CN111470506A - Preparation method of porous carbon material - Google Patents
Preparation method of porous carbon material Download PDFInfo
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- CN111470506A CN111470506A CN202010475954.3A CN202010475954A CN111470506A CN 111470506 A CN111470506 A CN 111470506A CN 202010475954 A CN202010475954 A CN 202010475954A CN 111470506 A CN111470506 A CN 111470506A
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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
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28073—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being in the range 0.5-1.0 ml/g
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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
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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
- C01B32/354—After-treatment
- C01B32/382—Making shaped products, e.g. fibres, spheres, membranes or foam
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Materials Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of a porous carbon material, which comprises the steps of uniformly mixing 5-20% of coal-charging dust removal ash, 20-55% of tar residue and 15-50% of weak sticky coal for coking by a mixing device, carrying out compression molding, heating to 240-plus-material temperature of 300 ℃, staying for not less than 20min, then continuing heating to 750-plus-material temperature of 800 ℃, introducing gas, heating to 900-plus-material temperature of 1200 ℃, keeping the temperature at the final temperature for not less than 1h, cooling, washing with water and drying to prepare the porous carbon material with the specific surface area of 1200m2More than g, total pore volume greater than 0.7cm3G, bulk density greater than 0.40g/cm3The iodine adsorption value of the porous carbon material product is 900-1200 mg/g. According to the invention, the high-porosity porous carbon material is prepared by taking the coking coal-charging dust removal ash, the tar residue and the weak-viscosity coking coal as raw materials, so that the resource utilization of the carbon-containing solid waste in the coking process is realized, and meanwhile, the porous carbon material with excellent performance can be prepared.
Description
Technical Field
The invention belongs to the technical field of carbon material preparation, relates to a resource utilization technology of solid wastes in the coking industry, and particularly relates to a preparation method for preparing a high-performance porous carbon material by using coking coal-charging dust removal ash and tar residue in combination with weak-caking coking coal.
Background
The porous carbon material has the advantages of large specific surface area, light weight, stable chemical property and the like. At present, carbon materials with application values comprise activated carbon, carbon fibers, graphene and the like, and the carbon materials can show unique excellent properties of high strength, heat resistance, friction resistance, chemical corrosion resistance, electric conduction, heat conduction, radiation resistance, low damping value, noise reduction, shock absorption and the like. At present, carbon materials are widely applied to the fields of energy, environment, machinery, electronics and the like. Patent 201110249825.3 proposes a method for preparing porous carbon material by using at least one of petroleum coke, raw pitch coke, metallurgical coke and charcoal as raw material and auxiliary material as pore-forming agent, which does not relate to the application of coking dust removal ash and weak caking coking coal in the preparation of porous carbon material. Therefore, if the treatment of the carbon-containing solid waste in the coking process can be combined with the development of the porous carbon material, the resource utilization can have obvious technical, environmental and economic values.
Disclosure of Invention
The method takes resource utilization of the coal-charging dust removal ash in the coking and coal-charging process as a starting point, integrates the coal blending coking theory and the mechanism characteristics of the porous carbon material, takes the coking and coal-charging dust removal ash, the tar residue and the weak-viscosity coking coal as raw materials, and prepares the porous carbon material with high porosity.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of a porous carbon material is characterized in that 5% -20% of coal-charging dust removal ash, 20% -55% of tar residues and 15% -50% of weak sticky coal for coking are mixed uniformly by a mixing device to be pressed and formed, the mixture is heated to 300 ℃ for not less than 20min, then the mixture is heated to 800 ℃ for 750 ℃ plus materials and gas is introduced, the mixture is heated to 1200 ℃ for 900 plus materials at the final temperature, the constant temperature time of the final temperature is not less than 1h, and the porous carbon material is cooled, washed by water and dried to prepare the porous carbon material with the specific surface area of 1200m2More than g, total pore volume greater than 0.7cm3G, bulk density greater than 0.40g/cm3And the iodine adsorption value of the porous carbon material product is 900-1200mg/g, and the percentages are mass percentages.
The particle sizes of the coal-charging dust-removing ash, the tar slag and the coking weakly sticky coal reach below 3mm, wherein the proportion of the particle size of the coal-charging dust-removing ash smaller than 100 meshes is not less than 80%, the proportion of the particle size of the tar slag smaller than 50 meshes is not less than 30%, the proportion of the particle size of the coking weakly sticky coal smaller than 100 meshes is not less than 30%, and the coal vitrinite average maximum reflectance meeting the coal petrology index reaches 1.5-2.3%.
The heating and temperature rising speed is 8-15 ℃/min.
The introduced gas is carbon dioxide gas or water vapor, and the gas flow rate is 0.5L/min-10L/min.
The molding pressure of the mixing equipment is 50-300kg/cm2。
The material mixing equipment is a three-dimensional material mixer.
The invention has the beneficial effects that: the porous carbon material is prepared by reasonably blending the coal-charging dust removal ash, the tar residue and the weakly caking coal, so that on one hand, a new method for utilizing the carbon-containing solid waste is provided, and the technical field of reutilization of the industrial carbon-containing solid waste is widened; on the other hand, the novel high-performance porous carbon material with high porosity, large specific surface area and strong adsorption capacity can be prepared, the practical problem of solid waste treatment in industrial production is solved, and the method has important economic benefits and social environmental protection values.
Detailed Description
The method for preparing the porous carbon material of the present invention will be described in detail with reference to the following embodiments. The scope of the invention is not limited to the following embodiments, which are set forth for illustrative purposes only and are not intended to limit the invention in any way.
Example 1:
1. according to the mass proportion, uniformly mixing 15% of coal-charging dust-removing ash, 50% of tar residue and 35% of weak-viscosity coal for coking, wherein the coal-charging dust-removing ash has the particle size of less than 3mm and is used for preparing the porous carbon material, and the three-dimensional mixer is used for mixing materials, wherein: the particle size of the coal-charging dust-removing ash is 95% when being smaller than 100 meshes, the particle size of the tar residue is 70% when being smaller than 50 meshes, the particle size of the weak sticky coal is 70% when being smaller than 100 meshes, and the average maximum reflectivity of the coal vitrinite group which meets the coal petrology index reaches 1.7%.
2. Uniformly mixing the materials in the step 1 at 180kg/cm2And (5) pressing and forming under a pressure condition.
3. Heating the press-formed sample in the step 2 to 260 ℃ at the speed of 10 ℃/min, staying for 25min, then continuing to heat to 750 ℃ at the same heating speed, introducing carbon dioxide gas at the flow rate of 2L/min, heating to 950 ℃ at the same heating speed, and staying for 2h at the final temperature.
4. Cooling, washing and drying the heat-treated sample obtained in step 3, and measuring the index of the sample to obtain the specific surface area of 1700m2More than g, total pore volume can reach 0.80cm3The volume density is 0.55 g/L, and the iodine adsorption value is 1030 mg/g.
Example 2:
1. according to the mass proportion, 5 percent of coal-charging dust removal ash, 45 percent of tar residue and 50 percent of weak-viscosity coal for coking generated by a gasification furnace for preparing the porous carbon material with the granularity of less than 3mm are uniformly mixed by a three-dimensional mixer, wherein: the proportion of the dust particle size of the coal-charging dust removal ash is less than 100 meshes and 90%, the proportion of the tar residue particle size is less than 50 meshes and 50%, the proportion of the weak sticky coal particle size is less than 100 meshes and 60%, and the average maximum reflectivity of the coal vitrinite group of the weak sticky coal meeting the coal petrography index reaches 1.8%.
2. Mixing the materials in the step 1 uniformly at 200kg/cm2And (5) pressing and forming under a pressure condition.
3. Heating the press-formed sample in the step 2 to 280 ℃ at the speed of 15 ℃/min, staying for 20min, then continuing to heat to 770 ℃ at the same heating speed, introducing steam at the flow rate of 4L/min, heating to 980 ℃ at the final temperature at the same heating speed, and staying for 1.5h at the final temperature.
4. Cooling, washing and drying the heat-treated sample obtained in the step 3, and measuring the index of the sample to obtain the specific surface area of 1650m2More than g, total pore volume can reach 0.73cm3The volume density is 0.50 g/L, and the iodine adsorption value is 950 mg/g.
Example 3:
1. according to the mass proportion, uniformly mixing 15% of coal-charging dust-removing ash, 35% of tar residue and 50% of weak-viscosity coal for coking, wherein the coal-charging dust-removing ash has the particle size of less than 3mm and is used for preparing the porous carbon material, and the three-dimensional mixer is used for mixing materials, wherein: the particle size of the coal-charging dust-removing ash is less than 100 meshes and is 90%, the particle size of the tar residue is less than 50 meshes and is 60%, the particle size of the weak-caking coal is less than 100 meshes and is 80%, and the average maximum reflectivity of the coal vitrinite group of the weak-caking coal meets the coal petrology index and reaches 2.0%.
2. Mixing the materials in the step 1 uniformly at 200kg/cm2And (5) pressing and forming under a pressure condition.
3. Heating the press-formed sample in the step 2 to 300 ℃ at the speed of 12 ℃/min, staying for 23min, then continuing to heat to 800 ℃ at the same heating speed, introducing carbon dioxide gas at the flow rate of 6L/min, heating to 1100 ℃ at the same heating speed, and staying for 1h at the final temperature.
4. Cooling, washing and drying the heat-treated sample obtained in step 3, and measuring the index of the sample to obtain the specific surface area of 1900m2More than g, total pore volume can reach 0.88cm3The specific carbon material product has the advantages of/g, volume density of 0.60 g/L and iodine adsorption value of 1180 mg/g.
Claims (6)
1. A preparation method of a porous carbon material is characterized in that 5% -20% of coal-charging dust removal ash, 20% -55% of tar residue and 15% -50% of weak sticky coal for coking are mixed uniformly by a mixing device for compression molding, the mixture is heated to 240 ℃ for 300 ℃ and stays for not less than 20min, and then the mixture is continuously heated to 800 ℃ and gas is introduced into the mixtureHeating to the final temperature of 900-2More than g, total pore volume greater than 0.7cm3G, bulk density greater than 0.40g/cm3And the iodine adsorption value of the porous carbon material product is 900-1200mg/g, and the percentages are mass percentages.
2. The preparation method of the porous carbon material according to claim 1, wherein the particle size of the coal-charging fly ash, the tar residue and the weak sticky coal for coking is less than 3mm, wherein the proportion of the particle size of the coal-charging fly ash being less than 100 meshes is not less than 80%, the proportion of the particle size of the tar residue being less than 50 meshes is not less than 30%, the proportion of the particle size of the weak sticky coal for coking being less than 100 meshes is not less than 30%, and the coal vitrinite average maximum reflectance meeting the coal petrology index is 1.5-2.3%.
3. The method for preparing a porous carbon material according to claim 1, wherein the heating rate is 8-15 ℃/min.
4. The method for preparing a porous carbon material according to claim 1, wherein the gas is carbon dioxide gas or water vapor, and the gas flow rate is 0.5L/min-10L/min.
5. The preparation method of the porous carbon material according to claim 1, characterized in that the forming pressure of the mixing equipment is 50-300kg/cm2。
6. The preparation method of the porous carbon material according to claim 1, characterized in that the mixing device is a three-dimensional mixer.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4440867A (en) * | 1982-05-14 | 1984-04-03 | Ensotech, Inc. | Calcined, high surface area, particulate matter, processes using this matter, and admixtures with other agents |
| CN1587038A (en) * | 2004-09-08 | 2005-03-02 | 天津大学 | Method for preparing granular active carbon using dust removing carbon as raw material |
| CN108219807A (en) * | 2016-12-13 | 2018-06-29 | 鞍钢股份有限公司 | A kind of preparation method of blast furnace biomass iron coke |
| CN109621893A (en) * | 2018-12-07 | 2019-04-16 | 鞍钢股份有限公司 | A method of activated coke is prepared using chemical industry waste materials containing carbon |
| CN110203927A (en) * | 2019-06-26 | 2019-09-06 | 鞍钢股份有限公司 | A method of active carbon is prepared using coking dead meal as primary raw material |
| CN111139115A (en) * | 2020-01-09 | 2020-05-12 | 包头钢铁（集团）有限责任公司 | Briquette based on tar residues and coking and coal blending method thereof |
-
2020
- 2020-05-29 CN CN202010475954.3A patent/CN111470506A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4440867A (en) * | 1982-05-14 | 1984-04-03 | Ensotech, Inc. | Calcined, high surface area, particulate matter, processes using this matter, and admixtures with other agents |
| CN1587038A (en) * | 2004-09-08 | 2005-03-02 | 天津大学 | Method for preparing granular active carbon using dust removing carbon as raw material |
| CN108219807A (en) * | 2016-12-13 | 2018-06-29 | 鞍钢股份有限公司 | A kind of preparation method of blast furnace biomass iron coke |
| CN109621893A (en) * | 2018-12-07 | 2019-04-16 | 鞍钢股份有限公司 | A method of activated coke is prepared using chemical industry waste materials containing carbon |
| CN110203927A (en) * | 2019-06-26 | 2019-09-06 | 鞍钢股份有限公司 | A method of active carbon is prepared using coking dead meal as primary raw material |
| CN111139115A (en) * | 2020-01-09 | 2020-05-12 | 包头钢铁（集团）有限责任公司 | Briquette based on tar residues and coking and coal blending method thereof |
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