temperature of homogeneous hydro-thermal reaction 12h, naturally cool to room temperature after the completion of reaction, the carbon fiber deionized water or ethanol that will be obtained Dried after washing, that is, obtain titania modified carbon fiber；
Step 3：By titania modified carbon fiber, bamboo fibre and Fanglun slurry cake according to 3:1:1 mass ratio is scattered in water In, fiber preform and naturally dry then is made using Vacuum filtration device, the fiber preform after drying is used into butyronitrile Phenol-formaldehyde resin modified impregnates, and uses vulcanizer after naturally dry again at a temperature of 170 DEG C, hot-forming under 5MPa pressure, system Obtain titania modified carbon fiber enhancement resin base composite material.
Embodiment 6
Step 1：In terms of mass fraction, 30 parts of deionized waters are taken, addition concentrated hydrochloric acid to pH=2 obtains acid molten thereto Liquid, then 3 parts of butyl titanates are added in acid solution and obtain mixed solution A, by 0.1 part through the pretreated carbon of concentrated nitric acid Fiber adds in mixed solution A and obtains mixed solution B, wherein, the method for concentrated nitric acid pretreatment carbon fiber is：By carbon fiber 80 Using concentrated nitric acid condensing reflux pretreatment 6h under the conditions of DEG C oil bath (silicone oil)；
Step 2：Mixed solution B is transferred to water heating kettle liner and water heating kettle is installed in homogeneous hydrothermograph, at 140 DEG C At a temperature of homogeneous hydro-thermal reaction 24h, naturally cool to room temperature after the completion of reaction, the carbon fiber deionized water or ethanol that will be obtained Dried after washing, that is, obtain titania modified carbon fiber；
Step 3：By titania modified carbon fiber, bamboo fibre and Fanglun slurry cake according to 3:1:1 mass ratio is scattered in water In, fiber preform and naturally dry then is made using Vacuum filtration device, the fiber preform after drying is used into butyronitrile Phenol-formaldehyde resin modified impregnates, and uses vulcanizer after naturally dry again at a temperature of 170 DEG C, hot-forming under 5MPa pressure, system Obtain titania modified carbon fiber enhancement resin base composite material.
Embodiment 7
Step 1：In terms of mass fraction, 30 parts of deionized waters are taken, addition concentrated hydrochloric acid to pH=-0.4 obtains acidity thereto Solution, then 2 parts of butyl titanates are added in acid solution and obtain mixed solution A, it is pretreated through concentrated nitric acid by 0.2 part Carbon fiber adds in mixed solution A and obtains mixed solution B, wherein, the method for concentrated nitric acid pretreatment carbon fiber is：Carbon fiber is existed Using concentrated nitric acid condensing reflux pretreatment 6h under the conditions of 80 DEG C of oil baths (silicone oil)；
Step 2：Mixed solution B is transferred to water heating kettle liner and water heating kettle is installed in homogeneous hydrothermograph, at 100 DEG C At a temperature of homogeneous hydro-thermal reaction 6h, naturally cool to room temperature after the completion of reaction, the carbon fiber deionized water or ethanol that will be obtained Dried after washing, that is, obtain titania modified carbon fiber；
Step 3：By titania modified carbon fiber, bamboo fibre and Fanglun slurry cake according to 3:1:1 mass ratio is scattered in water In, fiber preform and naturally dry then is made using Vacuum filtration device, the fiber preform after drying is used into butyronitrile Phenol-formaldehyde resin modified impregnates, and uses vulcanizer after naturally dry again at a temperature of 170 DEG C, hot-forming under 5MPa pressure, system Obtain titania modified carbon fiber enhancement resin base composite material.
Embodiment 8
Step 1：In terms of mass fraction, 30 parts of deionized waters are taken, addition concentrated hydrochloric acid to pH=-0.38 obtains acid thereto Property solution, then 2 parts of butyl titanates are added in acid solutions and obtain mixed solution A, by 0.1 part after concentrated nitric acid pre-processes Carbon fiber add mixed solution A in obtain mixed solution B, wherein, concentrated nitric acid pretreatment carbon fiber method be：By carbon fiber Using concentrated nitric acid condensing reflux pretreatment 6h under the conditions of 80 DEG C of oil baths (silicone oil)；
Step 2：Mixed solution B is transferred to water heating kettle liner and water heating kettle is installed in homogeneous hydrothermograph, at 150 DEG C At a temperature of homogeneous hydro-thermal reaction 6h, naturally cool to room temperature after the completion of reaction, the carbon fiber deionized water or ethanol that will be obtained Dried after washing, that is, obtain titania modified carbon fiber；
Step 3：By titania modified carbon fiber, bamboo fibre and Fanglun slurry cake according to 3:1:1 mass ratio is scattered in water In, fiber preform and naturally dry then is made using Vacuum filtration device, the fiber preform after drying is used into butyronitrile Phenol-formaldehyde resin modified impregnates, and uses vulcanizer after naturally dry again at a temperature of 170 DEG C, hot-forming under 5MPa pressure, system Obtain titania modified carbon fiber enhancement resin base composite material.
Embodiment 9
Step 1：In terms of mass fraction, 30 parts of deionized waters are taken, addition concentrated hydrochloric acid to pH=-0.38 obtains acid thereto Property solution, then 2 parts of butyl titanates are added in acid solutions and obtain mixed solution A, by 0.1 part after concentrated nitric acid pre-processes Carbon fiber add mixed solution A in obtain mixed solution B, wherein, concentrated nitric acid pretreatment carbon fiber method be：By carbon fiber Using concentrated nitric acid condensing reflux pretreatment 6h under the conditions of 80 DEG C of oil baths (silicone oil)；
Step 2：Mixed solution B is transferred to water heating kettle liner and water heating kettle is installed in homogeneous hydrothermograph, at 200 DEG C At a temperature of homogeneous hydro-thermal reaction 6h, naturally cool to room temperature after the completion of reaction, the carbon fiber deionized water or ethanol that will be obtained Dried after washing, that is, obtain titania modified carbon fiber；
Step 3：By titania modified carbon fiber, bamboo fibre and Fanglun slurry cake according to 3:1:1 mass ratio is scattered in water In, fiber preform and naturally dry then is made using Vacuum filtration device, the fiber preform after drying is used into butyronitrile Phenol-formaldehyde resin modified impregnates, and uses vulcanizer after naturally dry again at a temperature of 170 DEG C, hot-forming under 5MPa pressure, system Obtain titania modified carbon fiber enhancement resin base composite material.

Claims (5)

1. a kind of preparation method of titania modified carbon fiber enhancement resin base composite material, it is characterised in that including following Step：
Step 1：In terms of mass fraction, 20~30 parts of deionized waters are taken, concentrated hydrochloric acid is added thereto and obtains pH=-0.4~3 Acid solution, then 1~3 part of butyl titanate is added in acid solution and obtains mixed solution A, by 0.05~0.2 part through dense Carbon fiber after nitric acid pretreatment, which is added in mixed solution A, obtains mixed solution B；
Step 2：It is homogeneous hydro-thermal reaction, the temperature of homogeneous hydro-thermal reaction occur in homogeneous hydrothermograph by mixed solution B 100 DEG C~200 DEG C, the time is 5~24h, and room temperature is naturally cooled to after the completion of reaction, by obtained carbon fiber deionized water or Dried after ethanol washing, that is, obtain titania modified carbon fiber；
Step 3：By titania modified carbon fiber, bamboo fibre and Fanglun slurry cake according to 3:1:1 mass ratio is dispersed in water, Then fiber preform and naturally dry is made using Vacuum filtration device, the fiber preform after drying is used into modified phenolic Resin impregnates, hot-forming after naturally dry again, and titania modified carbon fiber enhancement resin base composite material is made.
2. a kind of preparation method of titania modified carbon fiber enhancement resin base composite material according to claim 1, Characterized in that, the method for concentrated nitric acid pretreatment carbon fiber is in step 1：By carbon fiber under the conditions of 80 DEG C of oil baths using dense Nitric acid condensing reflux pre-processes 6h.
3. a kind of preparation method of titania modified carbon fiber enhancement resin base composite material according to claim 1, Characterized in that, the phenol-formaldehyde resin modified used in step 3 is nbr modified phenolic resins.
4. a kind of preparation method of titania modified carbon fiber enhancement resin base composite material according to claim 1, Characterized in that, the temperature of hot pressing is 170 DEG C in step 3, pressure 5MPa.
5. a kind of preparation method of titania modified carbon fiber enhancement resin base composite material, it is characterised in that including following Step：
Step 1：In terms of mass fraction, 25 parts of deionized waters are taken, addition concentrated hydrochloric acid to pH=2 obtains acid solution thereto, so 2 parts of butyl titanates are added in acid solution afterwards and obtain mixed solution A, by 0.1 part through the pretreated carbon fiber of concentrated nitric acid Add in mixed solution A and obtain mixed solution B, wherein, the method for concentrated nitric acid pretreatment carbon fiber is：By carbon fiber in 80 DEG C of oil Using concentrated nitric acid condensing reflux pretreatment 6h under the conditions of bath；
Step 2：Mixed solution B is transferred to water heating kettle liner and water heating kettle is installed in homogeneous hydrothermograph, in 150 DEG C of temperature Homogeneous hydro-thermal reaction 6h down, room temperature is naturally cooled to after the completion of reaction, and obtained carbon fiber is washed with deionized water or ethanol After dry, that is, obtain titania modified carbon fiber；
Step 3：By titania modified carbon fiber, bamboo fibre and Fanglun slurry cake according to 3:1:1 mass ratio is dispersed in water, Then fiber preform and naturally dry is made using Vacuum filtration device, the fiber preform after drying is modified using butyronitrile Resin impregnating, vulcanizer is used after naturally dry again at a temperature of 170 DEG C, it is hot-forming under 5MPa pressure, it is made two Titanium oxide modified carbon fiber reinforced resin based composites.
CN201610077211.4A 2016-02-03 2016-02-03 A kind of preparation method of titania modified carbon fiber enhancement resin base composite material Active CN105602000B (en)

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CN107828188A (en) * 2017-11-30 2018-03-23 万丰航空工业有限公司 A kind of manufacture method of carbon fibre composite for airplane skin
CN108755102B (en) * 2018-06-20 2020-05-22 西安交通大学 Burred carbon composite titanium dioxide nano fiber and preparation method and application thereof
CN111635615A (en) * 2020-06-24 2020-09-08 陕西科技大学 Preparation method of carbon fiber-titanium dioxide multistage reinforced resin matrix composite material
CN112092412B (en) * 2020-09-07 2022-06-28 陕西科技大学 Preparation method of nano titanium dioxide/sulfur-doped modified fibrous composite material
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