CN112174137A - Method for preparing primary active carbon by activating shot coke through combination method - Google Patents
Method for preparing primary active carbon by activating shot coke through combination method Download PDFInfo
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- CN112174137A CN112174137A CN202011153147.6A CN202011153147A CN112174137A CN 112174137 A CN112174137 A CN 112174137A CN 202011153147 A CN202011153147 A CN 202011153147A CN 112174137 A CN112174137 A CN 112174137A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/336—Preparation characterised by gaseous activating agents
Abstract
The invention relates to a method for preparing primary active carbon by activating shot coke by a combined method, which comprises the following steps: s1 mixing with soda charcoal: uniformly mixing shot coke particles with uniform particle size and KOH solid with a certain proportion to obtain a mixture; s2 chemical activation: placing the mixture prepared in the step S1 in a high-temperature tube furnace, and performing high-temperature chemical activation in an inert gas atmosphere; s3 acid washing: placing the product subjected to high-temperature chemical activation in the step S2 in a glass container, adding HCl solution with a certain concentration for acid washing, neutralizing with deionized water until the pH value is 6.8-7.0 after the acid washing is carried out for a certain time, then drying through drying equipment, and then cooling and screening for later use; s4 physical activation: weighing a certain amount of the final product obtained after acid washing in the step S3, placing the product in a high-temperature tube furnace, and carrying out physical activation at a certain temperature. The invention has the following beneficial effects: the utilization rate of the byproduct of the shot coke is improved, thereby realizing the purpose of changing waste into valuable. The invention has simple process and is easy for large-scale production.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a method for preparing primary activated carbon by activating shot coke by a combination method.
Background
Shot coke is coke generated when a delayed coking device processes vacuum residue in the production process of petroleum coke in a refinery, and is a mixed solid of shot coke and sponge coke. The reason for generating the sponge coke is that the contents of asphaltene and heteroatoms in the raw oil are relatively low, and shot coke is relatively easily generated when the content is higher.
As the quality of coking raw materials for production in China is increasingly poor, the probability of producing shot coke is correspondingly increased. The coke forming route is that in the process of vacuum residue thermal conversion, when aromatic hydrocarbon in the four components of the residue is at high temperature, the carbon asphaltene is formed according to the process of aromatic hydrocarbon colloid asphaltene carbon asphaltene. Therefore, once the residual oil asphaltene content is too high, carbon asphaltenes are formed prematurely, the carbon asphaltenes form earlier particles of shot coke before the raw material enters a coke tower, the shot coke is formed after a series of processes, and how to prevent the generation of the shot coke becomes a technical problem which needs to be solved urgently by enterprises.
Disclosure of Invention
According to the defects in the prior art, the technical problems to be solved by the invention are as follows: in order to solve one of the problems, a method for preparing primary activated carbon by activating shot coke by a combined method is provided.
The technical scheme adopted by the invention for solving the problems is as follows:
the invention relates to a method for preparing primary activated carbon by activating shot coke by a combined method, which comprises the following steps:
s1 mixing with soda charcoal: uniformly mixing shot coke particles with uniform particle size and KOH solid with a certain proportion to obtain a mixture;
s2 chemical activation: placing the mixture prepared in the step S1 in a high-temperature tube furnace, and performing high-temperature chemical activation in an inert gas atmosphere;
s3 acid washing: placing the product subjected to high-temperature chemical activation in the step S2 in a glass container, adding HCl solution with a certain concentration for acid washing, neutralizing with deionized water until the pH value is 6.8-7.0 after the acid washing is carried out for a certain time, then drying through drying equipment, and then cooling and screening for later use;
s4 physical activation: weighing a certain amount of the final product obtained after acid washing in the step S3, placing the product in a high-temperature tube furnace, and carrying out physical activation at a certain temperature.
The activation method is carried out by a chemical-physical combination method. The method has simple process, the obtained shot coke has good sphericity, the CTC value and the strength reach the indexes of primary activated carbon, and the utilization rate of the shot coke byproduct is improved, thereby realizing the purpose of changing waste into valuable.
Preferably, in the step S1, the ratio of the alkali to the carbon is 2:1-0.3: 1.
Preferably, in the step S1, the ratio of the alkali to the carbon is 2:1-0.5: 1.
Preferably, in the step S2, the temperature of chemical activation is 800-900 ℃, and the activation time is 1-3 h.
Preferably, in the step S3, the concentration of the HCl solution is 8% to 20%, and the acid washing time is 20 to 28 hours.
Preferably, in step S4, the physical activation refers to water vapor activation, the activation temperature is 800 ℃ to 900 ℃, and the activation time is 1 to 3 hours.
Preferably, the atmosphere of the tube furnace is: nitrogen at a flow rate of 150 cc/min.
Preferably, the heating rate of the tube furnace is: heating to 800-900 ℃ at a heating rate of 5 ℃/min.
Compared with the prior art, the invention has the following beneficial effects:
the method uses a chemical-physical combined activation method to make the shot coke which is a byproduct with a shape normalized but without a pore structure into a certain pore structure, the CTC value and the strength reach the indexes of primary activated carbon, the utilization rate of the shot coke byproduct is improved, and the purpose of changing waste into valuable is realized.
The CTC value and the strength of the primary activated carbon prepared from the shot coke obtained by the invention reach the indexes of the primary activated carbon.
The invention has simple process and is easy for large-scale production.
Drawings
FIG. 1 is a photograph of the shot coke of example 1 before activation.
FIG. 2 is a photograph of the shot coke of example 1 after activation.
Fig. 3 is a photograph of the shot coke of example 2 before activation.
FIG. 4 is a photograph of the shot coke of example 2 after activation.
Detailed Description
The invention is further described below with reference to the accompanying drawings:
the present invention is further illustrated by the following specific examples, which are not intended to limit the scope of the invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
The conventional shot coke is in a regular spherical shape and uniform in size, but has undeveloped pores, so that the shot coke is treated by an activation method (a physical activation method and a chemical activation method) to form a spherical carbon material with a certain pore structure, and the spherical carbon material is used as primary activated carbon.
Example 1: uniformly mixing 16g of shot coke particles (the particle size is 2-3 mm) and 20g of KOH solid, placing the mixture in a high-temperature tube furnace, activating the mixture for 2h at 800 ℃ in the atmosphere of nitrogen, cooling the mixture to room temperature, taking the mixture out, placing the activated sample in a glass beaker, soaking the activated sample in 15% HCl solution for 24h, pouring out supernatant, and neutralizing the sample with deionized water until the pH value is 6.9. Drying in a 105 ℃ oven, and then sieving the dried sample by a 2-3mm sieve.
Weighing 3g of the sieved sample, continuously placing the sample in a high-temperature tube furnace, heating the sample to 800 ℃ in a nitrogen atmosphere, replacing nitrogen with water vapor, activating the sample for 2 hours, continuously replacing the water vapor with nitrogen, and cooling the sample to room temperature. And taking out a product obtained by steam activation, and sieving the product through a sieve of 2-3mm to obtain a finished product of the primary activated carbon prepared by the joint method activated shot coke, wherein the CTC value of the finished product is 51 percent, and the strength is 91 percent.
Example 2: uniformly mixing 20g of shot coke particles (the particle size is 2-3 mm) and 40g of KOH solid, placing the mixture in a high-temperature tube furnace, carrying out chemical activation in the atmosphere of nitrogen, wherein the chemical activation temperature is 850 ℃ and the chemical activation time is 2h, cooling to room temperature, taking out the mixture, placing the activated sample in a glass beaker, soaking the sample for 24h by using 15% HCl solution, pouring out supernatant, and neutralizing by using deionized water until the pH value is 6.9. Drying in a 105 ℃ oven, and then sieving the dried sample by a 2-3mm sieve.
Weighing 5g of the sieved sample, continuously placing the sample in a high-temperature tube furnace, heating the sample to 800 ℃ in a nitrogen atmosphere, replacing nitrogen with water vapor, activating the sample for 1.5h, continuously replacing the water vapor with nitrogen, and cooling the sample to room temperature. And taking out a product obtained by steam activation, and sieving the product through a sieve of 2-3mm to obtain a finished product of the primary activated carbon prepared by the joint method activated shot coke, wherein the CTC value of the finished product is 54% and the strength is 93%.
Example 3: uniformly mixing 40g of shot coke particles (the particle size is 2-3 mm) and 40g of KOH solid, placing the mixture in a high-temperature tube furnace, carrying out chemical activation in the atmosphere of nitrogen, wherein the chemical activation temperature is 800 ℃, the chemical activation time is 2h, taking out the mixture after cooling to room temperature, placing the activated sample in a glass beaker, soaking the sample in 15% HCl solution for 24h, pouring out supernatant, and neutralizing the sample with deionized water until the pH value is 7. Drying in a 105 deg.C oven, and sieving with 2-3mm sieve.
Weighing 5g of the sieved sample, continuously placing the sample in a high-temperature tube furnace, heating the sample to 800 ℃ in a nitrogen atmosphere, replacing nitrogen with water vapor, activating the sample for 1.5h, continuously replacing the water vapor with nitrogen, and cooling the sample to room temperature. And taking out a product obtained by steam activation, and sieving the product through a sieve of 2-3mm to obtain a finished product of the primary activated carbon prepared by the joint method activated shot coke, wherein the tested CTC value of the finished product is 58% and the strength is 90%.
Example 4: uniformly mixing 20g of shot coke particles (the particle size is 2-3 mm) and 40g of KOH solid, placing the mixture in a high-temperature tube furnace, carrying out chemical activation in the atmosphere of nitrogen, wherein the chemical activation temperature is 850 ℃, the chemical activation time is 2h, taking out the mixture after cooling to room temperature, placing the activated sample in a glass beaker, soaking the sample in 10% HCl solution for 28h, pouring out supernatant, and neutralizing the sample with deionized water until the pH value is 7. Drying in a 105 ℃ oven, and then sieving the dried sample by a 2-3mm sieve.
Weighing 5g of the sieved sample, continuously placing the sample in a high-temperature tube furnace, heating the sample to 800 ℃ in a nitrogen atmosphere, replacing nitrogen with water vapor, activating the sample for 1.5h, continuously replacing the water vapor with nitrogen, and cooling the sample to room temperature. And taking out a product obtained by steam activation, and sieving the product through a sieve of 2-3mm to obtain a finished product of the primary activated carbon prepared by the joint method activated shot coke, wherein the measured CTC value of the finished product is 55%, and the strength of the finished product is 92%.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A method for preparing primary active carbon by activating shot coke by a combined method is characterized by comprising the following steps: the method comprises the following steps:
s1 mixing with soda charcoal: uniformly mixing shot coke particles with uniform particle size and KOH solid with a certain proportion to obtain a mixture;
s2 chemical activation: placing the mixture prepared in the step S1 in a high-temperature tube furnace, and performing high-temperature chemical activation in an inert gas atmosphere;
s3 acid washing: placing the product subjected to high-temperature chemical activation in the step S2 in a glass container, adding HCl solution with a certain concentration for acid washing, neutralizing the acid washed product to be neutral by deionized water after certain time of acid washing, drying the acid washed product by drying equipment, and cooling and screening the dried product for later use;
s4 physical activation: weighing a certain amount of the final product obtained after acid washing in the step S3, placing the product in a high-temperature tube furnace, and carrying out physical activation at a certain temperature.
2. The method for preparing primary activated carbon by combined process activated shot coke according to claim 1, characterized in that: in the step S1, the mass ratio of the alkali carbon is 2:1-0.5: 1.
3. The method for preparing primary activated carbon by combined process activated shot coke according to claim 2, characterized in that: in the step S2, the temperature of chemical activation is 800-900 ℃, and the activation time is 1-3 h.
4. The method for preparing primary activated carbon by combined process activated shot coke according to claim 3, characterized in that: in the step S3, the concentration of the HCl solution is 8% -20%, and the pickling time is 20-28 h.
5. The method for preparing primary activated carbon by combined process activated shot coke according to claim 4, characterized in that: in the step S4, the physical activation refers to water vapor activation, the activation treatment temperature is 800-900 ℃, and the activation time is 1-3 h.
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Citations (5)
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| CN1334237A (en) * | 2000-07-25 | 2002-02-06 | 可乐丽股份有限公司 | Active carbon and its production method, polarizable electrode and double layer capacitor |
| US6475461B1 (en) * | 1995-03-30 | 2002-11-05 | Nippon Sanso Corporation | Porous carbonaceous material, manufacturing method therefor and use thereof |
| US20110312485A1 (en) * | 2010-06-18 | 2011-12-22 | The Governors Of The University Of Alberta | Method for preparation of activated carbon |
| CN103395783A (en) * | 2013-07-26 | 2013-11-20 | 武汉钢铁(集团)公司 | Preparation method and preparation equipment of activated carbon |
| CN104692382A (en) * | 2014-12-10 | 2015-06-10 | 山东钢铁股份有限公司 | Method for preparing active carbon by using coke reactivity testing device |
-
2020
- 2020-10-26 CN CN202011153147.6A patent/CN112174137A/en active Pending
Patent Citations (5)
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| US6475461B1 (en) * | 1995-03-30 | 2002-11-05 | Nippon Sanso Corporation | Porous carbonaceous material, manufacturing method therefor and use thereof |
| CN1334237A (en) * | 2000-07-25 | 2002-02-06 | 可乐丽股份有限公司 | Active carbon and its production method, polarizable electrode and double layer capacitor |
| US20110312485A1 (en) * | 2010-06-18 | 2011-12-22 | The Governors Of The University Of Alberta | Method for preparation of activated carbon |
| CN103395783A (en) * | 2013-07-26 | 2013-11-20 | 武汉钢铁(集团)公司 | Preparation method and preparation equipment of activated carbon |
| CN104692382A (en) * | 2014-12-10 | 2015-06-10 | 山东钢铁股份有限公司 | Method for preparing active carbon by using coke reactivity testing device |
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Effective date of registration: 20210709 Address after: 272000 No.99 Rencheng Avenue, Rencheng District, Jining City, Shandong Province (Jining Carbon Group Co., Ltd.) Applicant after: JINING CARBON GROUP Co.,Ltd. Applicant after: JINING KENON NEW CARBON MATERIALS TECHNOLOGY Co.,Ltd. Address before: 272000 No.99 Rencheng Avenue, Rencheng District, Jining City, Shandong Province (Jining Carbon Group Co., Ltd.) Applicant before: JINING CARBON GROUP Co.,Ltd. |