Preparation method of pitch-based carbon fiber carbon-carbon solid felt

Abstract

The invention discloses a pitch-based carbon fiber carbon-carbon solid felt preparation method, which comprises: S1, fumigating a carbon fiber felt in a closed environment by using water vapor with a pressure of 2.4-2.6 MPa and a temperature of 850-900 DEG C for half an hour, airing the fumigated carbon fiber felt to a normal temperature, and soaking in a graphene oxide dispersion liquid for 10 min to obtain an activated carbon fiber felt; s2, the activated carbon fiber felt is soaked in a water-soluble phenolic resin solution to be soaked for 20 minutes, and a resin-coated carbon fiber soft felt is obtained.The method relates to the technical field of carbon fiber product processing, the activated carbon fiber felt is soaked in a graphene oxide dispersion solution to be subjected to secondary activation treatment, the surface of graphene oxide is rich in functional groups, and the surface of the graphene oxide is rich in functional groups; the active groups can form strong interaction with the carbon fibers, so that the adhesive force between the carbon fibers and a polymer matrix is improved; meanwhile, the graphene oxide is grafted to the surfaces of the carbon fibers to form a lubricating layer, so that friction among the fibers is reduced, and the agglomeration phenomenon in the processing process of the composite material is avoided.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of carbon fiber product processing, in particular to a preparation method of pitch-based carbon fiber carbon carbon felt. BACKGROUND

[0002] Pitch-based carbon fiber is a kind of special fiber with carbon content greater than 92% which is made of petroleum pitch or coal tar pitch as raw material, through refining, spinning, pre-oxidation, carbonization or graphitization of pitch. Carbon fiber has the characteristics of corrosion resistance, high strength, high modulus, low density, high specific performance, no creep, good fatigue resistance and other characteristics in non-oxidizing environment, is a new material with excellent mechanical properties. The existing carbon fiber material is generally activated first, then immersed in resin material, and finally heat pressed and cured to obtain cured carbon fiber felt. However, the carbon fiber felt activated by water vapor has a large and more friction between the fibers, and when immersed in the resin solution, agglomeration occurs, which makes the resin material on the carbon fiber felt uneven, resulting in uneven quality of the subsequent cured carbon fiber felt. SUMMARY

[0003] In view of the shortcomings of the prior art, the present application provides a preparation method of pitch-based carbon fiber carbon carbon felt, which solves the problem that the existing carbon fiber felt will agglomerate during the curing process, affecting the production quality of the cured carbon fiber felt.

[0004] To achieve the above purpose, the present application realizes the following technical scheme: a preparation method of pitch-based carbon fiber carbon carbon felt, comprising the following steps: S1: carbon fiber felt is smoked with water vapor at 2.4-2.6 MPa and 850-900 DEG C for half an hour in a closed environment, and then the smoked carbon fiber felt is air-dried to room temperature and soaked in graphene oxide dispersion liquid for 10 minutes to obtain activated carbon fiber felt; S2: the activated carbon fiber felt is soaked in water-soluble phenolic resin solution for 20 minutes to obtain resin-coated carbon fiber soft felt; S3: the resin-coated carbon fiber soft felt is heat pressed and cured at a temperature of 180 DEG C to 200 DEG C for 1 hour to obtain cured carbon fiber felt; S4: a mixture of adhesive phenolic resin solution and graphene oxide suspension is coated on the surface of the cured carbon fiber felt, and sintered in a vacuum high-temperature furnace to obtain pitch-based carbon fiber carbon carbon felt.

[0005] Preferably, the adhesive phenolic resin solution contains water-soluble phenolic resin, active agent, thickening agent and viscous agent.

[0006] Preferably, the vacuum high-temperature furnace has a vacuum degree of ≤ 150 Pa and a sintering temperature of 1350-1450℃.

[0007] The present application provides a pitch-based carbon fiber carbon carbon felt preparation method, has the following beneficial effects: The fumigated and activated carbon fiber felt is soaked in the graphene oxide dispersion solution for secondary activation treatment, the graphene oxide surface is rich in oxygen-containing functional groups such as epoxy, hydroxyl and carbonyl, these active groups can form strong interaction with the carbon fiber, significantly improving the adhesion of the carbon fiber and the polymer matrix (such as epoxy resin); meanwhile, the graphene oxide is grafted to the carbon fiber surface to form a lubricating layer, reducing the friction between the fibers and avoiding the aggregation phenomenon in the composite material processing; and the modified carbon fiber can maintain high strength characteristics in the composite material, and the tensile strength, elongation at break and overall toughness are improved through the enhancement of the graphene oxide.

[0008] The cured carbon fiber felt obtained below the conventional curing processing temperature and time has lower performance than the cured carbon fiber felt obtained through conventional curing processing, but can be endowed with secondary processing performance; through the operation of coating the mixed solution of the adhesive phenolic resin solution and the graphene oxide suspension and finally sintering, the pitch-based carbon fiber carbon carbon felt with better performance is obtained, effectively improving the strength and overall service life of the cured carbon fiber felt. DETAILED DESCRIPTION

[0009] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0010] The present application provides a technical solution: a pitch-based carbon fiber carbon carbon felt preparation method, comprising the following steps: S1: carbon fiber felt is fumigated with water vapor at 2.4-2.6 MPa and 850-900℃ for half an hour in a closed environment, and then the fumigated carbon fiber felt is air-dried to room temperature and soaked in a graphene oxide dispersion solution for 10 minutes to obtain activated carbon fiber felt; S2: the activated carbon fiber felt is soaked in a water-soluble phenolic resin solution for 20 minutes to obtain resin-coated carbon fiber soft felt; S3: the resin-coated carbon fiber soft felt is subjected to heat pressing and curing treatment, the heat pressing and curing temperature is 180-200℃, and the time is 1 hour to obtain cured carbon fiber felt; S4: coating the surface of the cured carbon fiber felt with a mixture of the viscous phenolic resin solution and the graphene oxide suspension, sintering in a vacuum high-temperature furnace, and obtaining the pitch-based carbon fiber carbon-carbon solid felt after completion; The main effects of the carbon fiber soaking in the graphene oxide dispersion solution include surface modification, enhanced interfacial bonding, improved dispersibility, and improved composite material performance. The modified carbon fiber can maintain high strength characteristics in the composite material, and the tensile strength, elongation at break, and overall toughness can be improved through the enhancement of the graphene oxide. The soaking method is simple to operate, low in energy consumption, easy to scale up, and meets the green environmental protection requirements. The heat pressing and curing temperature and time are lower than the conventional curing temperature and time, so that the processed cured carbon fiber felt is an incomplete cured carbon fiber felt, which leaves room for subsequent coating and sintering processing.

[0011] Further, the viscous phenolic resin solution contains water-soluble phenolic resin, active agent, thickening agent, and viscous agent.

[0012] Further, the vacuum degree of the vacuum high-temperature furnace is ≤150 Pa, and the sintering temperature is 1350-1450℃.

[0013] By the skilled in the art, the raw materials in the case are processed in sequence, and the specific processing and operation sequence should be referred to the following working principle, and the detailed connection means is the known technology in the art, and the following mainly introduces the working principle and process.

[0014] Embodiment: First, the carbon fiber felt is smoked with 2.4-2.6 MPa, 850-900℃ steam in a sealed environment for half an hour, and then the smoked carbon fiber felt is air-dried to room temperature and soaked in the graphene oxide dispersion solution for 10 minutes to obtain the activated carbon fiber felt. Second, the activated carbon fiber felt is soaked in the water-soluble phenolic resin solution for 20 minutes to obtain the resin-coated carbon fiber soft felt. Then, the resin-coated carbon fiber soft felt is heat pressed and cured at a temperature of 180-200℃ for 1 hour to obtain the cured carbon fiber felt. Finally, the surface of the cured carbon fiber felt is coated with a mixture of the viscous phenolic resin solution and the graphene oxide suspension, sintered in a vacuum high-temperature furnace, and the pitch-based carbon fiber carbon-carbon solid felt is obtained after completion.

[0015] It has to be noted that, in the present document, the terms "first", "second", etc. merely serve to identify different entities or actions and do not necessarily require or imply any actual relationship or order between these entities or actions. Moreover, the terms "comprises", "comprising", or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but can include other elements not expressly listed or inherent to such process, method, article, or apparatus. In other words, without further restriction, reference to elements will not, without more limitations, exclude additional, unrecited elements of a process, method, article, or apparatus.

[0016] While embodiments of the application have been shown and described, it is to be understood that the application is not limited to the details of the embodiments described, since numerous modifications and changes can be made to the embodiments without departing from the spirit and scope of the application as defined by the appended claims and their equivalents.

Claims

1. A method for preparing pitch-based carbon fiber carbon-carbon solid felt, characterized in that, Includes the following steps: S1: The carbon fiber felt is fumigated in a closed environment with water vapor at 2.4-2.6MPa and 850-900℃ for half an hour. After the fumigated carbon fiber felt is dried to room temperature, it is soaked in graphene oxide dispersion for 10 minutes to obtain activated carbon fiber felt. S2: The activated carbon fiber felt is immersed in a water-soluble phenolic resin solution for 20 minutes to obtain resin-coated carbon fiber soft felt. S3: The resin-coated carbon fiber felt is subjected to hot-press curing treatment at a temperature of 180℃~200℃ for 1 hour to obtain cured carbon fiber felt. S4: A mixture of viscous phenolic resin solution and graphene oxide suspension is coated on the surface of the cured carbon fiber felt, and then sintered in a vacuum high-temperature furnace to obtain pitch-based carbon fiber carbon-carbon solid felt.

2. The method for preparing pitch-based carbon fiber carbon-carbon solid felt according to claim 1, characterized in that, The viscous phenolic resin solution contains water-soluble phenolic resin, activator, thickener, and viscous agent.

3. The method for preparing pitch-based carbon fiber carbon-carbon solid felt according to claim 1, characterized in that, The vacuum high-temperature furnace has a vacuum degree of ≤150Pa and a sintering temperature of 1350℃~1450℃.