CN111453714A - Treatment method for improving specific surface area of carbon material - Google Patents

Treatment method for improving specific surface area of carbon material Download PDF

Info

Publication number
CN111453714A
CN111453714A CN202010424234.4A CN202010424234A CN111453714A CN 111453714 A CN111453714 A CN 111453714A CN 202010424234 A CN202010424234 A CN 202010424234A CN 111453714 A CN111453714 A CN 111453714A
Authority
CN
China
Prior art keywords
carbon material
surface area
specific surface
flue gas
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.)
Pending
Application number
CN202010424234.4A
Other languages
Chinese (zh)
Inventor
王建国
李岩峰
孔祥宇
宋鑫
张乐乐
杨骏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang University of Technology ZJUT
Original Assignee
Zhejiang University of Technology ZJUT
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Zhejiang University of Technology ZJUT filed Critical Zhejiang University of Technology ZJUT
Priority to CN202010424234.4A priority Critical patent/CN111453714A/en
Publication of CN111453714A publication Critical patent/CN111453714A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/05Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

The invention discloses a treatment method for improving the specific surface area of a carbon material, which comprises the steps of placing the carbon material in a tubular furnace, introducing mixed gas of flue gas and air with the volume ratio of 0.2-5: 1, carrying out heat treatment at the temperature of 250-450 ℃ for 0.5-4h, taking out the heat-treated carbon material, washing with water, and drying to obtain a carbon material product with high specific surface area. The specific surface area of the carbon material treated by the method can be fully improved, in addition, the preparation process of the method has the advantages of simple process steps, short reaction time and the like, and meanwhile, the carbon material and the flue gas in the method are wide in source, low in price and low in equipment requirement, and are suitable for industrial large-scale production.

Description

Treatment method for improving specific surface area of carbon material
Technical Field
The invention relates to a treatment method for improving the specific surface area of a carbon material.
Background
Nowadays, with the development of social industry and economy, the automobile industry is continuously developed and strengthened, and the number of tire enterprises which are in charge of running is increased, so that waste tires called black pollution cause serious pollution to the environment, and meanwhile, improper treatment also causes serious waste of resources, so that the scrapping of automobile tires promotes the diversified development of the rubber regeneration processing industry.
The common method for recycling the waste tires comprises the steps of manufacturing the waste tires into reclaimed rubber or retreading the waste tires. But the performance of the reclaimed rubber is lower, the global consciousness of security is gradually improved in recent years, and the reclaimed rubber industry shows a plurality of disadvantages, such as excessive energy consumption, complex process, secondary pollution caused by waste water, waste residue and the like generated in the production process; the method has the limitations of tire retreading, has higher requirements on waste tires, requires that the tire body is complete and not damaged, and has limited retreading times, thus leading to that few enterprises are engaged in the waste tire retreading industry in China.
The pyrolysis technology of the waste tires becomes one of the most effective waste tire treatment technologies at present, and the pyrolysis carbon black is one of pyrolysis products of the waste tires, is derived from various carbon blacks added in the tire processing process, and accumulates and deposits along with the decomposition of rubber macromolecules during pyrolysis and is collected. The waste tire pyrolysis solves the danger and harm caused by waste tire accumulation, the waste tire can recover combustible gas, oil and pyrolytic carbon black through pyrolysis, the pyrolytic carbon black is a key product of tire pyrolysis, and the quality and market application of the pyrolytic carbon black restrict the economy of the waste tire pyrolysis recovery process. The pyrolysis technology not only solves the problem of black pollution, but also recovers valuable chemicals, so that secondary pollution can not be generated, the waste rubber is thoroughly regenerated, and all products are recovered as materials to be effectively reused.
Therefore, how to improve the performance of the tire pyrolytic carbon black, improve the use value of the tire pyrolytic carbon black and scientifically represent the performance of the pyrolytic carbon black is an important link for the comprehensive utilization of waste tire resources.
Residual materials or plant residues in agriculture, forestry and breeding industries such as sawdust, straws, livestock and poultry manure and the like are biomass raw materials, and the biomass raw materials are pyrolyzed under the high-temperature nitrogen atmosphere to obtain a black stable high-carbon-content solid compound, namely the biochar. The biochar is a cheap and efficient adsorbent, is widely applied to the fields of soil improvement, carbon dioxide sequestration, environmental remediation, resource recycling and the like, but the application value of the biochar is directly related to the specific surface area of the biochar, but the specific surface area of the initial carbon-containing solid compound obtained by pyrolysis is slightly lower, and further processing and improvement are needed.
Flue gas is a gaseous substance which is produced by burning fossil fuels such as coal and pollutes the environment. As these materials are typically exhausted from a flue or stack. The flue gas generation process is mostly caused by incomplete combustion due to insufficient utilization of fuel. Because of its higher temperature, it can be used as heat carrier for high-temperature reaction (600-700 deg.C). The flue gas is usually treated by a gas purification device and then discharged directly from the plant. The actual flue gas to be cleaned and evacuated generally has a volume content composition of: 40-62% of nitrogen, 30-50% of carbon dioxide, 2-10% of oxygen, 5-15% of water vapor, a very small amount of sulfide and the like, wherein inorganic pollutants account for more than 99%; the content of dust, powder slag and sulfur dioxide is less than 1 percent. Although the flue gas is purified and emptied, the direct discharge thereof causes environmental pollution and wastes resources.
In view of the technical background, the invention takes the cheap cracking carbon black and the biochar with lower added value as raw materials to fully utilize the flue gas to obtain the carbon material with higher specific surface area, and has great environmental protection significance and economic significance.
Disclosure of Invention
Aiming at the technical defects in the existing carbon material processing process, the application provides a treatment method capable of improving the specific surface area of a carbon material, and the treatment method is used for improving the additional value of the carbon material and the effective waste gas utilization of flue gas.
The treatment method for improving the specific surface area of the carbon material is characterized by comprising the following steps of: placing the carbon material in a tubular furnace, introducing mixed gas of flue gas and air with the volume ratio of 0.2-5: 1, carrying out heat treatment at the temperature of 250-450 ℃ for 0.5-4h, taking out the heat-treated carbon material, washing with water, and drying to obtain the carbon material product with high specific surface area.
The treatment method for improving the specific surface area of the carbon material is characterized by comprising the following steps of: the heat treatment temperature is 300-400 ℃, and the treatment time is 1-3 h.
The treatment method for improving the specific surface area of the carbon material is characterized by comprising the following steps of: the volume ratio of flue gas to air in the mixed gas introduced into the tubular furnace is 0.3-3: 1.
The treatment method for improving the specific surface area of the carbon material is characterized in that the volume flow of the mixed gas of the introduced flue gas and air is 30-60m L/h, preferably 40-50m L/h based on 1g of the carbon material subjected to heat treatment.
The treatment method for improving the specific surface area of the carbon material is characterized by comprising the following steps of: the carbon material is carbon black generated by rubber cracking or biochar generated by biomass pyrolysis.
The treatment method for improving the specific surface area of the carbon material is characterized by comprising the following steps of: the main components of the flue gas comprise carbon dioxide and nitrogen, wherein the volume ratio of the carbon dioxide to the nitrogen is 0.3-3: 1, and 1:1 is preferred.
The carbon material is tire cracking carbon black or biochar, and the preparation method of the tire cracking carbon black comprises the following steps: taking waste tires as raw materials, thermally cracking for 2-5 hours at the temperature of 600 ℃ in a thermal cracking reactor under the environment of isolating air (oxygen deficiency or inert gas atmosphere), discharging a mixture of carbon slag and steel wire scrap iron impurities from the thermal cracking reactor, and removing the steel wire scrap iron impurities through a magnetic separation iron removal process to form crude carbon black; and (3) milling the crude carbon black by a carbon black pulverizer, washing with water, and drying to obtain the carbon black product.
The preparation method of the biochar comprises the following steps: residual materials or plant residues of agriculture, forestry and breeding industries such as wood chips, straws, livestock and poultry manure and the like are used as raw materials, and the black stable high-carbon-content solid compound is obtained after thermal cracking for 2 to 5 hours at the temperature of 500-600 ℃ in the nitrogen atmosphere.
Compared with the prior art, the invention has the following beneficial effects:
1) according to the method, the carbon material is subjected to heat treatment in the mixed gas of the flue gas and the air, and by controlling the composition and the flow rate of the mixed gas, on one hand, oxygen contained in the mixed gas generates an oxidation reaction on the surface of the carbon material in the heat treatment process in the tubular furnace, and existing surface micropores are enlarged, so that the specific surface area is increased; on the other hand, unoxidized organic residues in the carbon material are also oxidized.
2) In the application, the cracking carbon black which is one of the carbon materials is derived from waste tires, so that the black pollution is solved, and the valuable cracking carbon black is recovered.
3) In the application, the biochar which is one of the carbon materials is obtained by pyrolyzing the residual materials or plant residues in agriculture, forestry and breeding industries such as sawdust, straws, livestock and poultry manure and the like under the atmosphere of high-temperature nitrogen, and the specific surface area of the biochar is improved after the biochar is subjected to heat treatment, so that the applicability and the applicable aspect are greatly improved.
4) In the application, the flue gas is used as harmful factory waste gas, and the heat and CO contained in the flue gas can be effectively further utilized after the flue gas is treated by the gas purification device2、N2And O2And the like, not only reduces the emission of atmospheric pollutants, but also realizes the reutilization of waste gas, and closely responds to the national environmental protection policy.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Comparative example 1: preparation of waste tyre cracking carbon black by conventional method
Taking 500g of waste tires as raw materials, placing the raw materials in a pyrolysis reactor, carrying out heat preservation treatment for 2 hours at the final pyrolysis temperature of 500 ℃ to carry out carbonization process treatment, and discharging a mixture of carbon slag and steel wire scrap iron impurities from the pyrolysis reactor. Removing impurities of the steel wire scrap iron by a magnetic separation iron removal process of the mixture of the carbon slag and the steel wire scrap iron impurities to form coarse carbon black; and carrying out superfine grinding on the crude carbon black by a carbon black grinder until the crude carbon black meets the granularity similar to that of the industrial carbon black, and forming fine carbon black. Washing with water, drying at 120 deg.C to obtain 95g waste tyre cracking carbon black, and the specific surface area of the finally obtained waste tyre cracking carbon black is about 69.6m2The sample number is 0/g. In the following examples, comparative experiments were conducted using the waste tire cracking carbon black obtained in comparative example 1 as a treatment object.
Examples 1 to 9: the improvement of the specific surface area of the carbon material due to the composition of different mixed gases during heat treatment affects CO2And N2Mixing according to the volume ratio of 1:1, and preparing a simulation in advanceFlue gas.
Taking 1g of carbon black in comparative example 1, placing the carbon black in a tubular furnace (the model of the tubular furnace is phi 6cm × 50cm, the volume of the furnace tube is 1.4L), mixing simulated flue gas and air according to the volume ratio of 1: 5-5: 1 by using a three-way valve, introducing the mixture into the tubular furnace, controlling the total flow of the mixed gas to be 50m L/min, heating to 400 ℃, then preserving heat for 4 hours, taking out the carbon material in the tubular furnace after the heat preservation is finished, cleaning the carbon material with deionized water, drying the carbon material at 80 ℃ to obtain a treated carbon material, and testing the specific surface area of a sample by using a specific surface area analyzer2Isothermal adsorption data are measured under 77K for adsorbates, the BET method is adopted to calculate the total specific surface area of the sample, and then the actual specific surface area increase rate of the method is calculated.
In various examples, the results of the test parameters for simulating the volume ratio of flue gas to air and finally obtaining the carbon material product are shown in Table 1.
TABLE 1 BET values and lift ratios of carbon materials at different volume ratios of air to simulated flue gas
Figure BDA0002498069240000061
According to the results in table 1, the specific surface area of the obtained carbon material is increased with the increase of the proportion of air in the mixed gas under the same other treatment conditions, which indicates that the oxygen in the air generates ablation reaction on the surface of the carbon material, so that new pores are formed in the carbon material, thereby increasing the specific surface area, and also indicates that it is feasible to increase the specific surface area of the carbon material under the heat treatment conditions by mixing the flue gas and the air. When the simulated flue gas to air volume ratio is 4: at 5, the specific surface area of the carbon material reaches the maximum value of 347.6m2However, as the air content continues to rise, the specific surface area is found to decrease, indicating that the ablation reaction is already at an excessive level and is not suitable for pore expansion of the carbon material. When the volume ratio of the flue gas to the air is 5:1, the specific surface area drops sharply, at which point the carbon material is expected to have been severely oxidatively ablated.
Examples 10 to 16: influence of flow of mixed gas on improvement of specific surface area of carbon material
Introducing CO2And N2Mixing according to the volume ratio of 1:1, and preparing a simulated flue gas in advance.
Taking 1g of carbon black in comparative example 1, placing the carbon black in a tubular furnace (the model of the tubular furnace is phi 6cm × 50cm, the volume of the furnace tube is 1.4L), mixing simulated flue gas and air according to the volume ratio of 1:1 by using a three-way valve, introducing the mixture into the tubular furnace, controlling the total flow of the mixed gas within the range of 20-80m L/min, heating to 400 ℃, keeping the temperature for 4h, taking out the carbon material in the tubular furnace after the heat preservation is finished, cleaning the carbon material with deionized water, drying the carbon material at 80 ℃ to obtain a treated carbon material, and testing the specific surface area of a sample by using a specific surface area analyzer2Isothermal adsorption data are measured under 77K for adsorbates, the BET method is adopted to calculate the total specific surface area of the sample, and then the actual specific surface area increase rate of the method is calculated.
In different embodiments, the flow rate of the mixed gas and the results of the specific parameters of the finally prepared carbon material product are shown in table 2.
Table 2: carbon material BET value and lifting rate thereof of mixed gas at different flow rates
Figure BDA0002498069240000071
According to the data in Table 2, when other treatment conditions are the same, only the flow rate of the introduced mixed gas is changed as a unique change amount, as the flow rate of the introduced mixed gas is increased, the ablation degree of the oxygen in the mixed gas on the carbon material is gradually enhanced, the BET (BET area) lifting rate of the carbon material is gradually increased from 204.71% to 490.57% along with the increase of the flow rate, the effect is most obvious when the flow rate of the introduced mixed gas is 60m L/min, and as the flow rate is continuously increased, the ablation degree of the mixed gas on the carbon material is in an excessive degree, according to the data in Table 2, when the flow rate of the mixed gas is 50-60m L/min, the specific surface area of the obtained carbon material can reach 300m2More than g.
Examples 17 to 23: effect of pyrolysis temperature on increasing specific surface area of carbon material
Introducing CO2And N2Mixing according to the volume ratio of 1:1, and preparing a simulated flue gas in advance.
Taking 1g of carbon black in comparative example 1, placing the carbon black in a tubular furnace (the model of the tubular furnace is phi 6cm × 50cm, the volume of the furnace tube is 1.4L), mixing simulated flue gas and air according to the volume ratio of 1:1 by using a three-way valve, introducing the mixture into the tubular furnace, controlling the total flow of the mixed gas within the range of 50m L/min, heating to the pyrolysis temperature, keeping the temperature for 4h, taking out the carbon material in the tubular furnace after the heat preservation is finished, cleaning the carbon material with deionized water, drying the carbon material at 80 ℃ to obtain the treated carbon material, testing the specific surface area of a sample by using a specific surface area analyzer2Isothermal adsorption data are measured under 77K for adsorbates, the BET method is adopted to calculate the total specific surface area of the sample, and then the actual specific surface area increase rate of the method is calculated.
In various examples, the results of the pyrolysis temperature and the specific parameters of the final carbon material product are shown in Table 3.
Table 3: carbon material BET value and lifting rate thereof at different pyrolysis temperatures of tubular furnace
Figure BDA0002498069240000081
From the result data in Table 3, when the heat treatment temperature was 250 ℃, the BET was found to be substantially unchanged within the average value, so that it can be concluded that the mixed gas had substantially no effect on the carbon material when the heat treatment temperature was 250 ℃. However, as the temperature rises, the action of the mixed gas on the carbon material gradually becomes prominent, the optimum condition is reached at 400 ℃, but the excessive ablation phenomenon can occur as the temperature continues to rise, and when the temperature reaches 450 ℃, the carbon material is seriously and excessively ablated, so that the structural collapse of the carbon material is caused, the carbon material is completely oxidized to be gray, and the experimental significance is lost.
Examples 24 to 28: simulating the effect of the volume ratio of carbon dioxide and nitrogen in the flue gas on the increase of the specific surface area of the carbon material
Introducing CO2And N2Mixing was performed, with a simulated flue gas being pre-formulated. And controlling the volume ratio of carbon dioxide to nitrogen in the simulated flue gas to be within the range of 0.3: 1-3: 1.
Taking 1g of carbon black in comparative example 1, placing the carbon black in a tubular furnace (the model of the tubular furnace is phi 6cm × 50cm, the volume of the furnace tube is 1.4L), mixing simulated flue gas and air according to the volume ratio of 1:1 by using a three-way valve, introducing the mixture into the tubular furnace, controlling the total flow of the mixed gas to be 50m L/min, heating to the pyrolysis temperature, keeping the temperature for 4h, taking out the carbon material in the tubular furnace after the heat preservation is finished, cleaning the carbon material with deionized water, drying the carbon material at 80 ℃ to obtain the treated carbon material, and testing the specific surface area of a sample by using a specific surface area analyzer according to a testing method commonly used in the industry2Isothermal adsorption data are measured under 77K for adsorbates, the BET method is adopted to calculate the total specific surface area of the sample, and then the actual specific surface area increase rate of the method is calculated.
In various examples, the results of the volume ratios of carbon dioxide and nitrogen in the simulated flue gas and the specific parameters of the tests for the final carbon material product are shown in Table 4.
Table 4: carbon material BET value and lifting rate thereof in different volume ratios of carbon dioxide to nitrogen in tubular furnace
Figure BDA0002498069240000091
According to the results in table 4, the specific surface area of the obtained carbon material is always increased with the increase of the ratio of carbon dioxide in the mixed gas under the same other treatment conditions, which indicates that the oxygen in the air and the carbon dioxide in the flue gas together have an ablation reaction on the surface of the carbon material, so that new pores are formed in the carbon material, thereby increasing the specific surface area thereof, and also indicates that it is feasible to increase the specific surface area of the carbon material under the heat treatment conditions by mixing the flue gas and the air. When the volume ratio of carbon dioxide to nitrogen in the simulated flue gas is 1:0.6, the specific surface area of the carbon material reaches the maximum value of 364.3m2Per g, but when the carbon dioxide volume ratio continuesThe specific surface area is reduced when the carbon dioxide is increased, which indicates that the ablation reaction is over-advanced, and the excessive volume ratio of the carbon dioxide does not help to increase the specific surface area of the cracked carbon.
Examples 29 to 33: influence of small amount of sulfide impurities in flue gas on improvement of specific surface area of carbon material
Introducing CO2And N2Mixing according to the volume ratio of 1:1, and preparing a simulated flue gas in advance.
During actual plant production, the actual flue gas that is cleaned and exhausted typically contains very small amounts of sulfide impurities. To verify that the flue gas contains a small amount of sulfide impurities that would adversely affect the increase in the specific surface area of the carbon material, the present application incorporated a small amount of SO in the simulated flue gas2The specific operation process of the gas is as follows: adding SO2Mixing the flue gas with a pre-prepared simulated flue gas according to the volume ratio of 0: 1-0.05: 1 to obtain a series of sulfur-doped simulated flue gases with different sulfur contents.
Putting 1g of carbon black in comparative example 1 into a tubular furnace (the model of the tubular furnace is phi 6cm × 50cm, the volume of the furnace tube is 1.4L), mixing sulfur-doped simulated flue gas and air according to the volume ratio of 1:1, introducing the mixture into the tubular furnace, controlling the total flow of the mixed gas to be 50m L/min, heating to 400 ℃, keeping the temperature for 4h, taking out the carbon material in the tubular furnace after the heat preservation is finished, cleaning the carbon material with deionized water, drying the carbon material at 80 ℃ to obtain the treated carbon material, and testing the specific surface area of a sample by using a specific surface area analyzer2Isothermal adsorption data are measured under 77K for adsorbates, the BET method is adopted to calculate the total specific surface area of the sample, and then the actual specific surface area increase rate of the method is calculated.
In various examples, sulfur doping simulates SO in flue gas2The results of the volume contents and the specific parameters of the final carbon material product are shown in Table 5.
TABLE 5 BET value and lift ratio of carbon Material with a small amount of sulfide impurity in flue gas
Figure BDA0002498069240000111
According to the results in table 5, when other treatment conditions are the same, the specific surface area of the obtained carbon material is slightly reduced with the increase of the proportion of sulfur dioxide in the mixed gas, which indicates that the oxygen in the air generates an ablation reaction on the surface of the carbon material to form new pores in the carbon material, and simultaneously, sulfide impurities such as sulfur dioxide in the flue gas are adsorbed on the surface of the pyrolysis carbon and the generated new pores, so that the hole expanding effect of the pyrolysis carbon is influenced, and a certain poisoning effect is generated. But when the concentration of sulfur dioxide is 5 percent, the specific surface area of the cracked carbon after pore expansion is from 331.7m at the optimal value2The/g is reduced to 313.4m2G, although sulfide impurities in the flue gas have a slight effect on the hole expansion, 94.5% of the hole expansion effect under normal conditions can still be achieved. Therefore, a small amount of sulfide impurities such as sulfur dioxide contained in the flue gas has little adverse effect on pore expansion of the cracked carbon, and in addition, the sulfide content in the actual flue gas purified and exhausted in a factory is basically below 1 percent, and the increase of the specific surface area of the carbon material hardly has any adverse effect. This is also because sulfur impurities are less likely to be adsorbed and deposited on carbon black when a high-temperature heat treatment is performed under an oxygen-containing atmosphere.
Comparative example 2: preparing the biochar by adopting a conventional method
500g of wood chips are taken as raw materials, the raw materials are placed in a cracking reactor, and after the raw materials are subjected to heat preservation treatment for 3 hours at the final pyrolysis temperature of 550 ℃ in the nitrogen atmosphere and are subjected to carbonization process treatment, decomposition of macromolecules in the wood chips is initiated, and micromolecular gas, condensable volatile components and biochar are generated. After the reaction is finished, the condensable volatile components are rapidly cooled into flowable tar, the thermal cracking reactor discharges biochar, small molecular gas and tar, the tar is dark brown or dark black and has pungent coke taste, the biochar is a black stable high carbon-containing solid compound, the biochar is subjected to superfine grinding by a grinder, washed by water and dried at 120 ℃ to obtain 76g of biochar, and the specific surface area of the finally prepared biochar is about 87.4m2(g), sample number 2. The following examples were carried out with the biochar obtained in comparative example 2 as the subject of treatmentComparative experiments were performed.
Examples 34 to 42: influence of different mixed gas compositions on improvement of specific surface area of biomass carbon material during heat treatment
Introducing CO2And N2Mixing according to the volume ratio of 1:1, and preparing a simulated flue gas in advance.
Taking 1g of biomass carbon material in comparative example 2, placing the biomass carbon material in a tubular furnace (the model of the tubular furnace is phi 6cm × 50cm, the volume of the furnace tube is 1.4L), mixing simulated flue gas and air according to the volume ratio of 1: 5-5: 1 by using a three-way valve, introducing the mixture into the tubular furnace, controlling the total flow of the mixed gas to be 50m L/min, heating to 350 ℃, then preserving heat for 3 hours, taking out the biomass carbon material in the tubular furnace after the heat preservation is finished, cleaning the biomass carbon material with deionized water, drying the biomass carbon material at 80 ℃ to obtain a treated carbon material, and testing the specific surface area of a sample by using a specific surface area analysis detector2Isothermal adsorption data are measured under 77K for adsorbates, the BET method is adopted to calculate the total specific surface area of the sample, and then the actual specific surface area increase rate of the method is calculated.
In various embodiments, the results of the specific parameters of the simulated flue gas to air volume ratio and the final biomass carbon material product are shown in table 6.
TABLE 6 BET values and lift ratios of biomass carbon materials at different volume ratios of air to simulated flue gas
Figure BDA0002498069240000121
Figure BDA0002498069240000131
According to the results in table 6, the specific surface area of the biomass carbon material obtained is increased with the increase of the proportion of air in the mixed gas, which indicates that the oxygen in the air generates ablation reaction on the surface of the biomass carbon material, so that new pores are formed in the biomass carbon material, thereby increasing the specific surface area thereof, and also indicates that the flue gas and the air are mixed to perform heat treatmentIt is possible to increase the specific surface area of the biomass carbon material under the conditions of (1). When the volume ratio of the simulated flue gas to the air is 5:5, the specific surface area of the biomass carbon material reaches the maximum value of 413.4m2The specific surface area increasing effect is greatly reduced when the air content is continuously increased, which indicates that the ablation reaction is excessive and is not suitable for pore expansion of the biomass carbon material, and indicates that O in the mixed gas2Concentration and CO2The concentration of the carbon dioxide can have great influence on the reaming of the biomass carbon material, and O in the mixed gas needs to be maintained2And CO2The content is within a suitable range.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.

Claims (6)

1. A treatment method for improving the specific surface area of a carbon material is characterized by comprising the following steps: placing the carbon material in a tubular furnace, introducing mixed gas of flue gas and air in a volume ratio of 0.2: 1-5: 1, carrying out heat treatment at the temperature of 250-450 ℃ for 0.5-4h, taking out the heat-treated carbon material, washing with water, and drying to obtain the carbon material product with high specific surface area.
2. A treatment method for increasing the specific surface area of a carbon material according to claim 1, wherein: the heat treatment temperature is 300-400 ℃, and the treatment time is 1-3 h.
3. A treatment method for increasing the specific surface area of a carbon material according to claim 1, wherein: the volume ratio of flue gas to air in the mixed gas introduced into the tubular furnace is 0.3: 1-3: 1.
4. The method for increasing the specific surface area of a carbon material as claimed in claim 1, wherein the volume flow rate of the mixed gas of the flue gas and the air introduced into the carbon material is 30-60m L/h, preferably 40-50m L/h, based on 1g of the carbon material subjected to the heat treatment.
5. A treatment method for increasing the specific surface area of a carbon material according to claim 1, wherein: the carbon material is carbon black generated by rubber cracking or biochar generated by biomass pyrolysis.
6. A treatment method for increasing the specific surface area of a carbon material according to claim 1, wherein: the main components of the flue gas comprise carbon dioxide and nitrogen, wherein the volume ratio of the carbon dioxide to the nitrogen is 0.3-3: 1, and 1:1 is preferred.
CN202010424234.4A 2020-05-19 2020-05-19 Treatment method for improving specific surface area of carbon material Pending CN111453714A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010424234.4A CN111453714A (en) 2020-05-19 2020-05-19 Treatment method for improving specific surface area of carbon material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010424234.4A CN111453714A (en) 2020-05-19 2020-05-19 Treatment method for improving specific surface area of carbon material

Publications (1)

Publication Number Publication Date
CN111453714A true CN111453714A (en) 2020-07-28

Family

ID=71677506

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010424234.4A Pending CN111453714A (en) 2020-05-19 2020-05-19 Treatment method for improving specific surface area of carbon material

Country Status (1)

Country Link
CN (1) CN111453714A (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102179232A (en) * 2011-02-17 2011-09-14 杭州电子科技大学 Method for preparing flying ash/activated carbon compound adsorbent used for demercuration
CN102964884A (en) * 2012-12-13 2013-03-13 新疆雅克拉炭黑有限责任公司 Hot cracking method process for preparing carbon black by using co-production of tail gas
US20160355402A1 (en) * 2014-07-25 2016-12-08 Farad Power, Inc., Method of making activated nano-porous carbon
CN107128923A (en) * 2017-06-14 2017-09-05 神雾科技集团股份有限公司 Calcium carbide, lime nitrogen and carbon black Joint Production system and method
CN110817839A (en) * 2019-12-06 2020-02-21 华南师范大学 Method for reducing carbon dioxide into porous carbon material, porous carbon material and application

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102179232A (en) * 2011-02-17 2011-09-14 杭州电子科技大学 Method for preparing flying ash/activated carbon compound adsorbent used for demercuration
CN102964884A (en) * 2012-12-13 2013-03-13 新疆雅克拉炭黑有限责任公司 Hot cracking method process for preparing carbon black by using co-production of tail gas
US20160355402A1 (en) * 2014-07-25 2016-12-08 Farad Power, Inc., Method of making activated nano-porous carbon
CN107128923A (en) * 2017-06-14 2017-09-05 神雾科技集团股份有限公司 Calcium carbide, lime nitrogen and carbon black Joint Production system and method
CN110817839A (en) * 2019-12-06 2020-02-21 华南师范大学 Method for reducing carbon dioxide into porous carbon material, porous carbon material and application

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘宝忠: "《腐植酸基多孔炭的制备及其电化学性能》", 31 March 2017 *
西鹏等: "《高技术纤维》", 30 September 2004 *

Similar Documents

Publication Publication Date Title
WO2016176906A1 (en) Method for producing canna indica biochar capable of adsorbing ammonia nitrogen and cadmium simultaneously
CN109096798B (en) Micro-oxidation activation method for waste tire pyrolytic carbon black
CN112919754A (en) Method for preparing biochar and solidifying heavy metal by virtue of pyrolysis of sludge coupled biomass
CN106395816B (en) A method of residue prepares adsorbent after extracting humic acid by lignite
CN111591986B (en) Plant VOCs treatment method and system based on petrochemical enterprise byproduct petroleum coke upgrading utilization
CN102000483A (en) Method for treating asphalt gas efficiently and harmlessly
Mukherjee et al. Optimization of adsorbent derived from non-biodegradable waste employing response surface methodology toward the removal of dye solutions
CN113651324B (en) Preparation method and application of sewage peat
CN110668440A (en) Recycling method of tar residue waste
CN101805636B (en) Scrap tire gasification device and method
CN111453714A (en) Treatment method for improving specific surface area of carbon material
CN110302748B (en) Preparation method of sludge-based biochar
CN106825023B (en) Method and system for restoring organic matter contaminated soil
CN106955660A (en) The preparation method and gasification process of gasification process heavy metal absorbent
CN112691640B (en) Coprinus comatus mushroom dreg porous carbon adsorbent and preparation method and application thereof
Semaan et al. Pilot scale pyro-gasification of biomass and waste: char characterization
EP4048738B1 (en) Ecological purification and reactivation process of carbon black obtained from the pyrolysis of used tyres
KR20170018134A (en) Manufacturing method of carbon black by thermosetting plastic waste
CN115612518B (en) Treatment method for recycling waste tires
CN102600800A (en) Preparation method of semi-coke adsorbent
CN113481023B (en) Method for preparing low-ash biomass semi-coke
CN104014306B (en) The method of Phenanthrene in a kind of active carbon from coal removing waste water
CN110699141B (en) Chain grate-rotary kiln injected biomass fuel and preparation method and application thereof
CN115820315B (en) Combustion-supporting material for smoldering of low-concentration organic matter polluted soil, and preparation method and application thereof
CN115532232B (en) Asphaltene-based adsorbent and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20200728

RJ01 Rejection of invention patent application after publication