CN103450501B - Method for modifying surface of carbon fiber by using potassium persulfate/silver nitrate system - Google Patents
Method for modifying surface of carbon fiber by using potassium persulfate/silver nitrate system Download PDFInfo
- Publication number
- CN103450501B CN103450501B CN201310428701.0A CN201310428701A CN103450501B CN 103450501 B CN103450501 B CN 103450501B CN 201310428701 A CN201310428701 A CN 201310428701A CN 103450501 B CN103450501 B CN 103450501B
- Authority
- CN
- China
- Prior art keywords
- carbon fiber
- silver nitrate
- potassium persulphate
- nitrate system
- carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention relates to carbon fiber surface modification methods and discloses a method for modifying the surface of carbon fiber by using a potassium persulfate/silver nitrate system. The method is used for solving the problems in the existing carbon fiber surface oxidation methods that the loss of the mechanical properties of a material is relatively high, the operation is tedious and the implementation is difficult. The method comprises the steps: (1) removing epoxy coatings from the surface of the carbon fiber; (2) preparing the potassium persulfate/silver nitrate system; (3) oxidizing the carbon fiber by the potassium persulfate/silver nitrate system; (4) cleaning and drying, thereby obtaining the carbon fiber which is subjected to surface modification by using the potassium persulfate/silver nitrate system. According to the method, the loss of the mechanical properties of the carbon fiber which is subjected to surface modification by using the potassium persulfate/silver nitrate system is low, the operation is simple, and the implementation is easy. The method is used for carrying out surface modification on the carbon fiber by using the potassium persulfate/silver nitrate system.
Description
Technical field
The present invention relates to carbon fiber surface modification method.
Background technology
Carbon fiber is a kind of desirable polymer matrix composites reinforcement, and owing to having excellent mechanical property, low density, erosion resistance and environmental stability, it is widely used in aerospace and mechanical manufacturing field.In carbon-fibre composite, the stress transfer that the interface of carbon fiber and resin matrix can be subject to body material is on carbon fiber to reinforcement, so carbon-fibre composite will be brought into play the too busy to get away good interface of excellent mechanical property.Yet the surface of carbon fiber is but smooth and has chemically inertly, this tends to cause the interface binding power between carbon fiber and matrix faint, has a strong impact on the performance of matrix material.Therefore,, in order to improve the interface binding power of carbon-fibre composite, must carry out modification to carbon fiber surface.Conventional method of modifying comprises oxidation, coating and the grafting of carbon fiber surface.Oxidation is devoted to generate active group at carbon fiber surface, improve carbon fiber surface can, surface wettability and surface reaction activity, thereby make it can with good compound of resin matrix, and process active site be provided for coating and grafting.Therefore, the surface oxidation of carbon fiber is carbon fiber to be carried out to the basic steps of surface modification.
Conventional method for oxidation comprises chemical oxidation, electrochemical oxidation, Cement Composite Treated by Plasma etc.These methods, when having improved carbon fiber surface activity, often cause the greater loss of its mechanical property, and complex operation, are difficult for implementing.For example most widely used nitration mixture oxidation in chemical oxidation, is used the mixture of the vitriol oil and concentrated nitric acid as oxygenant, and experiment is dangerous high, complex operation, and length consuming time, the fiber bodies loss of strength of using nitration mixture carbon oxide fiber to cause is many more than 10%.Electrochemical oxidation and Cement Composite Treated by Plasma not only can cause greater loss to the mechanical property of carbon fiber, and degree of oxidation is restive, the shortcoming such as under the condition that does not possess plant and instrument, cannot implement.
In sum, the process for surface oxidation of existing carbon fiber exists the loss of material mechanical performance larger, is lost in 10% left and right, and complex operation is difficult for the problem of implementing.
CN102888750A discloses a kind of method of carbon fiber surface modification, carry out according to the following steps: carbon fiber bundle is carried out to surface preparation, then the carbon fiber bundle after surface preparation is entered to carry out surface oxidation treatment in subcritical water-potassium permanganate system, finally the carbon fiber bundle after oxidation is carried out to cleaning-drying, obtain the carbon fiber after surface modification.
Summary of the invention
The process for surface oxidation that the present invention will solve existing carbon fiber exists material mechanical performance loss larger, and complex operation, is difficult for the problem of enforcement, and a kind of method of Potassium Persulphate/Silver Nitrate system to carbon fiber surface modification of utilizing is provided.
Utilize the method for Potassium Persulphate/Silver Nitrate system to carbon fiber surface modification, specifically according to following steps, carry out:
One, the removal of carbon fiber surface epoxy coat: carbon fiber is put into apparatus,Soxhlet's extraction tube, the acetone of take extracts removal of impurities as extraction agent carries out Soxhlet, in temperature, be condensing reflux reaction 4h～8h at 75 ℃～85 ℃, obtain removing the carbon fiber after surface impurity, then the carbon fiber of removing after surface impurity is put into overcritical device, in temperature, be to soak 15min～35min in 350 ℃～380 ℃ and the pressure overcritical acetone-water system that is 7MPa～15MPa, obtain removing the carbon fiber after epoxy coat, again the carbon fiber of removing after epoxy coat is put into apparatus,Soxhlet's extraction tube, the acetone of take extracts removal of impurities as extraction agent carries out Soxhlet, in temperature, be condensing reflux reaction 2h～4h at 75 ℃～85 ℃, carbon fiber after being cleaned, again the carbon fiber after cleaning is put into the dry 2h～4h of 70 ℃～80 ℃ baking ovens, obtain dried carbon fiber,
In described overcritical acetone-water system, water is distilled water, and the volume ratio of distilled water and acetone is (4～6): 1;
Two, configuration Potassium Persulphate/Silver Nitrate system: add after Potassium Persulphate, Silver Nitrate and distilled water in beaker, be uniformly mixed, obtain Potassium Persulphate/Silver Nitrate system;
Described Potassium Persulphate amount of substance and the volume ratio of distilled water are (0.1～0.2) mol:1L; Described Silver Nitrate amount of substance and the volume ratio of distilled water are (0～0.005) mol:1L;
Three, Potassium Persulphate/Silver Nitrate system carbon oxide fiber: the dried carbon fiber that step 1 is obtained is put into the Potassium Persulphate/Silver Nitrate system obtaining to step 2, is to keep 1h～2.5h at 60 ℃～85 ℃ in temperature, the carbon fiber after being oxidized;
The volume ratio of the quality of described carbon fiber and Potassium Persulphate/Silver Nitrate system is (8.5～15.0) g:1L;
Four, clean and be dried: the carbon fiber after being oxidized is placed in distilled water and soaked, soak 3～5 times, single soak time is 5min～10min, carbon oxide fiber after being soaked, again the carbon oxide fiber after soaking is put into the dry 2h～4h of 70 ℃～80 ℃ baking ovens, obtain dried carbon oxide fiber, then dried carbon oxide fiber is put into apparatus,Soxhlet's extraction tube, the ethanol of take extracts removal of impurities as extraction agent carries out Soxhlet, in temperature, be condensing reflux reaction 2h～4h at 90 ℃～100 ℃, carbon oxide fiber after being cleaned, finally the carbon oxide fiber after cleaning is put into the dry 2h～4h of 70 ℃～80 ℃ baking ovens, obtain the carbon fiber after surface modification.
The invention has the beneficial effects as follows: one, utilize the carbon fiber mechanical property loss of Potassium Persulphate/Silver Nitrate system surface modification little, be lost in below 5%, the process for surface oxidation that has solved existing carbon fiber exists the larger shortcoming of material mechanical performance loss; Two, simple to operate, easily implement.
The present invention is for a kind of method of Potassium Persulphate/Silver Nitrate system to carbon fiber surface modification of utilizing.
Accompanying drawing explanation
Fig. 1 is the carbon fiber surface XPS scintigram that embodiment bis-step 1 are removed epoxy coat;
Fig. 2 is the carbon fiber surface XPS scintigram after embodiment bis-surface modifications;
Fig. 3 is the carbon fiber surface scanning electron microscope (SEM) photograph that embodiment bis-step 1 are removed epoxy coat;
Fig. 4 is the carbon fiber surface scanning electron microscope (SEM) photograph after embodiment bis-surface modifications.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: a kind of method of Potassium Persulphate/Silver Nitrate system to carbon fiber surface modification of utilizing described in present embodiment, specifically according to following steps, carry out:
One, the removal of carbon fiber surface epoxy coat: carbon fiber is put into apparatus,Soxhlet's extraction tube, the acetone of take extracts removal of impurities as extraction agent carries out Soxhlet, in temperature, be condensing reflux reaction 4h～8h at 75 ℃～85 ℃, obtain removing the carbon fiber after surface impurity, then the carbon fiber of removing after surface impurity is put into overcritical device, in temperature, be to soak 15min～35min in 350 ℃～380 ℃ and the pressure overcritical acetone-water system that is 7MPa～15MPa, obtain removing the carbon fiber after epoxy coat, again the carbon fiber of removing after epoxy coat is put into apparatus,Soxhlet's extraction tube, the acetone of take extracts removal of impurities as extraction agent carries out Soxhlet, in temperature, be condensing reflux reaction 2h～4h at 75 ℃～85 ℃, carbon fiber after being cleaned, again the carbon fiber after cleaning is put into the dry 2h～4h of 70 ℃～80 ℃ baking ovens, obtain dried carbon fiber,
In described overcritical acetone-water system, water is distilled water, and the volume ratio of distilled water and acetone is (4～6): 1;
Two, configuration Potassium Persulphate/Silver Nitrate system: add after Potassium Persulphate, Silver Nitrate and distilled water in beaker, be uniformly mixed, obtain Potassium Persulphate/Silver Nitrate system;
Described Potassium Persulphate amount of substance and the volume ratio of distilled water are (0.1～0.2) mol:1L; Described Silver Nitrate amount of substance and the volume ratio of distilled water are (0～0.005) mol:1L;
Three, Potassium Persulphate/Silver Nitrate system carbon oxide fiber: the dried carbon fiber that step 1 is obtained is put into the Potassium Persulphate/Silver Nitrate system obtaining to step 2, is to keep 1h～2.5h at 60 ℃～85 ℃ in temperature, the carbon fiber after being oxidized;
The volume ratio of the quality of described carbon fiber and Potassium Persulphate/Silver Nitrate system is (8.5～15.0) g:1L;
Four, clean and be dried: the carbon fiber after being oxidized is placed in distilled water and soaked, soak 3～5 times, single soak time is 5min～10min, carbon oxide fiber after being soaked, again the carbon oxide fiber after soaking is put into the dry 2h～4h of 70 ℃～80 ℃ baking ovens, obtain dried carbon oxide fiber, then dried carbon oxide fiber is put into apparatus,Soxhlet's extraction tube, the ethanol of take extracts removal of impurities as extraction agent carries out Soxhlet, in temperature, be condensing reflux reaction 2h～4h at 90 ℃～100 ℃, carbon oxide fiber after being cleaned, finally the carbon oxide fiber after cleaning is put into the dry 2h～4h of 70 ℃～80 ℃ baking ovens, obtain the carbon fiber after surface modification.
Present embodiment is by the removal of carbon fiber surface epoxy coat, guaranteed that follow-up oxide treatment is the oxidation that occurs in carbon fiber body surface, rather than the oxidation in conjunction with not firm epoxy coat to fiber surface, make fiber after processing with matrix resin compound tense, can produce strong chemical bonding force, rather than weak physical bond power, be conducive to the raising of carbon-fibre composite performance.The oxide treatment of Potassium Persulphate/Silver Nitrate system to carbon fiber, has utilized a small amount of silver ions that Potassium Persulphate is significantly activated, and accelerates it and decomposes the very strong sulfate radical free radical SO of generation oxidisability
4 -(redox potential 2.4V), sulfate radical radical pair carbon fiber surface is oxidized, and makes carbon fiber surface produce a large amount of oxygen-content active groups, thereby improves surface energy and the surfactivity of carbon fiber, strengthens being combined with the interface of matrix resin.In addition, due to Potassium Persulphate/Silver Nitrate can with the unstable carboxyl reaction of carbon fiber surface, remove carboxyl, this system also can significantly be controlled the body loss of strength of the carbon fiber that hyperoxidation causes.Carbon fiber surface is a kind of rapid layer graphite-structure; the stacking not graphite linings of rule is the main body of its structure; the carboxyl that oxidizing reaction produces is because volume is larger; part carboxyl is because space steric effect is crossed conference and caused serious distortion even to peel off to graphite flake layer; thereby affect the body intensity of carbon fiber, and these carboxyls are unsettled often, Potassium Persulphate/Silver Nitrate can react with it; remove these sterically hindered excessive carboxyls, the body intensity of protection carbon fiber is not suffered a loss.
Silver Nitrate catalysis Potassium Persulphate decomposes generation sulfate radical free radical SO
4 -reaction expression is as follows:
Potassium Persulphate/Silver Nitrate decarboxylic reaction general formula is as follows:
Ag
2++RCO
2H→Ag
++RCO
2·+H
+
RCO
2·→R·+CO
2
The beneficial effect of present embodiment is: one, utilize the carbon fiber mechanical property loss of Potassium Persulphate/Silver Nitrate system surface modification little, be lost in below 5%, the process for surface oxidation that has solved existing carbon fiber exists the larger shortcoming of material mechanical performance loss; Two, simple to operate, easily implement.
Embodiment two: present embodiment is different from embodiment one: in the overcritical acetone-water system described in step 1, water is distilled water, and the volume ratio of distilled water and acetone is 5:1.Other is identical with embodiment one.
Embodiment three: present embodiment is different from one of embodiment one or two: then the carbon fiber of removing after impurity is put into overcritical device in step 1, in temperature, be to soak 20min～30min in 360 ℃～370 ℃ and the pressure overcritical acetone-water system that is 8MPa～14MPa, obtain removing the carbon fiber after epoxy coat.Other is identical with embodiment one or two.
Embodiment four: present embodiment is different from one of embodiment one to three: the volume ratio of the Potassium Persulphate amount of substance described in step 2 and distilled water is (0.1～0.15) mol:1L; The volume ratio of the Silver Nitrate amount of substance described in step 2 and distilled water is (0～0.004) mol:1L.Other is identical with embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to four: the volume ratio of the quality of the carbon fiber described in step 3 and Potassium Persulphate/Silver Nitrate system is (8.5～14.5) g:1L.Other is identical with embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five: the dried carbon fiber in step 3, step 1 being obtained is put into the Potassium Persulphate/Silver Nitrate system obtaining to step 2, at temperature 60 C～80 ℃, keep 1h～2h, the carbon fiber after being oxidized.Other is identical with embodiment one to five.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment mono-:
A kind of method of Potassium Persulphate/Silver Nitrate system to carbon fiber surface modification of utilizing described in the present embodiment, specifically according to following steps, carry out:
One, the removal of carbon fiber surface epoxy coat: carbon fiber is put into apparatus,Soxhlet's extraction tube, the acetone of take extracts removal of impurities as extraction agent carries out Soxhlet, in temperature, be condensing reflux reaction 4h at 80 ℃, obtain removing the carbon fiber after surface impurity, then the carbon fiber of removing after surface impurity is put into overcritical device, in temperature, be to soak 20min in 360 ℃ and the pressure overcritical acetone-water system that is 10MPa, obtain removing the carbon fiber after epoxy coat, again the carbon fiber of removing after epoxy coat is put into apparatus,Soxhlet's extraction tube, the acetone of take extracts removal of impurities as extraction agent carries out Soxhlet, in temperature, be condensing reflux reaction 2h at 80 ℃, carbon fiber after being cleaned, again the carbon fiber after cleaning is put into the dry 2h of 80 ℃ of baking ovens, obtain dried carbon fiber,
In described overcritical acetone-water system, water is distilled water, and the volume ratio of distilled water and acetone is 5:1;
Two, configuration Potassium Persulphate/Silver Nitrate system: add after Potassium Persulphate, Silver Nitrate and distilled water in beaker, be uniformly mixed, obtain Potassium Persulphate/Silver Nitrate system;
Described Potassium Persulphate amount of substance and the volume ratio of distilled water are 0.1mol:1L; Described Silver Nitrate amount of substance and the volume ratio of distilled water are 0.001mol:1L;
Three, Potassium Persulphate/Silver Nitrate system carbon oxide fiber: the dried carbon fiber 0.4g that step 1 is obtained puts into the Potassium Persulphate/Silver Nitrate system obtaining to step 2, is at 60 ℃, to keep 1h in temperature, the carbon fiber after being oxidized;
Four, clean and be dried: the carbon fiber after being oxidized is placed in 400mL distilled water and soaked, soak 3 times, single soak time is 5min, carbon oxide fiber after being soaked, again the carbon oxide fiber after soaking is put into the dry 2h of 80 ℃ of baking ovens, obtain dried carbon oxide fiber, then dried carbon oxide fiber is put into apparatus,Soxhlet's extraction tube, the ethanol of take extracts removal of impurities as extraction agent carries out Soxhlet, in temperature, be condensing reflux reaction 2h at 100 ℃, carbon oxide fiber after being cleaned, finally the carbon oxide fiber after cleaning is put into the dry 2h of 70 ℃～80 ℃ baking ovens, obtain the carbon fiber after surface modification.
Carbon fiber after Potassium Persulphate for the present embodiment/Silver Nitrate system surface modification utilizes XPS test, and after test result shows modification, carbon fiber surface oxygen level is compared with the carbon fiber of removing after epoxy coat, and content of surface oxygen is increased to 13.61% by 4.49%.
Carbon fiber after Potassium Persulphate for the present embodiment/Silver Nitrate system surface modification utilizes monofilament tensile strength test, test result to show after modification that the loss of carbon fiber monofilament tensile strength is 0.56%.
Carbon fiber after Potassium Persulphate for the present embodiment/Silver Nitrate system surface modification utilizes dynamic contact angle test, and can by the surface of Wu method calculating carbon fiber, after calculation result shows modification, carbon fibre surface energy is compared with the carbon fiber of removing after epoxy coat, and surface can improve 29%.
The present embodiment utilizes the carbon fiber after Potassium Persulphate/Silver Nitrate system surface modification to utilize interface shearing performance test, after test result shows modification, carbon fiber is compared with the interfacial adhesion power of epoxy resin with the carbon fiber of removing after epoxy coat with the interfacial adhesion power of epoxy resin, and interfacial adhesion power improves 52.99%.
Embodiment bis-: the difference of the present embodiment and embodiment mono-is: the dried carbon fiber 0.4g in step 3, step 1 being obtained puts into the Potassium Persulphate/Silver Nitrate system obtaining to step 2, in temperature, be to keep 1h at 70 ℃, the carbon fiber after being oxidized.Other are identical with embodiment mono-.
Carbon fiber after Potassium Persulphate for the present embodiment/Silver Nitrate system surface modification utilizes XPS test, and after test result shows modification, carbon fiber surface oxygen level is compared with the carbon fiber of removing after epoxy coat, and content of surface oxygen is increased to 14.11% by 4.49%.
Carbon fiber after Potassium Persulphate for the present embodiment/Silver Nitrate system surface modification utilizes monofilament tensile strength test, test result to show after modification that the loss of carbon fiber monofilament tensile strength is 4.5%.
Carbon fiber after Potassium Persulphate for the present embodiment/Silver Nitrate system surface modification utilizes dynamic contact angle test, and can by the surface of Wu method calculating carbon fiber, after calculation result shows modification, carbon fibre surface energy is compared with the carbon fiber of removing after epoxy coat, and surface can improve 34%.
Carbon fiber after Potassium Persulphate for the present embodiment/Silver Nitrate system surface modification utilizes interface shearing performance test, after test result shows modification, carbon fiber is compared with the interfacial adhesion power of epoxy resin with the carbon fiber of removing after epoxy coat with the interfacial adhesion power of epoxy resin, and interfacial adhesion power improves 62.52%.
The carbon fiber surface XPS scintigram of the present embodiment step 1 removal epoxy coat as shown in Figure 1, the oxygen peak that is positioned at as shown in Figure 1 532eV left and right is very low, sharp side is long-pending relatively little, after removal epoxy coat is described, unmodified carbon fiber surface oxygen element content is very low, oxygen element content is 4.49%, the high oxy radical of reactive behavior seldom, is difficult for reacting with epoxy resin generation strong interfacial bond.
Carbon fiber surface XPS scintigram after Potassium Persulphate for the present embodiment/Silver Nitrate System Modification as shown in Figure 2, near oxygen peak intensity 532eV is apparently higher than Fig. 1 as shown in Figure 2, oxygen element content is 14.11%, significantly the surface of enhanced carbon fiber can in the increase of oxygen element content, strengthen the infiltration of resin and carbon fiber surface, and improve the reactive behavior of carbon fiber surface, thereby improve interface cohesive force.
By Fig. 1 and the known Potassium Persulphate/Silver Nitrate of Fig. 2 system, can obviously be improved the reactive behavior of the oxygen element content raising carbon fiber surface of carbon fiber surface, increase the interface cohesive force of carbon fiber and epoxy resin.
The carbon fiber surface scanning electron microscope (SEM) photograph of the present embodiment step 1 removal epoxy coat as shown in Figure 3, remove as shown in Figure 3 the carbon fiber surface smoother of epoxy coat, but have a small amount of axial recess, this is by PAN precursor " heredity ", to be obtained in spinning process.
As shown in Figure 4, after modification, carbon fiber surface pattern is similar to precursor as shown in Figure 4 for carbon fiber surface scanning electron microscope (SEM) photograph after Potassium Persulphate for the present embodiment/Silver Nitrate System Modification, has a small amount of axial recess, and remarkable change does not occur for groove size and the degree of depth.
By the carbon fiber after the known modification of Fig. 3 and Fig. 4, still maintain the surface topography similar to the carbon fiber of removing epoxy coat; illustrate that this method of modifying does not cause serious etching and destruction to carbon fiber surface, thereby protected to a certain extent carbon fiber body intensity.
Embodiment tri-: the difference of the present embodiment and embodiment mono-is: the volume ratio of the Potassium Persulphate amount of substance described in step 2 and distilled water is 0.1mol:1L; Described Silver Nitrate amount of substance and the volume ratio of distilled water are 0mol:1L.Other are identical with experiment one.
Carbon fiber after Potassium Persulphate for the present embodiment/Silver Nitrate system surface modification utilizes XPS test, and after test result shows modification, carbon fiber surface oxygen level is compared with the carbon fiber of removing after epoxy coat, and content of surface oxygen is increased to 9.47% by 4.49%.
Carbon fiber after Potassium Persulphate for the present embodiment/Silver Nitrate system surface modification utilizes monofilament tensile strength test, test result to show after modification that the loss of carbon fiber monofilament tensile strength is 0.84%.
Carbon fiber after Potassium Persulphate for the present embodiment/Silver Nitrate system surface modification utilizes dynamic contact angle test, and can by the surface of Wu method calculating carbon fiber, after calculation result shows modification, carbon fibre surface energy is compared with the carbon fiber of removing after epoxy coat, and surface can improve 18%.
Carbon fiber after Potassium Persulphate for the present embodiment/Silver Nitrate system surface modification utilizes interface shearing performance test, after test result shows modification, carbon fiber is compared with the interfacial adhesion power of epoxy resin with the carbon fiber of removing after epoxy coat with the interfacial adhesion power of epoxy resin, and interfacial adhesion power improves 27.80%.
Claims (6)
1. utilize the method for Potassium Persulphate/Silver Nitrate system to carbon fiber surface modification, it is characterized in that a kind of Potassium Persulphate/Silver Nitrate system of utilizing carries out according to following steps the method for carbon fiber surface modification:
One, the removal of carbon fiber surface epoxy coat: carbon fiber is put into apparatus,Soxhlet's extraction tube, the acetone of take extracts removal of impurities as extraction agent carries out Soxhlet, in temperature, be condensing reflux reaction 4h～8h at 75 ℃～85 ℃, obtain removing the carbon fiber after surface impurity, then the carbon fiber of removing after surface impurity is put into overcritical device, in temperature, be to soak 15min～35min in 350 ℃～380 ℃ and the pressure overcritical acetone-water system that is 7MPa～15MPa, obtain removing the carbon fiber after epoxy coat, again the carbon fiber of removing after epoxy coat is put into apparatus,Soxhlet's extraction tube, the acetone of take extracts removal of impurities as extraction agent carries out Soxhlet, in temperature, be condensing reflux reaction 2h～4h at 75 ℃～85 ℃, carbon fiber after being cleaned, again the carbon fiber after cleaning is put into the dry 2h～4h of 70 ℃～80 ℃ baking ovens, obtain dried carbon fiber,
In described overcritical acetone-water system, water is distilled water, and the volume ratio of distilled water and acetone is (4～6): 1;
Two, configuration Potassium Persulphate/Silver Nitrate system: add after Potassium Persulphate, Silver Nitrate and distilled water in beaker, be uniformly mixed, obtain Potassium Persulphate/Silver Nitrate system;
Described Potassium Persulphate amount of substance and the volume ratio of distilled water are (0.1～0.2) mol:1L; Described Silver Nitrate amount of substance and the volume ratio of distilled water are (0～0.005) mol:1L;
Three, Potassium Persulphate/Silver Nitrate system carbon oxide fiber: the dried carbon fiber that step 1 is obtained is put into the Potassium Persulphate/Silver Nitrate system obtaining to step 2, is to keep 1h～2.5h at 60 ℃～85 ℃ in temperature, the carbon fiber after being oxidized;
The volume ratio of the quality of described carbon fiber and Potassium Persulphate/Silver Nitrate system is (8.5～15.0) g:1L;
Four, clean and be dried: the carbon fiber after being oxidized is placed in distilled water and soaked, soak 3～5 times, single soak time is 5min～10min, carbon oxide fiber after being soaked, again the carbon oxide fiber after soaking is put into the dry 2h～4h of 70 ℃～80 ℃ baking ovens, obtain dried carbon oxide fiber, then dried carbon oxide fiber is put into apparatus,Soxhlet's extraction tube, the ethanol of take extracts removal of impurities as extraction agent carries out Soxhlet, in temperature, be condensing reflux reaction 2h～4h at 90 ℃～100 ℃, carbon oxide fiber after being cleaned, finally the carbon oxide fiber after cleaning is put into the dry 2h～4h of 70 ℃～80 ℃ baking ovens, obtain the carbon fiber after surface modification.
2. a kind of method of Potassium Persulphate/Silver Nitrate system to carbon fiber surface modification of utilizing according to claim 1, is characterized in that in the overcritical acetone-water system described in step 1, water is distilled water, and the volume ratio of distilled water and acetone is 5:1.
3. a kind of method of Potassium Persulphate/Silver Nitrate system to carbon fiber surface modification of utilizing according to claim 1, it is characterized in that then the carbon fiber of removing after impurity being put into overcritical device in step 1, in temperature, be to soak 20min～30min in 360 ℃～370 ℃ and the pressure overcritical acetone-water system that is 8MPa～14MPa, obtain removing the carbon fiber after epoxy coat.
4. a kind of method of Potassium Persulphate/Silver Nitrate system to carbon fiber surface modification of utilizing according to claim 1, the volume ratio that it is characterized in that the Potassium Persulphate amount of substance described in step 2 and distilled water is (0.1～0.15) mol:1L; The volume ratio of the Silver Nitrate amount of substance described in step 2 and distilled water is (0～0.004) mol:1L.
5. a kind of method of Potassium Persulphate/Silver Nitrate system to carbon fiber surface modification of utilizing according to claim 1, is characterized in that the quality of the carbon fiber described in step 3 and the volume ratio of Potassium Persulphate/Silver Nitrate system are for (8.5～14.5) g:1L.
6. a kind of method of Potassium Persulphate/Silver Nitrate system to carbon fiber surface modification of utilizing according to claim 1, it is characterized in that the dried carbon fiber in step 3, step 1 being obtained puts into the Potassium Persulphate/Silver Nitrate system obtaining to step 2, at temperature 60 C～80 ℃, keep 1h～2h, the carbon fiber after being oxidized.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310428701.0A CN103450501B (en) | 2013-09-18 | 2013-09-18 | Method for modifying surface of carbon fiber by using potassium persulfate/silver nitrate system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310428701.0A CN103450501B (en) | 2013-09-18 | 2013-09-18 | Method for modifying surface of carbon fiber by using potassium persulfate/silver nitrate system |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103450501A CN103450501A (en) | 2013-12-18 |
| CN103450501B true CN103450501B (en) | 2014-11-26 |
Family
ID=49733365
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310428701.0A Active CN103450501B (en) | 2013-09-18 | 2013-09-18 | Method for modifying surface of carbon fiber by using potassium persulfate/silver nitrate system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103450501B (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103966843B (en) * | 2014-05-16 | 2015-12-02 | 哈尔滨工业大学 | A kind of aryldiazonium salt system that utilizes is to the method for carbon fiber surface modification |
| US20170233611A1 (en) * | 2014-10-31 | 2017-08-17 | Japan Matex Co., Ltd. | Method of manufacturing a carbon fiber resin tape and the carbon fiber resin tape |
| CN104562707B (en) * | 2014-12-26 | 2017-01-11 | 哈尔滨工业大学 | Method for adsorbing polymine on carbon fiber surface in supercritical methanol |
| CN106868902B (en) * | 2017-01-20 | 2018-11-20 | 陕西科技大学 | A kind of preparation method of sheet self assembly manganese dioxide modified carbon fiber reinforced resin base frication material |
| CN107266712B (en) * | 2017-07-05 | 2018-11-27 | 青岛大学 | A kind of method of carbon fiber surface grafting dissaving polymer |
| CN109385891B (en) * | 2018-11-15 | 2020-12-01 | 青岛大学 | Method for grafting curing agent imidazole on surface of carbon fiber |
| CN109868375B (en) * | 2019-04-03 | 2021-04-16 | 四川明宏恒进科技有限公司 | Production method of chromium metal |
| CN110512415A (en) * | 2019-08-27 | 2019-11-29 | 青岛大学 | A method of by opening in carbon fiber surface engrafted nanometer silica |
| CN114292490B (en) * | 2022-01-06 | 2023-11-28 | 深圳市爱康运动用品有限公司 | Continuous fiber reinforced thermoplastic composite material and preparation method and application thereof |
| CN114507447A (en) * | 2022-03-10 | 2022-05-17 | 广东华聚科技有限公司 | Method for preparing modified plastic from reinforced and toughened modified nylon |
| CN114806127B (en) * | 2022-05-10 | 2024-02-20 | 中山市卡邦碳纤维材料制品有限公司 | Carbon fiber pipe and manufacturing method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102851940A (en) * | 2012-08-30 | 2013-01-02 | 西北工业大学 | Method for supersonic wave-reinforced liquid chemical surface modification of carbon fibers |
| CN102888750A (en) * | 2012-10-29 | 2013-01-23 | 哈尔滨工业大学 | Method for modifying surface of carbon fiber |
-
2013
- 2013-09-18 CN CN201310428701.0A patent/CN103450501B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102851940A (en) * | 2012-08-30 | 2013-01-02 | 西北工业大学 | Method for supersonic wave-reinforced liquid chemical surface modification of carbon fibers |
| CN102888750A (en) * | 2012-10-29 | 2013-01-23 | 哈尔滨工业大学 | Method for modifying surface of carbon fiber |
Non-Patent Citations (2)
| Title |
|---|
| 吴越，等."液态氧化法处理超高分子量聚乙烯纤维".《玻璃钢学会第十三届全国玻璃钢/复合材料学术年会论文集》.1999,第61－64页. * |
| 吴越,等."液态氧化法处理超高分子量聚乙烯纤维".《玻璃钢学会第十三届全国玻璃钢/复合材料学术年会论文集》.1999,第61-64页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103450501A (en) | 2013-12-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103450501B (en) | Method for modifying surface of carbon fiber by using potassium persulfate/silver nitrate system | |
| CN103643503B (en) | A kind of processing method of silane coupler modified carbon fiber surface | |
| CN102888750B (en) | Method for modifying surface of carbon fiber | |
| CN104195835A (en) | Method for grafting polymer on surface of carbon fiber under supercritical condition | |
| CN106854833B (en) | A kind of antistatic ultra high molecular weight polyethylene fiber of lightweight and preparation method thereof | |
| CN106637923A (en) | Method of quickly and continuously depositing graphene on surface of electric-conductive fibers | |
| CN107174956B (en) | The preparation method of perfluoroethylene-propylene hollow-fibre membrane with finishing coat | |
| CN101985499A (en) | Method for preparing super-hydrophobic surface polypropylene | |
| CN108439457B (en) | Method for preparing zinc oxide nanorod/carbon cloth friction material by hydrothermal electrophoresis method | |
| CN107761375A (en) | A kind of method in carbon fiber surface grafting branching molecule tannic acid | |
| CN103806281A (en) | Method for improving interface performance of composite material by grafting hyperbranched polyglycerol on surfaces of carbon fibers | |
| CN109468843A (en) | A method of hydroxy-end capped dissaving polymer is grafted in carbon fiber surface | |
| CN108624043A (en) | A kind of aerogel composite and preparation method thereof of polypyrrole cladding copper nano-wire | |
| CN105449210A (en) | Preparation method for porous graphene micro-sheet | |
| CN103806274A (en) | Polymer surface grafting method for carbon fiber | |
| CN107163291A (en) | A kind of carbon fiber/polyphenyl thioether composite material and preparation method thereof | |
| CN101798752B (en) | Chemical method for activating aramid fiber surface | |
| CN111170307B (en) | Nanocarbon modified hollow activated carbon microtube and preparation method and application thereof | |
| KR101577429B1 (en) | Polyacrylonitrile polymer and the spinning solution comprising the same | |
| CN109986665B (en) | High-conductivity and high-flexibility nickel-plated wood chip and preparation method thereof | |
| CN110863341A (en) | Preparation method of PA66 grafted carbon fiber | |
| CN105332098A (en) | Carbon fiber activation process | |
| Klimov et al. | An investigation of the hydrophobic property stability of grafted polymeric coatings on a cellulose material surface | |
| CN105442302B (en) | A kind of compound knitmesh of water process based on graphene oxide, preparation method and applications | |
| CN109485912B (en) | Electro-promotion heterogeneous catalytic device for recycling CFRP (carbon fiber reinforced plastics) and control method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |