CN114702329A - Low-dimensional carbon material reinforced carbon graphite material and preparation method thereof - Google Patents
Low-dimensional carbon material reinforced carbon graphite material and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 92
- 239000007770 graphite material Substances 0.000 title claims abstract description 80
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 239000010426 asphalt Substances 0.000 claims abstract description 53
- 239000003607 modifier Substances 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 30
- 239000011230 binding agent Substances 0.000 claims abstract description 28
- 239000006185 dispersion Substances 0.000 claims abstract description 26
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 20
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000006229 carbon black Substances 0.000 claims abstract description 13
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims abstract description 10
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000006253 pitch coke Substances 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000000465 moulding Methods 0.000 claims abstract description 5
- 238000012216 screening Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 239000000853 adhesive Substances 0.000 claims abstract description 3
- 230000001070 adhesive effect Effects 0.000 claims abstract description 3
- 239000002134 carbon nanofiber Substances 0.000 claims description 15
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 15
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- 239000000835 fiber Substances 0.000 claims 2
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Abstract
A low-dimensional carbon material reinforced carbon graphite material comprises the following components which are uniformly dispersed: aggregate: pitch coke and carbon black; a low-dimensional carbon material; adhesive: modified asphalt and/or high temperature asphalt; dispersing modifier: at least one of tetrahydrofuran, toluene, or quinoline. The preparation method of the low-dimensional carbon material reinforced carbon graphite material comprises the following steps: (1) mixing and stirring a dispersion modifier and a binder, and mixing and stirring the dispersion modifier and a low-dimensional carbon material to obtain two parts of suspension; (2) and blending the two turbid liquids, adding aggregate, mixing at low temperature, drying, crushing, screening, molding and roasting to obtain the low-dimensional carbon material reinforced carbon graphite material. The low-dimensional carbon material reinforced carbon graphite material can realize the uniform dispersion of the low-dimensional carbon material in the reinforced carbon graphite material, inhibit the defect initiation in the roasting process, inhibit the crack propagation in the micro-area where the low-dimensional carbon material is positioned in the service process of the material and realize the improvement of the macro-mechanical property of the special carbon graphite material.
Description
Technical Field
The invention belongs to the technical field of graphite materials, and particularly relates to a low-dimensional carbon material reinforced carbon graphite material and a preparation method thereof.
Background
The special carbon graphite material has the characteristics of high strength, high density, high purity and the like, and is widely applied to the fields of aerospace, traffic, energy, chemical industry and the like. However, in the process of preparing and roasting the special carbon graphite material blank, a series of hot blood reactions such as pyrolysis, polycondensation and the like can occur to the binding agent, so that a large amount of light components escape, and inevitable random microcracks and pore defects are formed in the special carbon graphite material blank. Due to the defects, the special carbon graphite material is easy to abnormally lose efficacy under a special service working condition, and finally, a safety accident is caused. Therefore, how to regulate the microstructure of the special carbon graphite material, improve the macroscopic performance and realize the structural function integration becomes an important technical difficulty for researching the special carbon graphite material.
Analysis is carried out on the selection of preparation raw materials, the reduction of the particle size of the aggregate can obviously improve the strength of the material, and the asphalt binder with high softening point can endow the special carbon graphite material with higher strength, so that the preparation of the special carbon graphite material by adopting the fine particle carbonaceous aggregate and the high-temperature asphalt binder is a reasonable research method. Meanwhile, the low-dimensional carbon nano material is widely applied to the field of composite materials as a reinforcing phase due to the perfect crystal structure and excellent electric conduction, heat conduction and mechanical properties, and related researches show that the low-dimensional carbon nano material can inhibit the initiation and the expansion of microcracks and pore defects in the composite materials and improve the structural integrity of the materials. Based on the analysis, the special carbon graphite material is prepared by adopting the fine-particle carbonaceous aggregate, the high-temperature asphalt binder and the low-dimensional carbon nano-material reinforcing phase, and the structural function integration of the special carbon graphite material can be realized.
However, the problems of easy agglomeration among the particles and uneven mixing of the aggregate/the binder in the kneading process can be caused on the one hand due to small granularity and large specific surface area of the aggregate particles; on the other hand, the preparation material needs more high-temperature asphalt binder, so that more light components are volatilized during the roasting process to cause more defects to be generated. Meanwhile, the special carbon graphite material prepared by using the high-temperature asphalt binder has the problems of uneven asphalt/fine particle aggregate mixing and poor interface wettability in the kneading process due to poor fluidity; on the other hand, the special carbon graphite material prepared by using high-temperature asphalt with a higher softening point through the traditional kneading process has higher requirements on a heating system of kneading equipment. The special carbon graphite material prepared by the traditional melting and kneading preparation process is easy to agglomerate and difficult to uniformly disperse in a material matrix, so that stress concentration can be caused to influence the macroscopic performance of the special carbon graphite material.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects and shortcomings in the background technology and provides a low-dimensional carbon material reinforced carbon graphite material and a preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a low-dimensional carbon material reinforced carbon graphite material comprises the following components which are uniformly dispersed:
aggregate: pitch coke and carbon black;
a low-dimensional carbon material;
adhesive: modified asphalt and/or high temperature asphalt;
dispersing modifier: at least one of tetrahydrofuran, toluene, or quinoline.
The softening point of the asphalt is reduced by adding the dispersion modifier, so that an asphalt binder and an aggregate/asphalt mixing system with good fluidity at normal temperature are obtained; meanwhile, the dispersion modifier is used as a dispersion medium of the low-dimensional carbon material and is blended with an aggregate/asphalt mixed system to prepare the special carbon graphite material with the uniformly dispersed low-dimensional carbon material reinforced, and the low-dimensional carbon material is uniformly dispersed.
Organic solvents such as tetrahydrofuran, toluene or quinoline are used as dispersing modifiers, and on one hand, the dispersing modifiers are added into the asphalt to effectively improve the softening point of the asphalt, so that the asphalt has good fluidity at normal temperature, can coat the aggregate well and can permeate into pores of aggregate particles, and finally effectively improve the homogeneity of the special carbon graphite material. Meanwhile, tetrahydrofuran, toluene or quinoline and other organic solvents are used as dispersion media of the low-dimensional carbon material and are blended with the aggregate/asphalt mixed system, so that the dispersibility of the material is improved, and the uniformly dispersed low-dimensional carbon material micro-area toughening special carbon graphite material can be finally prepared.
Preferably, the particle size distribution D of the pitch coke50The asphalt coke and the carbon black are 85-95 parts by mass of the asphalt coke and 5-15 parts by mass of the carbon black.
The aggregate distribution in the fine particle range of the asphalt coke has high true density and specific strength, but the problem of easy agglomeration also exists. The dispersion modifier added in the method can improve the dispersibility of the fine particle aggregate and promote the uniform distribution of the fine particle aggregate while improving the dispersibility of the low-dimensional carbon material
Preferably, the low-dimensional carbon material comprises at least one of carbon nanofibers, carbon nanotubes or graphene, and the amount of the low-dimensional carbon material added is 0.5 to 1.5 wt% of the total mass of the binder pitch.
Preferably, the modified asphalt has a softening point of 140 ℃ at 120, the high-temperature asphalt has a softening point of 170 ℃ at 150, and the addition amount of the binder accounts for 70-100 wt% of the total mass of the aggregate.
Preferably, the dispersion modifier is of analytical grade, and the addition amount accounts for 300-400 wt% of the total mass of the binder.
As a general inventive concept, the present invention also provides a method for preparing a low-dimensional carbon material reinforced carbon graphite material, comprising the steps of:
(1) respectively mixing and stirring a dispersion modifier and a binder, and mixing and stirring the dispersion modifier and a low-dimensional carbon material to obtain two parts of turbid liquid;
(2) and blending the two turbid liquids, adding aggregate, mixing at low temperature, drying, crushing, screening, molding and roasting to obtain the low-dimensional carbon material reinforced carbon graphite material.
According to the method, the affinity between the low-dimensional carbon material and the dispersion modifier is improved by using the dispersion modifier, and the purpose of separating the low-dimensional carbon materials from each other is achieved by matching with mechanical stirring and ultrasonic treatment. On one hand, the dispersion modifier solves the problem that a low-dimensional carbon material is easy to agglomerate, and on the other hand, the dispersion modifier can also solve the problem that the homogeneity of a final material is poor due to the fact that fine particles are easy to agglomerate when a fine particle aggregate is used for preparing a carbon graphite material.
The application of the dispersion modifier can reduce the softening point of the binder and the requirement of melting temperature by matching the dispersion modifier with the binder. More preferably, the binder is modified asphalt and/or high-temperature asphalt, the softening point refers to the critical temperature when the asphalt has certain fluidity, and the addition of the organic solvent can greatly reduce the softening point of the asphalt for the asphalt with higher softening point.
The dispersing modifier, the binder and the low-dimensional carbon material are respectively stirred, so that the two suspensions are uniformly dispersed to a certain degree before blending, and the dispersibility of the final product is further improved.
Preferably, the dispersion modifier and the low-dimensional carbon material in the step (1) are subjected to ultrasonic treatment while being mixed and stirred, and the co-treatment time of mechanical stirring and ultrasonic treatment is 20-30 min. The ultrasonic treatment can promote the dispersion of the low-dimensional carbon material in the dispersion modifier, i.e., inhibit the agglomeration thereof.
Preferably, the stirring time of the modifier and the binder in the step (1) is 50-80 min;
preferably, the blending time of the suspension in the step (2) is 20-40 min; the low-temperature mixing temperature is 40-60 ℃; the mixing time is 1-2 h. The low-temperature mixing is to prevent the volatilization of the dispersing modifier and ensure that the high-temperature asphalt or the modified asphalt has good fluidity to coat the aggregate particles and the low-dimensional carbon material.
Preferably, the sieving screen in the step (2) is 250-350 meshes. Controlling the particle size distribution of the mixed particles to ensure the homogeneity of the obtained improved carbon graphite material.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation method of the low-dimensional carbon material reinforced carbon graphite material is different from the traditional preparation method, the softening point of the asphalt is reduced by adding the organic solvent of the dispersion modifier, the low-temperature fluidity of the asphalt is improved, the uniform coating and infiltration of the asphalt binder to the fine-particle carbonaceous aggregate can be realized, meanwhile, the dispersion modifier improves the dispersibility of the aggregate, the homogeneity of the special carbon graphite material can be effectively improved, the comprehensive mechanical property of the material is improved, and the structural function integration of the special carbon graphite material is realized.
(2) The low-dimensional carbon material reinforced carbon graphite material can realize the uniform dispersion of the low-dimensional carbon material in the reinforced carbon graphite material, the uniformly dispersed low-dimensional carbon material can inhibit the defect initiation in the roasting process, and the crack propagation is inhibited in the micro-area where the low-dimensional carbon material is located in the service process of the material, so that the improvement of the macro-mechanical property of the special carbon graphite material is realized.
Drawings
In order to more clearly illustrate the embodiments or technical solutions of the present invention, the drawings used in the embodiments or technical solutions in the prior art are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is an SEM photograph of the low-dimensional carbon material-reinforced carbon graphite material prepared in example 1 of the present invention.
Fig. 2 is an SEM photograph of the low-dimensional carbon material-reinforced carbon graphite material prepared in example 1 of the present invention.
Fig. 3 is an SEM photograph of the low-dimensional carbon material-reinforced carbon graphite material prepared in comparative example 1 of the present invention.
Fig. 4 is an SEM photograph of the low-dimensional carbon material-reinforced carbon graphite material prepared in comparative example 1 of the present invention.
Detailed Description
In order to facilitate understanding of the invention, the invention will be described more fully and in detail with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically indicated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the low-dimensional carbon material reinforced carbon graphite material provided by the invention; the special carbon graphite material is mainly prepared from the following raw materials in parts by mass: asphalt coke (D)5020um), 10 parts of carbon black, a small amount of binder modified asphalt (softening point 120 ℃), carbon nanofibers and tetrahydrofuran, wherein the addition amount of the modified asphalt accounts for 80 wt% of the total mass of the asphalt coke and the carbon black; the addition amount of the carbon nano-fiber accounts for 1 wt% of the total mass of the binder asphalt; the adding amount of tetrahydrofuran which is an organic solvent and is used for reducing the softening point of the asphalt is 400 wt% of the total mass of the binder; the organic solvent used for dispersing the carbon nanofibers was 200ml of tetrahydrofuran.
The preparation method of the low-dimensional carbon material reinforced carbon graphite material comprises the following steps:
(1) adding tetrahydrofuran and modified asphalt powder into a kneader and mixing for 1 h; simultaneously adding the carbon nanofibers and tetrahydrofuran into a beaker for mechanical stirring and ultrasonic treatment for 30 min.
(2) Adding the carbon nanofiber suspension obtained in the step (1) into a kneading machine for blending for 30min, then adding the pitch coke and the carbon black into the kneading machine, and heating to 50 ℃. And after mixing for 2 hours, putting the paste into a blast drier for drying, and then crushing, screening (sieving by a 300-mesh sieve), molding (compression molding under 15 MPa) and roasting the dried material to obtain the low-dimensional carbon material toughened special carbon graphite material.
SEM images of fracture surfaces of the low-dimensional carbon material reinforced carbon graphite material prepared in this embodiment are shown in fig. 1 and 2, and it can be observed from fig. 1 and 2 that micro-regions of the low-dimensional carbon material reinforced carbon graphite material of the present invention have uniformly dispersed single carbon nanofibers, and the carbon nanofibers present in the micro-regions can toughen the micro-regions of the carbon graphite material and inhibit crack propagation; compared with the fracture surface SEM images of figures 3 and 4 in comparative example 1, the low-dimensional carbon material reinforced carbon graphite material prepared by the embodiment has more compact combination among fracture surface particles and reduced size of pore defects.
The low-dimensional carbon material reinforced carbon graphite material sample in the embodiment was subjected to performance test, and the test results are shown in table 1.
TABLE 1 Properties of the carbon graphite Material reinforced with the Low-dimensional carbon Material of example 1
Wherein, the bending strength and the compressive strength of the low-dimensional carbon material reinforced carbon graphite material are tested by adopting a American INSTRON-3382 type hydraulic electronic universal material testing machine; hardness was measured using an SH-19A Shore hardness tester manufactured by Riizhou Huayin testing apparatus Ltd, using an automatic densimeter MH-300A to measure density, using a mercury porosimeter AutoPore IV 9500 to measure open porosity, 3 times for each test, and averaging the results.
Comparative example 1:
the low-dimensional carbon material reinforced carbon graphite material of the comparative example adopts a traditional preparation process, and is different from the process for preparing the low-dimensional carbon material reinforced carbon graphite material by adding and mixing a solvent in the embodiment. The low-dimensional carbon material reinforced carbon graphite material is mainly prepared from the following raw materials in parts by mass: asphalt coke (D)5020um), carbon black 10 parts, a small amount of binder modified pitch (softening point 120 ℃), and carbon nanofibers. Wherein the modified asphalt accounts for the asphalt cokeAnd 80 wt% of the total mass of carbon black; the addition amount of the carbon nano-fiber accounts for 1 wt% of the total mass of the binder asphalt;
the preparation method of the low-dimensional carbon material reinforced carbon graphite material comprises the following steps:
(1) putting the asphalt coke, the carbon black and the carbon nano-fiber into a kneading machine for dry mixing for 1h, then raising the temperature of the kneading machine to 140 ℃ for hot mixing for 1h, then adding the molten modified asphalt with the temperature of about 130 ℃, and continuing wet mixing for 2h, wherein the wet mixing temperature is kept at about 150 ℃;
(2) and (2) drying, crushing, screening (sieving by a 300-mesh sieve), molding (compression molding under 15 MPa) and roasting the paste subjected to wet mixing in the step (1), wherein the roasting curve is the same as that in the example 1, so that the low-dimensional carbon material toughened special carbon graphite material is obtained.
The SEM image of the fracture surface of the low-dimensional carbon material reinforced carbon graphite material prepared in the comparative example is shown in FIG. 2, and it can be observed from FIG. 2 that the micro-area carbon nanofibers of the special low-dimensional carbon material reinforced carbon graphite material prepared in the comparative example are unevenly dispersed and agglomerated, which can cause stress concentration to accelerate crack defect propagation and affect the macroscopic properties of the material.
The low-dimensional carbon material-reinforced carbon graphite material sample in the present comparative example was subjected to a performance test, and the test results are shown in table 2.
TABLE 2 Properties of carbon graphite Material reinforced with Low-dimensional carbon Material of comparative example 1
Comparing the test data in tables 1 and 2, the comprehensive mechanical properties and physical properties of the low-dimensional carbon material reinforced carbon graphite material prepared by the method of the present invention in example 1 are greatly improved and improved compared with the low-dimensional carbon material reinforced carbon graphite material prepared by the conventional preparation method in comparative example 1, the microstructure of the low-dimensional carbon material reinforced carbon graphite material can be effectively improved and the mutual coating effect of the aggregate and the binding property can be improved by adopting the preparation method of the low-dimensional carbon material reinforced carbon graphite material in which the organic solvent is used as the dispersed carbon nanofibers and the mixed aggregate/binder medium, and the uniform dispersion and the micro-domain toughening in the low-dimensional carbon material reinforced carbon graphite material can be promoted. The uniformly dispersed carbon nano-fiber can effectively inhibit the defect expansion and improve the macroscopic performance of the low-dimensional carbon material reinforced carbon graphite material.
Claims (10)
1. A low-dimensional carbon material reinforced carbon graphite material is characterized by comprising the following components which are uniformly dispersed:
aggregate: pitch coke and carbon black;
a low-dimensional carbon material;
adhesive: modified asphalt and/or high temperature asphalt;
dispersing modifier: at least one of tetrahydrofuran, toluene, or quinoline.
2. The low dimensional carbon material-reinforced carbon graphite material as claimed in claim 1, wherein the particle size distribution D of the pitch coke is50The asphalt coke and the carbon black are 85-95 parts by mass of the asphalt coke and 5-15 parts by mass of the carbon black.
3. The low dimensional carbon material-reinforced carbon graphite material according to claim 1, wherein the low dimensional carbon material comprises at least one of carbon nanofibers, carbon nanotubes, or graphene, and the amount of the low dimensional carbon material added is 0.5 to 1.5 wt% based on the total mass of the binder pitch.
4. The low-fiber carbon material-reinforced carbon graphite material as claimed in claim 1, wherein the modified asphalt has a softening point of 120-140 ℃, the high-temperature asphalt has a softening point of 150-170 ℃, and the binder is added in an amount of 70-100 wt% based on the total mass of the aggregate.
5. The low-fiber carbon material-reinforced carbon graphite material as claimed in claim 1, wherein the dispersion modifier is analytically pure and is added in an amount of 300-400 wt% based on the total mass of the binder.
6. A method for preparing the low dimensional carbon material reinforced carbon graphite material as claimed in any one of claims 1 to 5, comprising the steps of:
(1) respectively mixing and stirring a dispersion modifier and a binder, and mixing and stirring the dispersion modifier and a low-dimensional carbon material to obtain two parts of suspension;
(2) and blending the two turbid liquids, adding aggregate, mixing at low temperature, drying, crushing, screening, molding and roasting to obtain the low-dimensional carbon material reinforced carbon graphite material.
7. The method for preparing a low-dimensional carbon material reinforced carbon graphite material as claimed in claim 6, wherein the dispersion modifier is subjected to ultrasonic treatment while being mixed and stirred with the low-dimensional carbon material in the step (1), and the co-treatment time of mechanical stirring and ultrasonic treatment is 20-30 min.
8. The method for preparing a low-dimensional carbon material-reinforced carbon graphite material as claimed in claim 6, wherein the modifier and the binder are stirred for 50-80min in the step (1).
9. The method for preparing the low-dimensional carbon material reinforced carbon graphite material as claimed in claim 6, wherein the suspension in the step (2) is blended for 20-40 min; the low-temperature mixing temperature is 40-60 ℃; the mixing time is 1-2 h.
10. The method for preparing the low-carbon-content material-reinforced carbon graphite material as claimed in claim 6, wherein the sieving mesh in the step (2) is 250-350 mesh.
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