阅读说明：本技术 一种利用常温混捏工艺制备炭素制品的方法 (Method for preparing carbon product by normal-temperature kneading process ) 是由 刘占军 李国栋 于 2020-12-03 设计创作，主要内容包括：本发明涉及一种利用常温混捏工艺制备炭素制品的方法,属于炭素材料制备技术领域,解决炭素制品生产周期长、高能耗和环保的技术问题,本发明包括以下步骤：将骨料破碎后根据粒径进行分级,按产品骨料级配要求配制待混捏骨料备用→将沥青破碎制得沥青粉料→待混捏骨料与沥青粉料混合均匀后加入有机试剂,室温下混捏制得混捏均匀糊料→将制得的糊料在成型设备上成型,制得生坯→将生坯放入炭化炉中,采用常规炭化升温工艺焙烧得到所需炭制品。本发明利用常温混捏工艺制备炭素制品,解决了混捏、成型过程中的高能耗和环境污染问题；降低了对混捏和成型设备的要求,减少了设备投资；同时简化了生产工艺,缩短了生产周期,提高了设备产能。(The invention relates to a method for preparing a carbon product by using a normal-temperature kneading process, belongs to the technical field of preparation of carbon materials, and solves the technical problems of long production period, high energy consumption and environmental protection of the carbon product, and the method comprises the following steps: crushing the aggregate, grading according to the particle size, preparing the aggregate to be kneaded according to the grading requirement of the product aggregate for later use → crushing the asphalt to prepare asphalt powder → mixing the aggregate to be kneaded and the asphalt powder uniformly, adding an organic reagent, kneading at room temperature to prepare a uniformly kneaded paste → molding the prepared paste on molding equipment to prepare a green body → placing the green body into a carbonization furnace, and roasting by adopting a conventional carbonization and temperature rise process to obtain the required carbon product. The carbon product is prepared by using a normal-temperature kneading process, so that the problems of high energy consumption and environmental pollution in the kneading and forming processes are solved; the requirements on kneading and molding equipment are reduced, and the equipment investment is reduced; meanwhile, the production process is simplified, the production period is shortened, and the equipment capacity is improved.)

1. A method for preparing a carbon product by utilizing a normal-temperature kneading process is characterized by comprising the following steps:

s1, crushing the aggregate, grading according to particle size, and preparing the aggregate to be kneaded according to the grading requirement of the product aggregate for later use;

s2, crushing the asphalt until the particle size is 1-200 mu m to obtain asphalt powder;

s3, firstly, adding the asphalt powder prepared in the step S2 and the aggregate to be kneaded prepared in the step S1 into a kneading pot, and kneading to prepare a material mixture, wherein the asphalt powder accounts for 10-35% of the total weight of the material mixture; then, adding an organic reagent into the material mixture, wherein the weight of the organic reagent accounts for 2-25% of the total weight of the material mixture; finally, kneading the organic reagent and the material mixture in a kneading pot for 10-180 min at room temperature to prepare paste with uniform kneading;

s4, molding the paste prepared in the step S3 on a molding device to prepare a green body;

and S5, placing the green body prepared in the step S4 into a carbonization furnace, and roasting by adopting a conventional carbonization and temperature rise process to prepare a carbon product.

2. The method for preparing carbon products by using the normal-temperature kneading process according to claim 1, wherein the method comprises the following steps: in the step S1, the aggregate is one or more of anthracite, petroleum coke, pitch coke, natural graphite, artificial graphite, carbon microspheres, and carbon black.

3. The method for preparing carbon products by using the normal-temperature kneading process according to claim 1, wherein the method comprises the following steps: in the step S2, the softening point of the asphalt is 80-350 ℃.

4. The method for preparing carbon products by using the normal-temperature kneading process according to claim 1 or 3, wherein the method comprises the following steps: the asphalt is one or more of coal asphalt, petroleum asphalt, modified asphalt or mesophase asphalt.

5. The method for preparing carbon products by using the normal-temperature kneading process according to claim 1, wherein the method comprises the following steps: in step S3, the organic reagent is one or more of ketones, lipids, aromatic hydrocarbons or heterocyclic compounds.

6. The method for preparing carbon products by using the normal-temperature kneading process according to claim 1, wherein the method comprises the following steps: in the step S4, the molding method is any one of press molding, vibration molding, extrusion molding, or isostatic pressing.

Technical Field

The invention belongs to the technical field of carbon material preparation, and particularly relates to a method for preparing a carbon product by utilizing a normal-temperature kneading process.

Background

The carbon product has the advantages of light weight, high temperature resistance, ablation resistance, good heat conduction, electric conductivity and mechanical properties, is widely applied to various fields, and is increasingly deeply applied to the aspects of chemical industry, metallurgy, nuclear fusion reactor, electronics and the like. As society progresses, the economic growth mode changes from a rough open type to an intensive type and high technology. The economic growth of high energy consumption and high pollution cannot be suitable for the national conditions of China, the efficiency and the technology are improved, the cost is reduced, the energy consumption is reduced, and no pollution is generated, so that the mainstream of economic development is realized. The traditional carbon product production is a high-energy-consumption and high-pollution mode of hot kneading and hot forming, and has long production period and low efficiency. Therefore, the survival and development of the industry must rely on technological progress to overcome the shortcomings which do not meet the requirements of social development.

In recent years, some innovations have appeared in the field of carbon product preparation, such as: the patent with application number 201710682059.7 'a novel preparation process of a graphite electrode' mainly comprises the following steps: natural graphite and other raw materials → normal temperature mixing → mold filling vacuum → isostatic compaction → solidification → coating → carbonization and sintering → processing and finishing → coating → product. The liquid binding agents such as the liquid modified pitch resin and the furan resin are adopted to realize normal-temperature mixing, the energy consumption of the mixing process is reduced, but the processes of drying the paste and curing the formed blank are added after mixing, so that the energy consumption of production and the volatilization of pollutants are increased to a certain extent, and the production period is prolonged. The problems of long production period, high energy consumption and environmental protection of carbon products are not fundamentally solved.

Disclosure of Invention

In order to overcome the defects of the prior art and solve the technical problems of long production cycle, high energy consumption and environmental protection of carbon products, the invention provides a method for preparing the carbon products by using a normal-temperature kneading process, which is realized by the following ways:

a method for preparing a carbon product by using a normal-temperature kneading process comprises the following steps:

s1, crushing the aggregate, grading according to particle size, and preparing the aggregate to be kneaded according to the grading requirement of the product aggregate for later use;

s2, crushing the asphalt until the particle size is 1-200 mu m to obtain asphalt powder;

s3, firstly, adding the asphalt powder prepared in the step S2 and the aggregate to be kneaded prepared in the step S1 into a kneading pot, and kneading to prepare a material mixture, wherein the asphalt powder accounts for 10-35% of the total weight of the material mixture; then, adding an organic reagent into the material mixture, wherein the weight of the organic reagent accounts for 2-25% of the total weight of the material mixture; finally, kneading the organic reagent and the material mixture in a kneading pot for 10-180 min at room temperature to prepare paste with uniform kneading;

s4, molding the paste prepared in the step S3 on a molding device to prepare a green body;

and S5, placing the green body prepared in the step S4 into a carbonization furnace, and roasting by adopting a conventional carbonization and temperature rise process to prepare a carbon product.

Further, in the step S1, the aggregate is one or more of anthracite, petroleum coke, pitch coke, natural graphite, artificial graphite, carbon microspheres, and carbon black.

Further, in the step S2, the softening point of the asphalt is 80 to 350 ℃.

Further, the asphalt is one or more of coal asphalt, petroleum asphalt, modified asphalt or mesophase asphalt.

Further, in step S3, the organic reagent is one or more of ketones, lipids, aromatic hydrocarbons or heterocyclic compounds.

Further, in the step S4, the molding method is any one of press molding, vibration molding, extrusion molding, or isostatic pressing.

Compared with the prior art, the invention has the beneficial effects that:

1. the carbon product is prepared by utilizing a normal-temperature kneading process, so that hot kneading and hot forming are not needed, and the problems of high energy consumption and environmental pollution in the kneading and forming processes are solved;

2. the normal temperature kneading technology reduces the requirements on kneading and forming equipment and reduces equipment investment;

3. the invention does not need the heating of a kneading pot and a pressing device, the drying of paste and the curing of a formed green body, shortens the production period and improves the productivity of the device.

Detailed Description

The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. Unless otherwise specified, the examples follow conventional experimental conditions. In addition, it will be apparent to those skilled in the art that various modifications or improvements can be made to the material components and amounts in these embodiments without departing from the spirit and scope of the invention as defined in the appended claims.

The heating processes adopted for roasting in the following examples are all as follows:

example 1

A method for preparing a carbon product by utilizing a normal-temperature kneading process is characterized by comprising the following steps:

s1, in the embodiment 1, electrically calcined anthracite is selected as aggregate, the aggregate is crushed and then classified according to the particle size phi of less than or equal to 0.075mm, 0.075mm and less than or equal to 3 mm and less than or equal to 6mm, the aggregate to be kneaded is prepared for later use according to the product aggregate grading requirement, in the embodiment 1, powder with the phi of less than or equal to 0.075mm accounts for 40% of the total weight of the aggregate, particle material with the phi of more than 0.075mm and less than or equal to 3 accounts for 30% of the total weight of the aggregate, and particle material with the phi of more than 3 and;

s2, crushing the asphalt until the particle size is less than or equal to 100 mu m, and the softening point of the asphalt is 80 ℃ to obtain asphalt powder;

s3, firstly, adding the asphalt powder prepared in the step S2 and the aggregate to be kneaded prepared in the step S1 into a kneading pot, and kneading for 0.5h to prepare a material mixture, wherein the asphalt powder accounts for 10% of the total weight of the material mixture; then, adding an organic reagent to the material mixture, wherein the weight of the organic reagent accounts for 2% of the total weight of the material mixture, and quinoline is selected as the organic reagent in example 1; finally, mixing and kneading the organic reagent and the material mixture in a mixing and kneading pot for 180min at room temperature to prepare paste with uniform mixing and kneading;

s4, performing compression molding on the paste prepared in the step S3 in a molding device to prepare a green body;

s5, placing the green body prepared in the step S4 into a well type carbonization furnace, roasting to obtain a carbon block by adopting the temperature rising process shown in the table 1, wherein the highest roasting temperature is 1000 ℃, and performing performance detection on the carbon block, wherein the detection result is shown in the table 2.

Example 2

A method for preparing a carbon product by utilizing a normal-temperature kneading process is characterized by comprising the following steps:

s1, selecting calcined petroleum coke as an aggregate in the embodiment 2, crushing the aggregate, grading according to the particle size phi of less than or equal to 0.075mm, 0.075mm and less than or equal to 3 mm and less than or equal to 6mm, and preparing the aggregate to be kneaded according to the product aggregate grading requirement for later use, wherein in the embodiment 2, powder with the phi of less than or equal to 0.075mm accounts for 40% of the total weight of the aggregate, particles with the phi of more than 0.075mm and less than or equal to 3 account for 30% of the total weight of the aggregate, and particles with the phi of more than 3 and less than or equal;

s2, crushing the asphalt until the particle size is less than or equal to 120 mu m and the softening point of the asphalt is 100 ℃ to obtain asphalt powder;

s3, firstly, adding the asphalt powder prepared in the step S2 and the aggregate to be kneaded prepared in the step S1 into a kneading pot, and kneading for 0.5h to prepare a material mixture, wherein the asphalt powder accounts for 17% of the total weight of the material mixture; then, adding an organic reagent to the material mixture, wherein the weight of the organic reagent accounts for 3% of the total weight of the material mixture, and pyridine is selected as the organic reagent in this example 2; finally, kneading the organic reagent and the material mixture in a kneading pot for 120min at room temperature to prepare paste which is uniformly kneaded;

s4, vibrating and molding the paste prepared in the step S3 on a molding device to prepare a green body;

s5, placing the green body prepared in the step S4 into a well type carbonization furnace, roasting to obtain a carbon block by adopting the temperature rising process shown in the table 1, wherein the highest roasting temperature is 1000 ℃, and performing performance detection on the carbon block, wherein the detection result is shown in the table 2.

Example 3

A method for preparing a carbon product by utilizing a normal-temperature kneading process is characterized by comprising the following steps:

s1, selecting calcined asphalt coke as aggregate in the embodiment 3, classifying the crushed aggregate according to the particle size phi of less than or equal to 0.075mm, phi of more than 0.075mm and less than or equal to 3, and phi of more than 3 and less than or equal to 6mm, preparing the aggregate to be kneaded according to the product aggregate grading requirement for later use, wherein in the embodiment 3, the powder with the phi of less than or equal to 0.075mm accounts for 40% of the total weight of the aggregate, the particle material with the phi of more than 0.075mm and less than or equal to 3 accounts for 30% of the total weight of the aggregate, and the particle material with the phi of more;

s2, crushing the asphalt until the particle size is less than or equal to 150 mu m and the softening point of the asphalt is 120 ℃ to obtain asphalt powder;

s3, firstly, adding the asphalt powder prepared in the step S2 and the aggregate to be kneaded prepared in the step S1 into a kneading pot, and kneading for 0.5h to prepare a material mixture, wherein the asphalt powder accounts for 20% of the total weight of the material mixture; then, adding an organic reagent to the material mixture, wherein the weight of the organic reagent accounts for 5% of the total weight of the material mixture, and the organic reagent in this example 3 is octyl pyrrolidone; finally, kneading the organic reagent and the material mixture in a kneading pot for 90min at room temperature to prepare paste with uniform kneading;

s4, carrying out extrusion forming on the paste prepared in the step S3 on forming equipment to prepare a green body;

s5, placing the green body prepared in the step S4 into a well type carbonization furnace, roasting to obtain a carbon block by adopting the temperature rising process shown in the table 1, wherein the highest roasting temperature is 1000 ℃, and performing performance detection on the carbon block, wherein the detection result is shown in the table 2.

Example 4

A method for preparing a carbon product by utilizing a normal-temperature kneading process is characterized by comprising the following steps:

s1, selecting calcined asphalt coke as aggregate in the embodiment 4, classifying the crushed aggregate according to the particle size phi of less than or equal to 0.075mm, 0.075mm and less than or equal to 3 mm and less than or equal to 6mm, preparing the aggregate to be kneaded according to the product aggregate grading requirement for later use, wherein in the embodiment 4, asphalt coke powder with the phi of less than or equal to 0.075mm accounts for 35% of the total weight of the aggregate, natural graphite powder with the phi of less than or equal to 0.075mm accounts for 5% of the total weight of the aggregate, granular material with the phi of less than or equal to 3 mm accounts for 30% of the total weight of the aggregate, and granular material with the phi of less than or equal to;

s2, crushing the asphalt until the particle size is less than or equal to 180 mu m, and the softening point of the asphalt is 200 ℃ to obtain asphalt powder;

s3, firstly, adding the asphalt powder prepared in the step S2 and the aggregate to be kneaded prepared in the step S1 into a kneading pot, and kneading for 0.5h to prepare a material mixture, wherein the asphalt powder accounts for 28% of the total weight of the material mixture; then, adding an organic reagent to the material mixture, wherein the weight of the organic reagent accounts for 12% of the total weight of the material mixture, and the organic reagent in this example 4 is toluene; finally, mixing and kneading the organic reagent and the material mixture in a mixing and kneading pot for 60min at room temperature to prepare paste with uniform mixing and kneading;

s4, isostatic pressing the paste prepared in the step S3 on a forming device to prepare a green body;

s5, placing the green body prepared in the step S4 into a well type carbonization furnace, roasting to obtain a carbon block by adopting the temperature rising process shown in the table 1, wherein the highest roasting temperature is 1000 ℃, and performing performance detection on the carbon block, wherein the detection result is shown in the table 2.

Example 5

A method for preparing a carbon product by utilizing a normal-temperature kneading process is characterized by comprising the following steps:

s1, in the embodiment 4, electrically calcined anthracite is selected as aggregate, the aggregate is crushed and classified according to the particle size phi of less than or equal to 0.075mm, 0.075mm and less than or equal to 3 mm and less than or equal to 6mm, the aggregate to be kneaded is prepared for later use according to the product aggregate grading requirement, in the embodiment 5, powder with the phi of less than or equal to 0.075mm accounts for 40% of the total weight of the aggregate, particle material with the phi of more than 0.075mm and less than or equal to 3 accounts for 30% of the total weight of the aggregate, and particle material with the phi of more than 3 and less;

s2, crushing the asphalt until the particle size is less than or equal to 200 mu m and the softening point of the asphalt is 350 ℃ to obtain asphalt powder;

s3, firstly, adding the asphalt powder prepared in the step S2 and the aggregate to be kneaded prepared in the step S1 into a high-speed mixer, and kneading for 0.5h to prepare a material mixture, wherein the asphalt powder accounts for 35% of the total weight of the material mixture; then, adding an organic reagent to the material mixture, wherein the weight of the organic reagent accounts for 25% of the total weight of the material mixture, and the organic reagent in this example 5 is dimethyl carbonate; finally, kneading the organic reagent and the material mixture in a kneading pot for 10min at room temperature to prepare paste with uniform kneading;

s4, performing compression molding on the paste prepared in the step S3 in a molding device to prepare a green body;

s5, placing the green body prepared in the step S4 into a well type carbonization furnace, roasting to obtain a carbon block by adopting the temperature rising process shown in the table 1, wherein the highest roasting temperature is 1000 ℃, and performing performance detection on the carbon block, wherein the detection result is shown in the table 2.

The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.