CN112758929A - Waste activated carbon regeneration method - Google Patents
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- CN112758929A CN112758929A CN202110218969.6A CN202110218969A CN112758929A CN 112758929 A CN112758929 A CN 112758929A CN 202110218969 A CN202110218969 A CN 202110218969A CN 112758929 A CN112758929 A CN 112758929A
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- C01B32/00—Carbon; Compounds thereof
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- C01B32/36—Reactivation or regeneration
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Abstract
The invention aims to provide a method for regenerating waste activated carbon, which comprises the steps of firstly using ball milling to enable the size of waste activated carbon particles to be smaller than 200 meshes, then soaking the activated carbon particles and new activated carbon in ammonia water, then adding an active agent, then carrying out ball milling, heating in an inert gas environment after ball milling, and endowing the activated carbon with activity; according to the invention, the effect of endowing the activated carbon with activity is realized by controlling the addition amounts of the waste activated carbon, the new activated carbon and the activating agent and then controlling the temperature rise rate in the inert gas environment, and the iodine value of the activated carbon is ensured.
Description
Technical Field
The invention relates to the field of activated carbon preparation, in particular to a method for regenerating waste activated carbon.
Background
The active carbon has developed pore structure and huge specific surface area, has the dual characteristics of physical adsorption and chemical adsorption, is widely applied to the treatment of toxic and harmful (waste) gas, sewage (waste) water and the like, is entitled 'penicillin' for treating environmental pollution, and plays an important role in protecting the living environment of human beings. The active carbon is widely applied to various fields of production and life due to the adsorption performance, high quality and low price; but the activated carbon does not realize the complete degradation and elimination of the pollutants, but transfers and enriches the pollutants. In addition, the activated carbon has the characteristic of saturated adsorption, and loses adsorption activity after being applied to pollution treatment for a certain time; as a carrier highly enriching pollutants, solid (dangerous) wastes are formed again and can be recycled after regeneration treatment; otherwise, the waste is handed to a qualified solid waste and dangerous waste company and is treated according to the standard. With the increase of the demand of various industries on the activated carbon, the disposal of the waste activated carbon gradually becomes a new problem for the environmental pollution treatment of enterprises.
Disclosure of Invention
In view of the problems of the prior art, it is an object of the present invention to provide a method for regenerating waste activated carbon, which solves the problem of disposal of waste activated carbon.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for regenerating waste activated carbon comprises the following steps:
1) ball-milling the waste activated carbon, and sieving the ball-milled waste activated carbon with a 200-mesh sieve to obtain the ball-milled waste activated carbon;
2) soaking the ball-milled waste activated carbon obtained in the step 1) in ammonia water for 2-3h, and then adding new activated carbon, wherein the mass ratio of the new activated carbon to the waste activated carbon before soaking is 1: 1 to 0.8: 1, then adding an activating agent to obtain a mixture, wherein the mass of the activating agent is 10% of that of the waste activated carbon before soaking;
3) fully ball-milling the mixture obtained in the step 2), wherein the ball-milling speed is 400-500rpm, and the volume ratio of the ball-milling balls to the mixture obtained in the step 2) is 1: 1 to 1.5: 1, obtaining a ball-milled mixture;
4) carrying out solid-liquid separation on the ball-milled mixture obtained in the step 3), heating the solid obtained after the solid-liquid separation to 500 ℃ from room temperature under the condition of a moist inert atmosphere, wherein the heating speed is 5-10 ℃/min, introducing nitric oxide and oxygen when the temperature is raised to 250 ℃, maintaining for 2-3h after the temperature is raised to 500 ℃, then raising the temperature to 1000 ℃ at the speed of 20-30 ℃/min, maintaining for 2-3h after the temperature is raised to 1000 ℃, wherein the atmosphere is inert gas, and cooling to obtain the regenerated activated carbon.
Preferably, the step 1) is to perform ball milling on the waste activated carbon until the powder can pass through a 200-mesh sieve, so as to obtain the ball-milled waste activated carbon.
Preferably, the step 2) is specifically to soak the ball-milled waste activated carbon obtained in the step 1) in ammonia water for 2 hours, and to put new activated carbon after soaking, wherein the mass ratio of the new activated carbon to the waste activated carbon before soaking is 1: 1, then adding an activating agent to obtain a mixture, wherein the mass of the activating agent is 10% of that of the waste activated carbon before soaking.
Preferably, the mass ratio of the potassium chloride to the zinc nitrate is 2:1, and the mass of the activating agent is 10% of that of the waste activated carbon after ball milling.
Preferably, the step 3) is to fully ball mill the mixture obtained in the step 2), the ball milling speed is 400-500rpm, and the volume ratio of the ball milling balls to the mixture obtained in the step 2) is 1.5: and 1, obtaining a ball-milled mixture.
Preferably, the step 4) is specifically to perform solid-liquid separation on the ball-milled mixture obtained in the step 3), heat the solid obtained after the solid-liquid separation to 500 ℃ from room temperature under the condition of a humid nitrogen atmosphere, the heating speed is 10 ℃/min, when the temperature is raised to 250 ℃, introduce nitrogen monoxide and oxygen, heat the solid to 500 ℃ and maintain the temperature for 2 hours, then raise the temperature to 1000 ℃ at the speed of 20 ℃/min, heat the solid to 1000 ℃ and maintain the temperature for 2 hours, wherein the atmosphere is inert gas, and the regenerated activated carbon is obtained after cooling.
Advantageous effects
The regeneration method of the waste activated carbon provided by the invention comprises the steps of firstly enabling the size of waste activated carbon particles to be smaller than 200 meshes by using ball milling, then soaking the activated carbon particles and new activated carbon in ammonia water together, then adding an active agent, then carrying out ball milling, and heating in an inert gas environment after ball milling to endow the activated carbon with activity; according to the invention, the effect of endowing the activated carbon with activity is realized by controlling the addition amounts of the waste activated carbon, the new activated carbon and the activating agent and then controlling the temperature rise rate in the inert gas environment, and the iodine value of the activated carbon is ensured.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for regenerating spent activated carbon, comprising the steps of:
1) ball-milling the waste activated carbon, and sieving the ball-milled waste activated carbon through a 200-mesh sieve to obtain the ball-milled waste activated carbon, wherein the particle size of the ball-milled waste activated carbon is not more than 200 meshes;
2) soaking the ball-milled waste activated carbon obtained in the step 1) in ammonia water for 2 hours, and then adding new activated carbon, wherein the mass ratio of the new activated carbon to the waste activated carbon before soaking is 1: 1, adding an activating agent to obtain a mixture, wherein the mass of the activating agent is 10% of that of the waste activated carbon before soaking, the mass ratio of potassium chloride to zinc nitrate is 2:1, and the mass of the activating agent is 10% of that of the waste activated carbon after ball milling;
3) fully ball-milling the mixture obtained in the step 2), wherein the ball-milling speed is 400rpm, and the volume ratio of the ball-milling balls to the mixture obtained in the step 2) is 1: 1, obtaining a ball-milled mixture;
4) carrying out solid-liquid separation on the ball-milled mixture obtained in the step 3), heating the solid obtained after the solid-liquid separation to 500 ℃ from room temperature under the condition of a moist inert atmosphere, wherein the heating speed is 5 ℃/min, introducing nitric oxide and oxygen when the temperature is raised to 250 ℃, maintaining for 2h after the temperature is raised to 500 ℃, then raising the temperature to 1000 ℃ at the speed of 20 ℃/min, maintaining for 2h after the temperature is raised to 1000 ℃, wherein the ambient atmosphere is inert gas, and cooling to obtain the regenerated activated carbon.
Example 2
A method for regenerating spent activated carbon, comprising the steps of:
1) ball-milling the waste activated carbon, and sieving the ball-milled waste activated carbon through a 200-mesh sieve to obtain the ball-milled waste activated carbon, wherein the particle size of the ball-milled waste activated carbon is not more than 200 meshes;
2) step 2) specifically comprises the steps of soaking the ball-milled waste activated carbon obtained in the step 1) in ammonia water for 2 hours, and then adding new activated carbon, wherein the mass ratio of the new activated carbon to the waste activated carbon before soaking is 1: 1, adding an activating agent to obtain a mixture, wherein the mass of the activating agent is 10% of that of the waste activated carbon before soaking, the mass ratio of potassium chloride to zinc nitrate is 2:1, and the mass of the activating agent is 10% of that of the waste activated carbon after ball milling;
3) fully ball-milling the mixture obtained in the step 2), wherein the ball-milling speed is 400rpm, and the volume ratio of the ball-milling balls to the mixture obtained in the step 2) is 1.5: 1, obtaining a ball-milled mixture;
4) carrying out solid-liquid separation on the ball-milled mixture obtained in the step 3), heating the solid obtained after the solid-liquid separation to 500 ℃ from room temperature under the condition of a moist inert atmosphere, wherein the heating speed is 10 ℃/min, introducing nitric oxide and oxygen when the temperature is raised to 250 ℃, maintaining for 2h after the temperature is raised to 500 ℃, then raising the temperature to 1000 ℃ at the speed of 20 ℃/min, maintaining for 3h after the temperature is raised to 1000 ℃, wherein the ambient atmosphere is inert gas, and cooling to obtain the regenerated activated carbon.
Example 3
A method for regenerating spent activated carbon, comprising the steps of:
1) step 1) specifically, carrying out ball milling on the waste activated carbon until the powder can pass through a 200-mesh sieve, so as to obtain the ball-milled waste activated carbon;
2) soaking the ball-milled waste activated carbon obtained in the step 1) in ammonia water for 2 hours, and then adding new activated carbon, wherein the mass ratio of the new activated carbon to the waste activated carbon before soaking is 0.9: 1, adding an activating agent to obtain a mixture, wherein the mass of the activating agent is 10% of that of the waste activated carbon before soaking, the mass ratio of potassium chloride to zinc nitrate is 2:1, and the mass of the activating agent is 10% of that of the waste activated carbon after ball milling;
3) fully ball-milling the mixture obtained in the step 2), wherein the ball-milling speed is 400-500rpm, and the volume ratio of the ball-milling balls to the mixture obtained in the step 2) is 1.2: 1, obtaining a ball-milled mixture;
4) carrying out solid-liquid separation on the ball-milled mixture obtained in the step 3), heating the solid obtained after the solid-liquid separation to 500 ℃ from room temperature under the condition of a moist inert atmosphere, wherein the heating speed is 8 ℃/min, introducing nitric oxide and oxygen when the temperature is raised to 250 ℃, maintaining for 3h after the temperature is raised to 500 ℃, then raising the temperature to 1000 ℃ at the speed of 30 ℃/min, maintaining for 2h after the temperature is raised to 1000 ℃, wherein the ambient atmosphere is inert gas, and cooling to obtain the regenerated activated carbon.
Example 4
A method for regenerating spent activated carbon, comprising the steps of:
1) ball-milling the waste activated carbon, and sieving the ball-milled waste activated carbon through a 200-mesh sieve to obtain the ball-milled waste activated carbon, wherein the particle size of the ball-milled waste activated carbon is not more than 200 meshes;
2) soaking the ball-milled waste activated carbon obtained in the step 1) in ammonia water for 2.5 hours, and then adding new activated carbon, wherein the mass ratio of the new activated carbon to the waste activated carbon before soaking is 0.9: 1, adding an activating agent to obtain a mixture, wherein the mass of the activating agent is 10% of that of the waste activated carbon before soaking, the mass ratio of potassium chloride to zinc nitrate is 2:1, and the mass of the activating agent is 10% of that of the waste activated carbon after ball milling;
3) fully ball-milling the mixture obtained in the step 2), wherein the ball-milling speed is 450rpm, and the volume ratio of the ball-milling balls to the mixture obtained in the step 2) is 1.3: 1, obtaining a ball-milled mixture;
4) carrying out solid-liquid separation on the ball-milled mixture obtained in the step 3), heating the solid obtained after the solid-liquid separation to 500 ℃ from room temperature under the condition of a moist inert atmosphere, wherein the heating speed is 8 ℃/min, introducing nitric oxide and oxygen when the temperature is raised to 250 ℃, maintaining for 2.5h after the temperature is raised to 500 ℃, then raising the temperature to 1000 ℃ at the speed of 25 ℃/min, maintaining for 2.5h after the temperature is raised to 1000 ℃, wherein the atmosphere is an inert gas, and cooling to obtain the regenerated activated carbon.
Example 5
A method for regenerating spent activated carbon, comprising the steps of:
1) ball-milling the waste activated carbon, and sieving the ball-milled waste activated carbon through a 200-mesh sieve to obtain the ball-milled waste activated carbon, wherein the particle size of the ball-milled waste activated carbon is not more than 200 meshes;
2) soaking the ball-milled waste activated carbon obtained in the step 1) in ammonia water for 2.5 hours, and then adding new activated carbon, wherein the mass ratio of the new activated carbon to the waste activated carbon before soaking is 1: 1 to 0.8: 1, adding an activating agent to obtain a mixture, wherein the mass of the activating agent is 10% of that of the waste activated carbon before soaking, the mass ratio of potassium chloride to zinc nitrate is 2:1, and the mass of the activating agent is 10% of that of the waste activated carbon after ball milling;
3) fully ball-milling the mixture obtained in the step 2), wherein the ball-milling speed is 400-500rpm, and the volume ratio of the ball-milling balls to the mixture obtained in the step 2) is 1: 1 to 1.5: 1, obtaining a ball-milled mixture;
4) carrying out solid-liquid separation on the ball-milled mixture obtained in the step 3), heating the solid obtained after the solid-liquid separation to 500 ℃ from room temperature under the condition of a moist inert atmosphere, wherein the heating speed is 8 ℃/min, introducing nitric oxide and oxygen when the temperature is raised to 250 ℃, maintaining for 2.5h after the temperature is raised to 500 ℃, then raising the temperature to 1000 ℃ at the speed of 25 ℃/min, maintaining for 2.5h after the temperature is raised to 1000 ℃, wherein the atmosphere is an inert gas, and cooling to obtain the regenerated activated carbon.
Example 6
A method for regenerating spent activated carbon, comprising the steps of:
1) ball-milling the waste activated carbon, and sieving the ball-milled waste activated carbon through a 200-mesh sieve to obtain the ball-milled waste activated carbon, wherein the particle size of the ball-milled waste activated carbon is not more than 200 meshes;
2) soaking the ball-milled waste activated carbon obtained in the step 1) in ammonia water for 3 hours, and then adding new activated carbon, wherein the mass ratio of the new activated carbon to the waste activated carbon before soaking is 1: 1, adding an activating agent to obtain a mixture, wherein the mass of the activating agent is 10% of that of the waste activated carbon before soaking, the mass ratio of potassium chloride to zinc nitrate is 2:1, and the mass of the activating agent is 10% of that of the waste activated carbon after ball milling;
3) fully ball-milling the mixture obtained in the step 2), wherein the ball-milling speed is 500rpm, and the volume ratio of the ball-milling balls to the mixture obtained in the step 2) is 1: 1, obtaining a ball-milled mixture;
4) carrying out solid-liquid separation on the ball-milled mixture obtained in the step 3), heating the solid obtained after the solid-liquid separation to 500 ℃ from room temperature under the condition of a moist inert atmosphere, wherein the heating speed is 8 ℃/min, introducing nitric oxide and oxygen when the temperature is raised to 250 ℃, maintaining for 2h after the temperature is raised to 500 ℃, then raising the temperature to 1000 ℃ at the speed of 20 ℃/min, maintaining for 3h after the temperature is raised to 1000 ℃, wherein the ambient atmosphere is inert gas, and cooling to obtain the regenerated activated carbon.
Comparative example 1
Comparative example 1 differs from example 1 only in that the mass ratio of the new activated carbon to the spent activated carbon before soaking was 0.7: 1, other preparation conditions and preparation methods were the same as in example 1.
Comparative example 2
Comparative example 1 differs from example 1 only in that the mass ratio of the new activated carbon to the spent activated carbon before soaking was 1.1: 1, other preparation conditions and preparation methods were the same as in example 1.
Comparative example 3
The difference between the comparative example 3 and the example 1 is that nitrogen monoxide and oxygen are introduced, the temperature is raised to 500 ℃ and then maintained for 2h, then the temperature is raised to 1000 ℃ at the speed of 15 ℃/min, the temperature is raised to 1000 ℃ and then maintained for 2h, the atmosphere is inert gas, and regenerated activated carbon is obtained after cooling, and other preparation conditions are the same as those of the example 1.
Comparative example 4
The difference between the comparative example 4 and the example 1 is that nitrogen monoxide and oxygen are introduced, the temperature is raised to 500 ℃ and then maintained for 2h, then the temperature is raised to 1000 ℃ at the speed of 35 ℃/min, the temperature is raised to 1000 ℃ and then maintained for 2h, the atmosphere is inert gas, and the regenerated activated carbon is obtained after cooling, and other preparation conditions are the same as those of the example 1.
Adsorption measurements were performed on examples 1-6, comparative examples 1-4, and the novel activated carbon, and the results are shown in Table 1, below
| Methylene blue adsorption number (ml) | Iodine adsorbate (mg/g) | |
| Example 1 | 10 | 960 |
| Example 2 | 10 | 980 |
| Example 3 | 10 | 950 |
| Example 4 | 10 | 970 |
| Example 5 | 9 | 960 |
| Example 6 | 11 | 980 |
| Comparative example 1 | 5 | 750 |
| Comparative example 2 | 7 | 800 |
| Comparative example 3 | 6 | 720 |
| Comparative example 4 | 8 | 700 |
| Novel activated carbon | 11 | 1000 |
As can be seen from Table 1, in examples 1 to 6, the methylene blue adsorption value is substantially the same as that of the fresh activated carbon, and the iodine adsorbate is 95% or more of that of the fresh activated carbon, and it can be seen that the activated carbon is activated by the present realization, and the iodine value of the activated carbon is ensured, and in example 1, as can be seen from comparison with comparative examples 1 to 4, the mass ratio of the fresh activated carbon to the waste activated carbon before soaking is controlled to (0.8 to 1): 1, after the temperature is raised to 500 ℃, the temperature raising rate of raising the temperature to 1000 ℃ is controlled to be 20-30 ℃/min, so that the obtained activated carbon has good adsorption effect, and the iodine adsorbate is more than 95% of that of the new activated carbon.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (6)
1. A method for regenerating spent activated carbon, comprising the steps of:
1) ball-milling the waste activated carbon, and sieving the ball-milled waste activated carbon with a 200-mesh sieve to obtain the ball-milled waste activated carbon;
2) soaking the ball-milled waste activated carbon obtained in the step 1) in ammonia water for 2-3h, and then adding new activated carbon, wherein the mass ratio of the new activated carbon to the waste activated carbon before soaking is 1: 1 to 0.8: 1, then adding an activating agent to obtain a mixture, wherein the mass of the activating agent is 10% of that of the waste activated carbon before soaking;
3) fully ball-milling the mixture obtained in the step 2), wherein the ball-milling speed is 400-500rpm, and the volume ratio of the ball-milling balls to the mixture obtained in the step 2) is 1: 1 to 1.5: 1, obtaining a ball-milled mixture;
4) carrying out solid-liquid separation on the ball-milled mixture obtained in the step 3), heating the solid obtained after the solid-liquid separation to 500 ℃ from room temperature under the condition of a moist inert atmosphere, wherein the heating speed is 5-10 ℃/min, introducing nitric oxide and oxygen when the temperature is raised to 250 ℃, maintaining for 2-3h after the temperature is raised to 500 ℃, then raising the temperature to 1000 ℃ at the speed of 20-30 ℃/min, maintaining for 2-3h after the temperature is raised to 1000 ℃, wherein the atmosphere is inert gas, and cooling to obtain the regenerated activated carbon.
2. The method as claimed in claim 1, wherein the step 1) is specifically to ball mill the waste activated carbon until the powder can pass through a 200-mesh sieve, so as to obtain the ball-milled waste activated carbon.
3. The method as claimed in claim 1, wherein the step 2) is specifically to soak the ball-milled waste activated carbon obtained in the step 1) in ammonia water for 2 hours, and to put new activated carbon after soaking, wherein the mass ratio of the new activated carbon to the waste activated carbon before soaking is 1: 1, then adding an activating agent to obtain a mixture, wherein the mass of the activating agent is 10% of that of the waste activated carbon before soaking.
4. The method according to claim 1, wherein the activators potassium chloride and zinc nitrate are used, the mass ratio of potassium chloride to zinc nitrate is 2:1, and the mass of the activators is 10% of that of the waste activated carbon after ball milling.
5. The method as claimed in claim 1, wherein the step 3) is implemented by fully ball-milling the mixture obtained in the step 2), wherein the ball-milling speed is 400-500rpm, and the volume ratio of the ball-milling balls to the mixture obtained in the step 2) is 1.5: and 1, obtaining a ball-milled mixture.
6. The method as claimed in claim 1, wherein the step 4) is specifically to perform solid-liquid separation on the ball-milled mixture obtained in the step 3), heat the solid obtained after the solid-liquid separation from room temperature to 500 ℃ under a humid nitrogen atmosphere at a heating speed of 10 ℃/min, introduce nitrogen monoxide and oxygen when the temperature is raised to 250 ℃, heat the solid to 500 ℃ and maintain the temperature for 2h, then raise the temperature to 1000 ℃ at a speed of 20 ℃/min, heat the solid to 1000 ℃ and maintain the temperature for 2h under an inert atmosphere, and obtain the regenerated activated carbon after cooling.
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| JPS6177615A (en) * | 1984-09-21 | 1986-04-21 | Japan Steel Works Ltd:The | Regeneration of waste powdery active carbon |
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