Waste carbon black regeneration method

Abstract

The invention provides a waste carbon black regeneration method, which comprises: S1, drying waste carbon black, adding into a reaction kettle, adding a solvent, sealing the reaction kettle, carrying out a thermal reaction in the solvent at a temperature of 150 DEG C for 8 h, cooling to a room temperature, and standing; and S2, separating the upper-layer solvent after standing in the step S1, carrying out multiple centrifugal washing on the residual lower-layer carbon black solid with distilled water, drying in a drying oven, and calcining at 700-1000 DEG C for 5-8 hours to obtain a regenerated carbon black product. According to the invention, the waste carbon black recovery process is demonstrated in the early stage, the waste carbon black is subjected to a small-scale recovery experiment through the process technologies such as high-temperature calcination, grinding and washing, acid leaching treatment and the like, deep technical research is carried out around the liquid absorption value and the microstructure of the special conductive carbon black for the lithium battery, and the high-performance and low-cost superconducting carbon black is developed; the high liquid absorption value of the conductive carbon black is greater than or equal to 4.0 cm < 3 > / g.

Description

Technical Field

[0001] The present application belongs to the technical field of conductive carbon black preparation, and specifically relates to a method for regenerating waste carbon black. Background Art

[0002] Carbon black, as a carbon-based nano-functional material, is widely used in many industries such as plastics, chemical fibers, inks, rubber, and batteries. However, the recycling of waste carbon black materials is becoming increasingly serious. With the rapid development of the electric vehicle industry and the electronics field, energy storage lithium batteries are particularly important as key components of the industry's power. Superconductive carbon black is an important negative electrode key material that meets the requirements and development trends of the new generation of energy storage lithium batteries. It can increase the conductivity of electrons and lithium ions, accelerate the rate of electron transmission, and has special performance and development prospects. Existing conductive carbon black products used in lithium-ion batteries have problems such as low liquid absorption and unsatisfactory conductive effect. In addition, the production cost is high and the efficiency is low, which has become an important factor restricting the expansion of conductive carbon black production capacity.

[0003] Based on the increasing problems of recycling waste carbon black materials and the requirements for high liquid absorption and high conductivity of superconducting carbon black, how to reduce and modify waste carbon black to prepare superconducting carbon black is a key process technology for achieving low-cost, high added value, sustainable carbon-based materials and large-scale preparation of key negative electrode materials for energy storage lithium batteries. my country's research and development of superconducting carbon black is currently in its infancy, and domestic ordinary conductive carbon black cannot meet the current technical needs of the industrial and electric vehicle markets. Most companies have high costs and low benefits, and high-end products are heavily dependent on imports. Against the background of strong demand for lithium batteries, the industry's supply and demand are tight. According to relevant statistics, my country's imports of conductive carbon black reached 9,300 tons in 2021, and the domestic market maintained rapid growth in 2022, with the demand for conductive carbon black reaching 28,600 tons. Summary of the invention

[0004] The purpose of this application is to provide a method for regenerating waste carbon black to achieve the recovery of waste carbon black.

[0005] In order to achieve the above object, the present application provides a method for regenerating waste carbon black, comprising:

[0006] S1, drying the waste carbon black, then putting it into a reactor, adding a solvent, sealing the reactor, and performing a thermal reaction in a solvent at 150°C for 8 hours, then cooling to room temperature and standing;

[0007] S2. Separate the upper layer solvent after standing in step S1, and wash the remaining lower layer carbon black solid with distilled water by centrifugation for multiple times, dry it in an oven, and then calcine it at 700-1000° C. for 5-8 hours to obtain a regenerated carbon black product.

[0008] In the above scheme, the solvent is at least one of glacial acetic acid, DMF or DMSO.

[0009] In the above scheme, the ratio of waste carbon mass to solvent volume is 35g:65ml.

[0010] In the above scheme, the drying temperature of the waste carbon black in step S1 is 60°C.

[0011] The beneficial effects of this application are:

[0012] The present invention has demonstrated the recovery process of waste carbon black in the early stage, and carried out a small-scale recovery experiment using waste carbon black through high-temperature calcination, grinding, water washing, acid leaching and other process technologies. It has carried out in-depth technical research on the liquid absorption value and microstructure of conductive carbon black for lithium batteries, and developed high-performance, low-cost superconductive carbon black, achieving a high liquid absorption value of conductive carbon black ≥4.0cm 3 / g effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 This is the SEM picture of carbon black: Figure 1 a is the SEM image of the original carbon black without treatment; b is the SEM image of A1; c is the SEM image of A2, and d is the SEM image of A3. DETAILED DESCRIPTION

[0014] The embodiments of the technical solution of the present application will be described in detail below. The following embodiments are only used to more clearly illustrate the technical solution of the present application, and are therefore only used as examples, and cannot be used to limit the protection scope of the present application. In addition, the technical features involved in each embodiment of the present application described below can be combined with each other as long as they do not conflict with each other.

[0015] Example 1

[0016] S1. Weigh 35 g of waste carbon black, dry it in an oven at 60° C., then put it into a 100 mL sealed reactor, add 65 mL of glacial acetic acid, seal the reactor, perform solvent thermal reaction at 150° C. for 8 hours, and cool to room temperature.

[0017] S2. Separate the upper layer of acetic acid in the above step S1, and wash the remaining lower layer of carbon black solid with distilled water by centrifugation for multiple times, dry it in an oven at 90° C., and then calcine it at 900° C. for 6 hours to obtain a regenerated carbon black product A1.

[0018] Example 2

[0019] S1. Weigh 35 g of waste carbon black, dry it in an oven at 60°C, then put it into a 100 mL sealed reactor, add 65 mL of DMF (i.e., N,N-dimethylformamide), seal the reactor, perform solvent thermal reaction at 130°C for 8 hours, and cool to room temperature.

[0020] S2. Separate the upper layer of DMF in the above step S1, and wash the remaining lower layer of carbon black solid with distilled water by centrifugation for multiple times, dry it in an oven at 90° C., and then dry it at 900° C. for 6 hours to obtain a regenerated carbon black product A2.

[0021] Example 3

[0022] S1. Weigh 35 g of waste carbon black, dry it in an oven at 60° C., then put it into a 100 mL sealed reactor, add 65 mL of DMSO (i.e. dimethyl sulfoxide), seal the reactor, perform solvent thermal reaction at 130° C. for 8 hours, and cool to room temperature.

[0023] S2. Separate the upper layer of DMSO in the above step S1, and wash the remaining lower layer of carbon black solid with distilled water by centrifugation for multiple times, dry it in an oven at 90° C., and then dry it at 900° C. for 6 hours to obtain a regenerated carbon black product A3.

[0024] As shown in Table 1, there are significant changes in the data between waste carbon black and treated carbon black, among which the liquid absorption value required by the process has also changed greatly, from no liquid absorption of waste carbon black to about 3.5 after the improvement of this process.

[0025] Table 1 Carbon black test data

[0026]

[0027] like Figure 1 As shown, a is the SEM image of the untreated waste carbon black, b is the SEM image of A1, c is the SEM image of A2, and d is the SEM image of A3. It can be seen from the figure that the particle size of carbon black has changed due to different treatments, which may be partially affected and changed by the grinding process in the treatment step.

[0028] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit it. Although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A method for regenerating waste carbon black, characterized in that: include: S1, drying the waste carbon black, then putting it into a reactor, adding a solvent, sealing the reactor, and performing a thermal reaction in a solvent at 150°C for 8 hours, then cooling to room temperature and standing; S2. Separate the upper layer solvent after standing in step S1, and wash the remaining lower layer carbon black solid with distilled water by centrifugation for multiple times, dry it in an oven, and then calcine it at 700-1000° C. for 5-8 hours to obtain a regenerated carbon black product.

2. The waste carbon black regeneration method according to claim 1, characterized in that: The solvent is at least one of glacial acetic acid, DMF or DMSO.

3. The waste carbon black regeneration method according to claim 1, characterized in that: The ratio of waste carbon mass to solvent volume is 35g:65ml.

4. The waste carbon black regeneration method according to claim 1, characterized in that: The drying temperature of the waste carbon black in step S1 is 60°C.

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