CN110980728A - Coal slime activated carbon and self-activation preparation method thereof - Google Patents
Coal slime activated carbon and self-activation preparation method thereof Download PDFInfo
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- 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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- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Abstract
The invention discloses a coal slime active carbon and a self-activation preparation method thereof, the method comprises the steps of drying and dehydrating coal slime, uniformly mixing the dried coal slime with coal coke and pitch to prepare coal paste, then pyrolyzing and carbonizing the coal paste in an internal heating type rotary kiln furnace, and finally activating carbonized materials in a self-activation device by adopting water vapor and carbon dioxide as activating agents to obtain the coal slime active carbon. The sludge, the asphalt and the tar adopted by the invention are all solid wastes, the activators such as carbon dioxide, water vapor and the like required by self-activation come from tail gas generated by the multi-hearth furnace of the system, and heat sources required by system drying are all recycled from flue gas waste heat, so that the cost is effectively saved. The specific surface area of the coal slime active carbon is more than 400-850m2The iodine adsorption value is 300-900mg/g, which is close to the adsorption performance of the coal-based activated carbon.
Description
Technical Field
The invention relates to the technical field of preparation processes of environment-friendly materials, in particular to coal slime activated carbon and a self-activation preparation method thereof.
Background
The activated carbon has the advantages of high strength, developed pores, large specific surface area and the like, and is widely applied to the fields of deep purification of drinking water and industrial wastewater, food decolorization, air purification, enrichment and recovery of useful elements and the like. In recent years, with the increasing environmental pollution problem, people pay more and more attention to environmental protection problems such as water treatment, air pollution prevention and control and the like, and the market demand of the activated carbon is larger and larger.
The traditional active carbon is prepared by mainly processing wood or coal as a raw material, and compared with the wood active carbon, the coal active carbon has the advantages of wide raw material source, low price and the like, and occupies a larger proportion in the market. However, the number of coal types suitable for making coal-based activated carbon is not large, and sufficient raw material supply is an important factor for restricting the development of the activated carbon industry.
The yield of the solid waste coal slime produced by the pressure gasification process in the coal chemical industry is about 7000 tons/day in Jiangsu province. At present, the coal slime is mainly used for traditional building engineering and landfill treatment in China. Under the action of factors such as descending of macroscopic economy, lack of effective demand, shrinking of export market, stricter environmental protection policy and the like, the treatment and disposal of coal slime in China face more severe challenges. In order to solve the problem, the activated carbon is prepared by utilizing the coal slime, so that the problem of coal activated carbon raw material supply is solved, the problem of the environment difficult to treat by the coal slime is solved, and the method has important significance for energy conservation and emission reduction.
CN109095467 discloses a method for extracting active carbon from fly ash or its residue after extracting aluminum, which needs diesel oil, kerosene, motor oil or fuel oil as collecting agent, octanol, terpineol oil, fusel oil and GF oil as flotation agent to increase carbon content, and needs additional water vapor and activating agent such as carbon dioxide. However, the collecting agent, the flotation agent and the activating agent used in the application increase the preparation cost of the activated carbon, and the concept of energy conservation and emission reduction by waste utilization cannot be effectively embodied.
Disclosure of Invention
The invention aims to provide the coal slime activated carbon prepared by the self-activation preparation method aiming at the defects in the prior art.
The invention also aims to provide a preparation method of the coal slime through active self-activation.
The purpose of the invention is realized by the following technical scheme:
a coal slime activated carbon self-activation preparation method comprises the following specific steps:
step 1, drying and dehydrating solid waste coal slime generated by a pressure gasification process in the coal chemical industry to obtain dry coal slime.
And 2, uniformly mixing the dried coal slime, coking coal and a binder to prepare coal paste, wherein the weight contents of the components are 45-55% of the dried coal slime, 30-35% of the coking coal and 15-20% of the binder respectively, and granulating and molding the coal paste to obtain granular materials with the grain diameter of 3.0-10.0 mm.
Step 3, carrying out pyrolysis and carbonization on the granular materials in an internal heating type rotary kiln or an internal heating type tunnel kiln, wherein the pyrolysis and carbonization temperature is between 200 ℃ and 750 ℃, and the pyrolysis and carbonization time is controlled to be 20-50 min; obtaining a carbonized material; and (3) continuing to serve as a heat source for drying and dehydrating the coal slime in the step 1 by combustible gas generated by pyrolysis and carbonization.
Step 4, adopting steam and carbon dioxide as activating agents in a self-activating device, and activating the carbonized material obtained in the step 3, wherein the activation temperature is controlled to be between 750 and 900 ℃, the activation time is controlled to be 1-2 h, and the dosage ratio of the activating agents to the non-combustible carbon after carbonization is 0.5-6:1 by weight; and cooling with water to obtain the coal slime active carbon.
In a further design scheme of the invention, the fixed carbon content of the coal slime produced by the ammonia synthesis gasification furnace in the step 1 is 30-50%, the drying and dehydration are carried out in a flash evaporation drying furnace, the flash evaporation temperature is 120-150 ℃, and the water content of the coal slime after drying and dehydration is lower than 15%.
In a further design scheme of the invention, the adhesive in Zhongshan city in the step 2 is asphalt and tar, and dried coal slime and coking coal are required to be sieved by a 300-mesh sieve.
In a further design of the invention, the volatile content of the carbonized material obtained in step 3 is less than 11%.
In a further design scheme of the invention, the pyrolysis carbonization temperature is between 300 ℃ and 450 ℃, and the pyrolysis carbonization time is controlled within 30-45 min.
In a further design scheme of the invention, the activation temperature in the step 4 is 800-.
In a further embodiment of the invention, the ratio of the amount of activator to the amount of unburned carbon after the carbonization in step 4 is 1-2: 1.
In a further design scheme of the invention, the self-activating device in the step 4 is a multi-stage rake furnace, and the high concentration CO and H is generated in the activation process2The tail gas is combusted to generate carbon dioxide and water vapor, and then the carbon dioxide and the water vapor return to the self-activation device to activate the activated carbon.
The coal slime activated carbon prepared by the coal slime activated carbon self-activation preparation method has the specific surface area of more than 400-850m2/g and the iodine adsorption value of 900 mg/g.
Compared with the prior art, the invention has the following outstanding beneficial effects:
in the coal slime activated carbon self-activation preparation method, the adopted sludge, asphalt and tar are solid wastes, the activators such as carbon dioxide, water vapor and the like required by self-activation come from tail gas generated by a multi-hearth furnace of the system, and heat sources required by system drying come from flue gas waste heat recycling, so that the cost is effectively saved.
The specific surface area of the coal slime active carbon obtained by the method is larger than 400-850m2/g, the iodine adsorption value is 300-900mg/g, the specific surface area is close to the adsorption performance of the coal active carbon, the method can be widely used for purification treatment of waste gas and waste water, the purpose of preparing waste from waste is achieved, and the method has good social benefit, economic benefit and application prospect.
Drawings
FIG. 1 is a flow chart of the recycling of the activating agent and the heat source in the example.
Detailed Description
The invention is further explained below with reference to the drawings and examples.
Example 1
The invention discloses a coal slime activated carbon self-activation preparation method, which comprises the following specific steps:
step 1, drying and dehydrating solid waste coal slime generated by a pressure gasification process in the coal chemical industry, firstly carrying out primary dehydration on the coal slime by plate-and-frame filter pressing, wherein the water content of the coal slime subjected to plate-and-frame filter pressing is about 60% generally, then conveying the coal slime into a flash evaporation drying furnace by a screw conveyor for dehydration, wherein the water content is required to be not more than 15% generally, and then crushing the coal slime into 200-mesh coal powder by a grinding process to obtain the dried coal slime.
Step 2, uniformly mixing the dried coal slime with coking coal and a binder to prepare coal paste, wherein the weight contents of the components are respectively 50% of the dried coal slime, 30% of the coking coal and 20% of the binder, and the binder is prepared from the following components in percentage by mass: 1, the fineness of coking coal powder requires that the passing rate of 300 meshes is more than 90 percent, and the coal paste is granulated and formed to obtain granular materials with the grain diameter of 10.0 mm.
3, carrying out pyrolysis and carbonization on the granular materials in an internal heating type rotary kiln or an internal heating type tunnel kiln, wherein the pyrolysis and carbonization temperature is 550 ℃, and the pyrolysis and carbonization time is controlled to be 30 min; obtaining a carbonized material; volatile matters in the carbonized materials are less than 11%, and combustible gas generated by pyrolysis and carbonization is continuously used as a heat source for drying and dehydrating the coal slime in the step 1.
The carbonization furnace produces carbonized products from the formed strip-shaped materials in the converter at a certain temperature according to the mode of convection operation, so that the volatile matter of the carbonized products is reduced to below 11 percent, the products are ensured not to be mutually bonded in the activation furnace, and the carbonized products have preliminary pore structures. The main working principle of the rotary kiln carbonization furnace is as follows: the coal gas and the like are combusted in the combustion chamber, the hot flue gas flows to the front end from the tail part of the furnace body and is directly contacted with materials coming from the reverse direction, the materials flow to the tail part of the furnace body along with the flowing of the materials, the temperature is gradually increased, and the materials are subjected to drying, devolatilization and carbonization processes and finally discharged from the tail part to enter a cold stock ground. The furnace body is inclined at an angle of 2-5 degrees and rotates slowly during operation, and a spiral material pushing plate is arranged inside the front end of the furnace body to push the material box to flow in front. The final carbonization temperature is generally 300-750 ℃; the carbonization temperature gradient should also be set in detail, generally speaking, when using converter carbonization, the temperature at the tail of the converter is generally not allowed to exceed 300 ℃, and the temperature near the discharge port is 750 ℃. For the carbonization mode of the internal heating converter, the final temperature is controlled by regulating and controlling the temperature of a furnace end combustion chamber, the furnace tail temperature and the temperature gradient distribution along the axial direction of the furnace body are regulated and controlled by the length and the rotating speed of the furnace body and the draft of a flue, and when the length and the rotating speed of the furnace body are fixed, the draft is adjusted to partially realize the temperature distribution regulation and control function.
Step 4, conveying the carbonized granular material to a multi-hearth furnace for activation, adopting steam and carbon dioxide as activating agents in the multi-hearth furnace of a self-activation device, and performing activation treatment on the carbonized material obtained in the step 3, wherein the activation temperature is controlled to be 800 ℃, the activation time is controlled to be 1.5h, and the using amount ratio of the activating agents to the carbonized non-combustible carbon is 2:1 by weight; and cooling with water to obtain coal slime active carbon with the particle size of 10.0 mm.
The detection shows that the iodine adsorption value of the coal slime active carbon is more than or equal to 300 mg/g, the strength is more than or equal to 97 percent, the apparent density is 0.6 g/cm, and the ignition point is more than 400 ℃. The adsorption performance of the coal-based activated carbon is close to that of the coal-based activated carbon.
The multistage rake furnace is a cylinder type made of vertical steel plates, a shell is lined with refractory materials, the interior of the multistage rake furnace is built by refractory bricks, the multistage rake furnace is divided into six sections of hearths from top to bottom, each section of hearth is respectively provided with a discharge port around the hearths and in the center of the hearth, the activated carbon moves and stirs in the hearths and is driven by a low-rotation-speed central shaft, stirring teeth are arranged below stirring arms of each layer, the activated carbon moves to an inner side discharge port from the outer side of the 1 st section of hearth and falls into the inner side of the 2 nd section of hearth, the activated carbon is moved to an outer side discharge port from the inner side of the hearth by the 2 nd section of stirring teeth and falls into the inner side of the 3. Due to the action of the stirring teeth, the activated carbon exchanges heat with high-temperature flue gas of a burner in the furnace, and is in high-convection-advection multi-shear contact with the steam for regeneration, and mass transfer and chemical reaction processes occur. The central shaft and the stirring arm arranged in the center of the furnace are designed by air interlayers, and are forcibly cooled by a special shaft cold air vehicle so as to protect the material and the operation stability of the structures of the central shaft and the harrow arm.
The multi-hearth furnace is controlled to operate under the condition that the oxygen content is below 1 percent, so that the exhaust gas of the activated carbon activation furnace contains high-concentration CO and H2After setting upThe chamber is heated to over 1100 ℃ again to completely oxidize the waste gas into CO2And H2And O. The high-temperature flue gas discharged from the post-combustion chamber has heat recovery value, and a waste heat boiler is generally adopted to recover the waste heat of the flue gas and produce process steam required by the regeneration process.
The central shaft cooling air can be heated when passing through the central shaft, and the heated air serving as one part of the combustion-supporting air can raise the temperature of the combustion-supporting air, so that the fuel gas consumption is saved.
The steam required by the activated carbon in the activation process is high-temperature steam generated by a multi-section rake type furnace waste heat boiler, the steam generation capacity of the waste heat boiler is about 2.0 tons/h by accounting for 10000 tons/year of activated carbon capacity, and the steam amount required in the activated carbon activation process can be completely met.
FIG. 1 is a flow chart of the recycling of an activating agent and a heat source in the invention, a material after granulation and molding enters a carbonization furnace for pyrolysis and carbonization, the carbonized material continues to enter a multi-hearth furnace for activation, combustible tail gas generated by the carbonization furnace and an activation furnace enters an incinerator for incineration, the temperature of flue gas at an outlet of the incinerator is 1100 ℃, the flue gas flows into a subsequent waste heat boiler for cooling, the outlet temperature is 500 ℃, part of waste heat steam after cooling is used as a drying heat source in step 1, and part of CO is used as a drying heat source in step 12And H20, the residual tail gas enters a tail gas treatment unit for treatment, so that the environmental pollution is avoided. The process has the greatest advantages that the heat source required by drying, the carbon dioxide and the water vapor required by activation are recycled from tail gas generated in the system, and the energy of the system is saved.
Example 2
The self-activation preparation method of the coal slime activated carbon comprises the following specific steps:
step 1, drying and dehydrating solid waste coal slime produced by a pressure gasification process in the coal chemical industry, and crushing the coal slime into 300-mesh coal powder through a grinding process to obtain the dried coal slime.
And 2, uniformly mixing the dried coal slime, coking coal and a binder to prepare coal paste, wherein the weight contents of the components are 45% of the dried coal slime, 35% of the coking coal and 20% of the binder respectively, and granulating and molding the coal paste to obtain granular materials with the grain diameter of 4.0 mm.
3, carrying out pyrolysis and carbonization on the granular materials in an internal heating type rotary kiln or an internal heating type tunnel kiln, wherein the pyrolysis and carbonization temperature is 200 ℃, and the pyrolysis and carbonization time is controlled to be 50 min; obtaining a carbonized material; and (3) continuing to serve as a heat source for drying and dehydrating the coal slime in the step 1 by combustible gas generated by pyrolysis and carbonization.
Step 4, adopting water vapor and carbon dioxide as activating agents in a self-activating device multi-hearth furnace, carrying out activation treatment on the carbonized material obtained in the step 3, controlling the activation temperature at 7500 ℃, controlling the activation time at 2 h, and controlling the dosage ratio of the activating agents to the carbonized unburned carbon to be 6:1 by weight; and cooling with water to obtain coal slime active carbon with the particle size of 4.0 mm.
The detection shows that the iodine adsorption value of the coal slime active carbon is 650 mg/g, the strength is more than or equal to 95 percent, the apparent density is 0.5 g/cm, and the ignition point is more than 400 ℃.
The above are preferred embodiments of the present invention, and all changes made according to the technical scheme of the present invention that produce functional effects do not exceed the scope of the technical scheme of the present invention belong to the protection scope of the present invention.
Claims (9)
1. A coal slime activated carbon self-activation preparation method comprises the following specific steps:
step 1, drying and dehydrating solid waste coal slime generated by a pressure gasification process in the coal chemical industry to obtain dried coal slime;
step 2, uniformly mixing the dried coal slime, coking coal and a binder to prepare coal paste, wherein the weight contents of all components are 45-55% of the dried coal slime, 30-35% of the coking coal and 15-20% of the binder respectively, and granulating and molding the coal paste to obtain granular materials with the grain diameter of 3.0-10.0 mm;
step 3, carrying out pyrolysis and carbonization on the granular materials in an internal heating type rotary kiln or an internal heating type tunnel kiln, wherein the pyrolysis and carbonization temperature is between 200 ℃ and 750 ℃, and the pyrolysis and carbonization time is controlled to be 20-50 min; obtaining a carbonized material; combustible gas generated by pyrolysis and carbonization is continuously used as a heat source for drying and dehydrating the coal slime in the step 1;
step 4, adopting steam and carbon dioxide as activating agents in a self-activating device, and activating the carbonized material obtained in the step 3, wherein the activation temperature is controlled to be between 750 and 900 ℃, the activation time is controlled to be 1-2 h, and the dosage ratio of the activating agents to the non-combustible carbon after carbonization is 0.5-6:1 by weight; and cooling with water to obtain the coal slime active carbon.
2. The self-activation preparation method of coal slime activated carbon as claimed in claim 1, wherein the fixed carbon content of the coal slime produced by the ammonia synthesis gasification furnace in the step 1 is 30% -50%, the drying and dehydration are carried out in a flash evaporation drying furnace, the flash evaporation temperature is 120-150 ℃, and the water content of the coal slime after the drying and dehydration is lower than 15%.
3. The self-activation preparation method of coal slime activated carbon as claimed in claim 1, wherein the binder in step 2 is asphalt and tar, and the dried coal slime and coking coal are required to be sieved by a 300-mesh sieve.
4. The self-activation preparation method of coal slime activated carbon as claimed in claim 1, wherein the volatile matter in the carbonized material obtained in step 3 is less than 11%.
5. The coal slime activated carbon self-activation preparation method as claimed in claim 1, wherein the pyrolysis carbonization temperature is between 300 ℃ and 450 ℃, and the pyrolysis carbonization time is controlled within 30-45 min.
6. The self-activation preparation method of coal slime activated carbon as recited in claim 1, wherein the activation temperature in step 4 is 800-850 ℃, and the activation time is 1.5 h.
7. The self-activation preparation method of coal slime activated carbon as claimed in claim 1, wherein the dosage ratio of the activating agent to the carbonized unburned carbon in the step 4 is 1-2: 1.
8. The self-activation preparation method of coal slime activated carbon as claimed in claim 1, wherein the self-activation device in the step 4 is a multi-stage deviceRake furnace, high concentration CO and H produced during activation2The tail gas is combusted to generate carbon dioxide and water vapor, and then the carbon dioxide and the water vapor return to the self-activation device to activate the activated carbon.
9. The coal slime activated carbon prepared by the coal slime activated carbon self-activation preparation method as set forth in claims 1-8, the specific surface area of the coal slime activated carbon is more than 400-2The iodine adsorption value is 300-900 mg/g.
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Cited By (6)
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| CN111533126A (en) * | 2020-05-22 | 2020-08-14 | 东华大学 | Preparation method of high-compressive-strength high-porosity formed sludge activated carbon |
| CN112830489A (en) * | 2021-01-20 | 2021-05-25 | 煤炭科学技术研究院有限公司 | Resourceful treatment method for coal tar residues |
| CN113184844A (en) * | 2021-05-25 | 2021-07-30 | 马鞍山钢铁股份有限公司 | Method for preparing activated carbon by using carbon-containing dust and mud |
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| CN115007107A (en) * | 2022-06-14 | 2022-09-06 | 浙江工业大学 | Method for efficiently utilizing coffee grounds in cooperation with municipal sludge through thermal conversion |
| CN115321535A (en) * | 2022-07-28 | 2022-11-11 | 中国矿业大学 | Preparation method of coal slime-based activated carbon |
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| CN115007107A (en) * | 2022-06-14 | 2022-09-06 | 浙江工业大学 | Method for efficiently utilizing coffee grounds in cooperation with municipal sludge through thermal conversion |
| CN115321535A (en) * | 2022-07-28 | 2022-11-11 | 中国矿业大学 | Preparation method of coal slime-based activated carbon |
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