CN110877909A - Coal columnar activated carbon and preparation method thereof - Google Patents
Coal columnar activated carbon and preparation method thereof Download PDFInfo
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- CN110877909A CN110877909A CN201911342941.2A CN201911342941A CN110877909A CN 110877909 A CN110877909 A CN 110877909A CN 201911342941 A CN201911342941 A CN 201911342941A CN 110877909 A CN110877909 A CN 110877909A
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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
- C01B32/33—Preparation characterised by the starting materials from distillation residues of coal or petroleum; from petroleum acid sludge
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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 coal columnar activated carbon and a preparation method thereof, belonging to the technical field of activated carbon. The invention mainly solves the technical problems of great pollution and damage to the environment and the health of operators, more floating ash, low strength and the like in the existing production process of the coal columnar activated carbon. The technical scheme of the invention is as follows: a coal columnar activated carbon is prepared from the following raw materials in parts by weight: 50-65 parts of weak sticky coal, 20-25 parts of asphalt and 15-25 parts of binder; a method for preparing a coaly cylindrical activated carbon, comprising the steps of: 1) and milling the powder; 2) preparing a binder; 3) mixing and forming; 4) drying and carbonizing; 5) activating and cooling. The invention has the advantages of high strength, high specific surface area, no additional impurity pollution of the added binder, simple process, high product yield and the like.
Description
Technical Field
The invention belongs to the technical field of activated carbon, and particularly relates to coal columnar activated carbon and a preparation method thereof.
Background
Activated carbon is an important porous adsorption material and has been widely applied to the fields of air purification, water treatment, liquid phase adsorption, catalyst carriers and the like. The active carbon prepared by taking coal as a raw material, namely the coal-based active carbon, currently accounts for six to seven components of the total production amount of the active carbon, and the coal-based active carbon is divided into columnar, pressed block-shaped, amorphous, namely crushed and the like, wherein the production scale and the yield of the columnar coal-based active carbon account for 30 to 40 percent of the coal-based active carbon in China.
Raw materials in the traditional coal columnar activated carbon production technology comprise raw coal, a binder and the like, wherein the binder is mostly coal tar in the traditional process, the coal tar is a mixture containing a plurality of chemical substances, and the coal tar contains 1) oxygen-containing compounds, such as phenol, cresol, xylenol and the like; 2) sulfur-containing compounds such as thiophene, benzo, etc.; 3) the nitrogen-containing compounds comprise pyridine, quinoline, carbazole, pyrrole and the like. These substances are highly polluting and harmful both to the environment and to the health of the operators. In addition, coal tar is an oily substance, is a black to brown viscous liquid at normal temperature, has odor, and seriously influences clean production.
In addition to coal tar, a binder such as pulp waste liquid, starch, and sodium humate is used as a binder for producing the coal-based columnar activated carbon. However, the pulp waste liquid, starch and carbon skeleton required by the activated carbon cannot be formed in the activated carbon activation process, so that the prepared activated carbon is often rich in floating ash and low in strength; sodium humate has been reported successfully in small trials, but there are many problems in practical production.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides coal columnar activated carbon and a preparation method thereof, and solves the technical problems of great pollution and damage to the environment and the health of operators, much floating ash, low strength and the like in the production process of the existing coal columnar activated carbon.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a coal columnar activated carbon is prepared from the following raw materials in parts by weight: 50-65 parts of weak sticky coal, 20-25 parts of asphalt and 15-25 parts of binder; the coal columnar activated carbon is columnar black particles with the column diameter of 1-4mm, the strength value of the coal columnar activated carbon is 80-93, the specific surface area is 800-1000 square meters per gram, the iodine value is 800-1000mg/g, and the carbon tetrachloride adsorption value is 50-70%.
Furthermore, the water content of the weakly caking coal is less than or equal to 5 percent, the ash content is less than or equal to 8 percent, the volatile matter is less than or equal to 15 percent, and the fixed carbon is 70-85 percent.
Further, the asphalt has a softening point of more than 90 ℃, an ash content of less than 1%, a moisture content of less than 3%, and free carbon of 18-22%.
Further, the binder is a mixture of carboxymethyl cellulose and calcium lignosulfonate, and the weight ratio of the carboxymethyl cellulose to the calcium lignosulfonate is 1: 1, the density of the carboxymethyl cellulose is 0.5-0.7g/cm3The lignin content of the calcium lignosulphonate is 50-65%, and the water insoluble substance is less than or equal to 1.0%.
A method for preparing a coaly cylindrical activated carbon, comprising the steps of:
1) milling: taking 50-65 parts by weight of weak sticky coal and 20-25 parts by weight of asphalt, uniformly mixing and then pulverizing to obtain powder with the passing rate of more than 90 percent of 200 meshes;
2) preparing a binder: mixing carboxymethyl cellulose and calcium lignosulfonate according to a weight ratio of 1: 1 to prepare a binder;
3) mixing and forming: putting the powder prepared in the step 1) into a mixer, adding 15-25 parts of the binder prepared in the step 2), adding pure water, stirring and mixing for 15 minutes to obtain paste materials, adding the paste materials into a mold of a forming machine, and forming into cylindrical particles under the pressure of 50-80 Mpa;
4) drying and carbonizing: adding the formed cylindrical particles into a converter for drying and carbonizing in sequence, wherein: the drying temperature is 100-180 ℃, the carbonization furnace gradually heats up for carbonization, the carbonization time is calculated when the temperature is raised to 600 ℃, and the carbonization time is 50-80 minutes;
5) activating and cooling: and transferring the carbonized material into an activation furnace, introducing a steam activating agent when the temperature of the activation furnace rises to above 800-850 ℃, introducing the steam activating agent with the introduction amount of 8-10 ml/min, continuing to rise to 900 ℃, starting to calculate the activation time, activating for 60-120 minutes, transferring the material into a cooling device after the activation is finished, cooling to below 40 ℃, and screening to remove powder to obtain the coal columnar activated carbon.
The coal columnar activated carbon prepared by the method has high wear-resisting strength, and the strength value is 80-90; the composite material has developed pore volume and higher specific surface area, and the specific surface area can reach 800-1000 square meters per gram; the coal tar is not added in the preparation process, the preparation environment is clean and pollution-free, and certain guarantee is provided for guaranteeing the preparation environment and protecting the body health of preparation staff; compared with the traditional coal tar binder, the raw material and the binder provided by the invention have the advantage of low cost. Compared with the prior art, the invention has the advantages of high strength, high specific surface area, no additional impurity pollution of the added binder, simple process, high product yield (the yield is 30-35 percent), and the like.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
The coal columnar activated carbon provided in the embodiment 1 is prepared from the following raw materials in parts by weight: 50 parts of weakly caking coal, 20 parts of asphalt and 20 parts of binder; the coal columnar activated carbon is columnar black particles with the column diameter of 3mm, the strength value of the coal columnar activated carbon is 80-93, the specific surface area is 800-1000 square meters per gram, the iodine value is 800-1000mg/g, and the carbon tetrachloride adsorption value is 50-70%.
A method for preparing a coaly cylindrical activated carbon, comprising the steps of:
1) milling: taking 50 parts by weight of weakly sticky coal and 20 parts by weight of asphalt, uniformly mixing and then pulverizing to obtain powder with the passing rate of 95% of 200 meshes;
2) preparing a binder: mixing carboxymethyl cellulose and calcium lignosulfonate according to a weight ratio of 1: 1 to prepare a binder;
3) mixing and forming: putting the powder prepared in the step 1) into a mixer, adding 20 parts of the binder prepared in the step 2), adding pure water, stirring and mixing for 15 minutes to obtain paste materials, adding the paste materials into a mold of a forming machine, and forming into cylindrical particles under the pressure of 50-80 Mpa;
4) drying and carbonizing: adding the formed cylindrical particles into a converter for drying and carbonizing in sequence, wherein: the drying temperature is 100 ℃, the drying time is 60 minutes, the carbonization furnace is gradually heated to be carbonized, the carbonization time is calculated when the temperature is raised to 600 ℃, and the carbonization time is 60 minutes;
5) activating and cooling: and transferring the carbonized material into an activation furnace, introducing a water vapor activating agent when the temperature of the activation furnace is raised to be more than 800 ℃, introducing 8ml/min of the water vapor activating agent, continuously raising the temperature to be 900 ℃, starting to calculate the activation time, activating for 100 minutes, transferring the material into a cooling device after the activation is finished, cooling the material to be below 40 ℃, screening to remove powder, and transferring the material into a sealing device to obtain the coal columnar activated carbon sample A.
The weak sticky coal has the water content of less than or equal to 5 percent, the ash content of less than or equal to 8 percent, the volatile matter of less than or equal to 15 percent and the fixed carbon of 70 to 85 percent.
The asphalt has a softening point of more than 90 ℃, an ash content of less than 1%, a moisture content of less than 3%, and free carbon of 18-22%.
The binder is a mixture of carboxymethyl cellulose and calcium lignosulfonate, and the weight ratio of the carboxymethyl cellulose to the calcium lignosulfonate is 1: 1, the density of the carboxymethyl cellulose is 0.5-0.7g/cm3The lignin content of the calcium lignosulphonate is 50-65%, and the water insoluble substance is less than or equal to 1.0%.
Example 2
The coal columnar activated carbon provided in the embodiment 2 is prepared from the following raw materials in parts by weight: 62.5 parts of weakly caking coal, 25 parts of asphalt and 25 parts of binder; the coal columnar activated carbon is columnar black particles with the column diameter of 3mm, the strength value of the coal columnar activated carbon is 80-93, the specific surface area is 800-1000 square meters per gram, the iodine value is 800-1000mg/g, and the carbon tetrachloride adsorption value is 50-70%.
A method for preparing a coaly cylindrical activated carbon, comprising the steps of:
1) milling: uniformly mixing 62.5 parts by weight of weak sticky coal and 25 parts by weight of asphalt, and pulverizing to obtain powder with a passing rate of 94% of 200 meshes;
2) preparing a binder: mixing carboxymethyl cellulose and calcium lignosulfonate according to a weight ratio of 1: 1 to prepare a binder;
3) mixing and forming: putting the powder prepared in the step 1) into a mixer, adding 25 parts of the binder prepared in the step 2), adding pure water, stirring and mixing for 15 minutes to obtain paste materials, adding the paste materials into a mold of a forming machine, and forming into cylindrical particles under the pressure of 50-80 Mpa;
4) drying and carbonizing: adding the formed cylindrical particles into a converter for drying and carbonizing in sequence, wherein: the drying temperature is 100 ℃, the drying time is 60 minutes, the carbonization furnace is gradually heated to be carbonized, the carbonization time is calculated when the temperature is raised to 600 ℃, and the carbonization time is 60 minutes;
5) activating and cooling: and transferring the carbonized material into an activation furnace, introducing a water vapor activating agent when the temperature of the activation furnace is raised to be more than 800 ℃, introducing 8ml/min of the water vapor activating agent, continuously raising the temperature to be 900 ℃, starting to calculate the activation time, activating for 100 minutes, transferring the material into a cooling device after the activation is finished, cooling the material to be below 40 ℃, screening to remove powder, and transferring the material into a sealing device to obtain the coal columnar activated carbon sample B.
The weak sticky coal has the water content of less than or equal to 5 percent, the ash content of less than or equal to 8 percent, the volatile matter of less than or equal to 15 percent and the fixed carbon of 70 to 85 percent.
The asphalt has a softening point of more than 90 ℃, an ash content of less than 1%, a moisture content of less than 3%, and free carbon of 18-22%.
The binder is a mixture of carboxymethyl cellulose and calcium lignosulfonate, and the weight ratio of the carboxymethyl cellulose to the calcium lignosulfonate is 1: 1, the density of the carboxymethyl cellulose is 0.5-0.7g/cm3The lignin content of the calcium lignosulphonate is 50-65%, and the water insoluble substance is less than or equal to 1.0%.
Example 3
The coal columnar activated carbon provided in this embodiment 3 is prepared from the following raw materials in parts by weight: 50 parts of weakly caking coal, 21.25 parts of asphalt and 20 parts of binder; the coal columnar activated carbon is columnar black particles with the column diameter of 4mm, the strength value of the coal columnar activated carbon is 80-93, the specific surface area is 800-1000 square meters per gram, the iodine value is 800-1000mg/g, and the carbon tetrachloride adsorption value is 50-70%.
A method for preparing a coaly cylindrical activated carbon, comprising the steps of:
1) milling: taking 50 parts by weight of weak sticky coal and 21.25 parts by weight of asphalt, uniformly mixing and then pulverizing to obtain powder with the passing rate of 95% of 200 meshes;
2) preparing a binder: mixing carboxymethyl cellulose and calcium lignosulfonate according to a weight ratio of 1: 1 to prepare a binder;
3) mixing and forming: putting the powder prepared in the step 1) into a mixer, adding 20 parts of the binder prepared in the step 2), adding pure water, stirring and mixing for 15 minutes to obtain paste materials, adding the paste materials into a mold of a forming machine, and forming into cylindrical particles under the pressure of 50-80 Mpa;
4) drying and carbonizing: adding the formed cylindrical particles into a converter for drying and carbonizing in sequence, wherein: the drying temperature is 100 ℃, the drying time is 60 minutes, the carbonization furnace is gradually heated to be carbonized, the carbonization time is calculated when the temperature is raised to 600 ℃, and the carbonization time is 80 minutes;
5) activating and cooling: and transferring the carbonized material into an activation furnace, introducing a water vapor activating agent when the temperature of the activation furnace is raised to above 850 ℃, introducing 10ml/min of the water vapor activating agent, continuing to raise the temperature to 900 ℃, starting to calculate the activation time, activating for 120 minutes, transferring the activated material into a cooling device after the activation is finished, cooling to below 40 ℃, screening to remove powder, and transferring the activated material into a sealing device to obtain the coal columnar activated carbon sample C.
The weakly caking coal has a moisture content of 0.9%, an ash content of 6.8%, a volatile matter content of 14%, and fixed carbon content of 80%.
The asphalt has a softening point of 93 ℃, an ash content of 0.85%, a moisture content of 0.9%, and free carbon of 19%.
The binder is a mixture of carboxymethyl cellulose and calcium lignosulfonate, and the weight ratio of the carboxymethyl cellulose to the calcium lignosulfonate is 1: 1, the density of the carboxymethyl cellulose is 0.5-0.7g/cm3The lignin content of the calcium lignosulphonate is 50-65%, and the water insoluble substance is less than or equal to 1.0%.
The A, B, C samples obtained in the 3 examples were compared with Ningxia coal columnar activated carbon D (using coal tar as a binder) sample of the same standard, and the specific surface area, strength, iodine adsorption value, and carbon tetrachloride adsorption rate were compared.
1. Determination of specific surface area: respectively taking 5g of A, B, C, D samples, sending the samples to a metering and testing center of Xinhua chemical engineering Limited, Shanxi for specific surface area detection, and respectively obtaining the following results: sample a: 920 square meters per gram; sample B.913 square meters per gram; sample C: 922 square meters per gram; sample D: 918 square meters per gram;
2. and (3) measuring intensity values: respectively taking 200ml of A, B, C, D four samples, drying for two hours, cooling for later use, then respectively taking 50ml of dried samples, ball-milling for 5 minutes in a roller of a strength instrument after weighing, weighing after sieving the samples by a sieve, and calculating strength values, wherein the results are respectively as follows: sample a: 92 percent; sample B: 91.3 percent; sample C: 92.5 percent; sample D: 92 percent;
3. measuring iodine adsorption value, taking 10g of A, B, C, D four samples respectively, grinding to 90%, passing through a test sieve of 0.075mm, drying in an oven of 150 +/-5 ℃ for 2 hours, cooling for standby, taking 4 kinds of quantitative samples and an iodine standard solution, fully oscillating and adsorbing, measuring the residual iodine amount of the solution by a titration method, calculating the number of milligrams of iodine adsorbed by each sample, making an adsorption isotherm, and calculating the adsorption value of the activated carbon to iodine, wherein the results are respectively: sample a: 942 mg/g; sample B: 948 mg/g; sample C: 945 mg/g; sample D: 946 mg/g;
4. measuring the carbon tetrachloride adsorption rate, taking A, B, C, D four kinds of active carbon, 50ml each, placing in a drying oven of 150 + -5 deg.C for drying for 2 hours, cooling for standby. And (3) respectively putting the 4 dry samples into a measuring tube, sealing and weighing, connecting the measuring tube to a carbon tetrachloride adsorption instrument, introducing mixed gas containing certain carbon tetrachloride steam concentration, and measuring the percentage of the weight of the carbon tetroxide adsorbed by the sample to the weight of the sample when the activated carbon reaches adsorption saturation.
The results were respectively: sample a: 62.8 percent; sample B: 61.9 percent; sample C: 62.5 percent; sample D: 62.0 percent;
5. summary of test conditions
In the above table, it can be seen that, in the case of using no coal tar as a binder, compared with the columnar activated carbon produced in Ningxia using coal tar as a binder, the sample A, B, C has no great change in main properties, and is almost close to the main properties, thereby achieving the quality standard of the high-quality coal columnar activated carbon.
Claims (5)
1. A coal columnar activated carbon characterized by: the traditional Chinese medicine is prepared from the following raw materials in parts by weight: 50-65 parts of weak sticky coal, 20-25 parts of asphalt and 15-25 parts of binder; the coal columnar activated carbon is columnar black particles with the column diameter of 1-4mm, the strength value of the coal columnar activated carbon is 80-93, the specific surface area is 800-1000 square meters per gram, the iodine value is 800-1000mg/g, and the carbon tetrachloride adsorption value is 50-70%.
2. A coal-based columnar activated carbon as claimed in claim 1, which comprises: the weak sticky coal has the water content of less than or equal to 5 percent, the ash content of less than or equal to 8 percent, the volatile matter of less than or equal to 15 percent and the fixed carbon of 70 to 85 percent.
3. A coal-based columnar activated carbon as claimed in claim 1, which comprises: the asphalt has a softening point of more than 90 ℃, an ash content of less than 1%, a moisture content of less than 3%, and free carbon of 18-22%.
4. A coal-based columnar activated carbon as claimed in claim 1, which comprises: the binder is a mixture of carboxymethyl cellulose and calcium lignosulfonate, and the weight ratio of the carboxymethyl cellulose to the calcium lignosulfonate is 1: 1, the carboxymethyl celluloseThe density of the extract is 0.5-0.7g/cm3The lignin content of the calcium lignosulphonate is 50-65%, and the water insoluble substance is less than or equal to 1.0%.
5. A method for producing the coal-based columnar activated carbon as claimed in claim 1, characterized by comprising the steps of:
1) milling: taking 50-65 parts by weight of weak sticky coal and 20-25 parts by weight of asphalt, uniformly mixing and then pulverizing to obtain powder with the passing rate of more than 90 percent of 200 meshes;
2) preparing a binder: mixing carboxymethyl cellulose and calcium lignosulfonate according to a weight ratio of 1: 1 to prepare a binder;
3) mixing and forming: putting the powder prepared in the step 1) into a mixer, adding 15-25 parts of the binder prepared in the step 2), adding pure water, stirring and mixing for 15 minutes to obtain paste materials, adding the paste materials into a mold of a forming machine, and forming into cylindrical particles under the pressure of 50-80 Mpa;
4) drying and carbonizing: adding the formed cylindrical particles into a converter for drying and carbonizing in sequence, wherein: the drying temperature is 100-180 ℃, the carbonization furnace gradually heats up for carbonization, the carbonization time is calculated when the temperature is raised to 600 ℃, and the carbonization time is 50-80 minutes;
5) activating and cooling: and transferring the carbonized material into an activation furnace, introducing a steam activating agent when the temperature of the activation furnace rises to above 800-850 ℃, introducing the steam activating agent with the introduction amount of 8-10 ml/min, continuing to rise to 900 ℃, starting to calculate the activation time, activating for 60-120 minutes, transferring the material into a cooling device after the activation is finished, cooling to below 40 ℃, and screening to remove powder to obtain the coal columnar activated carbon.
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| CN113401899A (en) * | 2021-07-07 | 2021-09-17 | 山西新华防化装备研究院有限公司 | Method for preparing desulfurization and denitrification active carbon without coal tar |
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| CN116970367A (en) * | 2023-08-14 | 2023-10-31 | 上海华严检测技术有限公司 | Adhesive, adhesive preparation method and carbon adsorbent adopting adhesive |
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