CN113713794B - Desulfurization activated carbon regeneration system and method using microwave coupling hydrogen peroxide - Google Patents
Desulfurization activated carbon regeneration system and method using microwave coupling hydrogen peroxide Download PDFInfo
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- CN113713794B CN113713794B CN202111052994.8A CN202111052994A CN113713794B CN 113713794 B CN113713794 B CN 113713794B CN 202111052994 A CN202111052994 A CN 202111052994A CN 113713794 B CN113713794 B CN 113713794B
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3416—Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3441—Regeneration or reactivation by electric current, ultrasound or irradiation, e.g. electromagnetic radiation such as X-rays, UV, light, microwaves
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
Abstract
The invention belongs to the technical field of desulfurization catalyst regeneration, and relates to a desulfurization activated carbon regeneration system and method by utilizing microwave coupling hydrogen peroxide, wherein the system comprises an activated carbon regeneration tower, a microwave generator and a spraying device for spraying a solution into the activated carbon regeneration tower, and the microwave generator is arranged on the activated carbon regeneration tower; and the active carbon regeneration tower is also connected with a purging pipeline, a drainage pipeline and a tail gas discharge pipeline. When regeneration is carried out, the microwave generator and the spraying device are started, a large amount of hydroxyl free radicals can be generated under the condition that microwave radiation and hydrogen peroxide coexist, and then sulfur simple substances adsorbed in the activated carbon are oxidized to generate sulfate radicals, so that desulfurization regeneration is realized; and the potassium dichromate is utilized to further remove sulfur simple substance in the activated carbon, and the chromium element remained on the activated carbon plays a catalytic role, so that the desulfurization efficiency of the activated carbon is increased. The regeneration method has short time, low cost and high efficiency, can produce byproducts with economic value, and does not cause secondary pollution.
Description
Technical Field
The invention belongs to the technical field of desulfurization activated carbon regeneration, and particularly relates to a desulfurization activated carbon regeneration system and method by utilizing microwave coupling hydrogen peroxide.
Background
Activated carbon is widely used for purifying waste water and waste gas, such as adsorbing dyes in water or removing sulfides in blast furnace gas, because of the advantages of low cost, good treatment effect, simple process equipment and the like. But is limited by the specific surface area and pore volume of the activated carbon, and the treatment effect is greatly reduced after the adsorption capacity reaches saturation. If the waste activated carbon is directly treated, or a larger landfill site is needed for landfill treatment, or the waste of resources is caused, serious pollution is caused to the atmospheric environment, and high cost is paid. Therefore, the method has obvious advantages and significance in the application of the economic value and environment-friendly regeneration technology, namely, the method releases the pore canal of the surface of the activated carbon occupied by pollutants through the regeneration means and restores the adsorption capacity of the activated carbon.
The common active carbon regeneration method in the technology is a thermal regeneration method, a solvent method and the like. The thermal regeneration method is to treat waste activated carbon at high temperature under a certain gas atmosphere, and as disclosed in Chinese patent document with publication number of CN201711361255, an activated carbon regeneration device and a regeneration method thereof are disclosed, and the thermal regeneration method and related equipment are described. The thermal regeneration method has the advantages of high regeneration efficiency, short time, universality on adsorbates and the like, but has high cost and large carbon loss, and most of the method is to forcedly replace or release substances adsorbed in the waste activated carbon, does not degrade and remove the substances, and is easy to generate harmful gases. The solvent law refers to a method for regenerating waste activated carbon by immersing the waste activated carbon in a specific solution, and common solvents include inorganic solvents (hydrochloric acid, sodium hydroxide solution and the like) and organic solvents (benzene, methanol and the like), and the method has the advantages that useful substances can be recovered through recovery waste liquid in the regeneration process, carbon loss is small, regeneration efficiency is low, a large amount of waste water is generated, and the activated carbon is easily corroded by chemicals.
Disclosure of Invention
In view of the above, the present invention aims to solve the above-mentioned drawbacks of the regeneration method, and provides a desulfurization activated carbon regeneration system and method using microwave-coupled hydrogen peroxide.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the desulfurization activated carbon regeneration system utilizing the microwave coupling hydrogen peroxide comprises an activated carbon regeneration tower, a microwave generator and a spraying device for spraying a solution into the activated carbon regeneration tower, wherein the microwave generator is arranged on the activated carbon regeneration tower; and the active carbon regeneration tower is also connected with a purging pipeline, a drainage pipeline and a tail gas discharge pipeline.
Further, the spraying device comprises a hydrogen peroxide storage tank, a potassium dichromate storage tank and a plurality of nozzles, wherein the nozzles are arranged at the top of the active carbon regeneration tower and are respectively communicated with the hydrogen peroxide storage tank and the potassium dichromate storage tank through pipelines; and regulating valves and cut-off valves are arranged on connecting pipelines between the nozzle and the hydrogen peroxide storage tank and between the nozzle and the potassium dichromate storage tank.
Further, all be equipped with the trip valve on sweeping pipeline, drainage pipe, the exhaust emission pipeline, all still be equipped with the blast gate on sweeping pipeline and the exhaust emission pipeline.
Further, the output power of the microwave generator is 250-1000W and is continuously adjustable, and the emission time is 0-9999 min and is continuously adjustable.
The desulfurization activated carbon regeneration method by utilizing the microwave coupling hydrogen peroxide adopts the desulfurization activated carbon regeneration system by utilizing the microwave coupling hydrogen peroxide, and comprises the following steps:
1) Acquiring the weight of the active carbon to be regenerated, and setting heating parameters of a microwave generator according to the weight; meanwhile, adding the hydrogen peroxide with the set concentration into a hydrogen peroxide storage tank;
2) The method comprises the steps of presetting the required output power and the emission time of a microwave generator according to the weight of active carbon to be regenerated;
3) Closing a purging pipeline, a drainage pipeline and a tail gas discharge pipeline, and starting a microwave generator to heat the activated carbon; after heating to a set temperature, opening a hydrogen peroxide storage tank, controlling the flow of hydrogen peroxide through a regulating valve, spraying hydrogen peroxide into an activated carbon regeneration tower through a nozzle, and removing sulfur adsorbed in activated carbon by oxidizing elemental sulfur with hydrogen peroxide;
4) After the emission time is over, closing the microwave generator and the spraying device, opening a drainage pipeline, and discharging the generated solution;
5) Opening a potassium dichromate storage tank, introducing a potassium dichromate solution into the activated carbon regeneration tower through a nozzle, removing elemental sulfur remained on the activated carbon, and enabling the activated carbon to adsorb chromium elements; then a drainage pipeline is opened to drain the generated solution;
6) After the solution is discharged, closing the drainage pipeline, opening the purging pipeline and the tail gas discharge pipeline, blowing inert gas into the activated carbon regeneration tower through the purging pipeline, purging, discharging residual gas in the activated carbon regeneration tower from the tail gas discharge pipeline, and completing the regeneration of the activated carbon.
Further, the concentration of the hydrogen peroxide solution in the hydrogen peroxide storage tank is 1-30%.
Further, the ratio of the emission time of the microwave generator to the weight of the active carbon is 0.5:1-2:1, and the temperature of the active carbon is controlled to be 80-600 ℃; wherein, the emission time unit is minutes, and the mass unit of the activated carbon is grams.
Further, the inert gas is nitrogen or argon.
Further, the flow rate of the inert gas is controlled to be 1-5L/min, and the ratio of the purging time to the weight of the activated carbon is 1:1-5:1; wherein the purging time unit is minutes, and the mass unit of the activated carbon is grams.
Further, the activated carbon is one or a mixture of a plurality of coal activated carbon, biomass activated carbon and wood activated carbon.
The invention has the beneficial effects that:
1) The invention realizes the rapid regeneration of the waste desulfurization active carbon, and the regenerated active carbon has high sulfur capacity recovery rate, small mechanical abrasion of the active carbon, low hydrogen peroxide and microwave generation operation cost and recyclable waste liquid.
2) The regeneration tower can adopt a fixed bed or moving bed process, no moving equipment is arranged in the tower, and the damage of the desulfurization catalyst is small.
3) In the invention, hydrogen peroxide solution is firstly used for desulfurization treatment, and under the condition of the coexistence of microwave radiation and hydrogen peroxide, a large amount of hydroxyl free radicals can be generated, so that sulfur simple substance adsorbed in the activated carbon is oxidized to generate sulfate radical; then potassium dichromate solution is introduced, and on the one hand, the potassium dichromate can remove untreated elemental sulfur on the activated carbon; on the other hand, the active carbon is used for removing sulfides, and chromium element remained on the active carbon can participate in the desulfurization process after the active carbon is regenerated, so that the catalytic effect is achieved, and the desulfurization efficiency of the active carbon is increased.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objects and other advantages of the invention may be realized and obtained by means of the instrumentalities and combinations particularly pointed out in the specification.
Drawings
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in the following preferred detail with reference to the accompanying drawings, in which:
FIG. 1 is a schematic diagram of a desulfurization activated carbon regeneration system using microwave-coupled hydrogen peroxide in the present invention;
reference numerals: 1-an active carbon regeneration tower; 2-a microwave generator; 3-spraying device; 4-purging the pipeline; 5-an air valve; 6-a shut-off valve; 7-a regulating valve; 8-a shut-off valve; 9-a hydrogen peroxide storage tank; 10-a drainage pipeline; 11-a shut-off valve; 12-an exhaust emission pipeline; 13-an air valve; 14-a shut-off valve; 15-a regulating valve; 16-a shut-off valve; 17-potassium dichromate storage tank.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention. It should be noted that the illustrations provided in the following embodiments merely illustrate the basic idea of the present invention by way of illustration, and the following embodiments and features in the embodiments may be combined with each other without conflict.
Wherein the drawings are for illustrative purposes only and are shown in schematic, non-physical, and not intended to limit the invention; for the purpose of better illustrating embodiments of the invention, certain elements of the drawings may be omitted, enlarged or reduced and do not represent the size of the actual product; it will be appreciated by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.
The same or similar reference numbers in the drawings of embodiments of the invention correspond to the same or similar components; in the description of the present invention, it should be understood that, if there are terms such as "upper", "lower", "left", "right", "front", "rear", etc., that indicate an azimuth or a positional relationship based on the azimuth or the positional relationship shown in the drawings, it is only for convenience of describing the present invention and simplifying the description, but not for indicating or suggesting that the referred device or element must have a specific azimuth, be constructed and operated in a specific azimuth, so that the terms describing the positional relationship in the drawings are merely for exemplary illustration and should not be construed as limiting the present invention, and that the specific meaning of the above terms may be understood by those of ordinary skill in the art according to the specific circumstances.
Example 1
Referring to fig. 1, the desulfurization activated carbon regeneration system using microwave coupling hydrogen peroxide comprises an activated carbon regeneration tower 1, a microwave generator 2 and a spraying device 3 for spraying a solution into the activated carbon regeneration tower 1, wherein the microwave generator 2 is arranged on the side wall of the activated carbon regeneration tower 1; the active carbon regeneration tower 1 is also connected with a purging pipeline 4, a drainage pipeline 10 and a tail gas discharge pipeline 12.
The spraying device 3 comprises a hydrogen peroxide storage tank 9, a potassium dichromate storage tank 17 and a plurality of nozzles, wherein the nozzles are arranged at the top of the active carbon regeneration tower 1, and the nozzles are respectively communicated with the hydrogen peroxide storage tank 9 and the potassium dichromate storage tank 17 through pipelines; and the regulating valve 7, the cut-off valve 8, the regulating valve 15 and the cut-off valve 16 are arranged on the connecting pipelines between the nozzle and the hydrogen peroxide storage tank 9 and between the nozzle and the potassium dichromate storage tank 17.
Wherein, install the trip valve 6 on the purge line 4, install the trip valve 11 on the drain line 10, install the trip valve 14 on the exhaust emission pipeline 12, still install the blast gate 5 on the purge line 4, still install blast gate 13 on the exhaust emission pipeline 12.
The output power of the microwave generator 2 is 250-1000W and is continuously adjustable, and the emission time is 0-9999 min and is continuously adjustable.
The desulfurization activated carbon regeneration method by utilizing the microwave coupling hydrogen peroxide adopts the desulfurization activated carbon regeneration system by utilizing the microwave coupling hydrogen peroxide, and comprises the following steps:
1) Acquiring the weight of the active carbon to be regenerated, and setting heating parameters of the microwave generator 2 according to the weight; meanwhile, adding the hydrogen peroxide with the set concentration into a hydrogen peroxide storage tank 9;
2) The required output power and emission time of the microwave generator 2 are preset according to the weight of the active carbon to be regenerated;
3) Closing the purging pipeline 4, the drainage pipeline 10 and the tail gas discharge pipeline 12, and starting the microwave generator 2 to heat the activated carbon; after heating to a set temperature, opening a hydrogen peroxide storage tank 9, controlling the flow of hydrogen peroxide through a regulating valve 7, spraying hydrogen peroxide into the activated carbon regeneration tower 1 through a nozzle, and removing sulfur adsorbed in the activated carbon by oxidizing elemental sulfur with hydrogen peroxide;
4) After the emission time is over, closing the microwave generator 2 and the spraying device 3, opening the drainage pipeline 10, and discharging the generated solution;
5) Opening a potassium dichromate storage tank 17, controlling the flow of the potassium dichromate solution through a regulating valve 15, introducing the potassium dichromate solution into the activated carbon regeneration tower 1 through a nozzle, removing elemental sulfur remained on the activated carbon, and enabling the activated carbon to adsorb chromium elements; then the drainage pipeline 10 is opened to drain the generated solution;
6) After the solution is discharged, closing the drainage pipeline 10, opening the purging pipeline 4 and the tail gas discharge pipeline 12, blowing nitrogen or argon into the activated carbon regeneration tower 1 through the purging pipeline 4 for purging, and controlling the flow of inert gas to be 1-5L/min, wherein the ratio of the purging time to the weight of the activated carbon is 1:1-5:1; wherein the purging time unit is minutes, and the mass unit of the activated carbon is gram; and discharging residual gas in the activated carbon regeneration tower 1 from the tail gas discharge pipeline 12, and completing the activated carbon regeneration.
Wherein, the weight of the active carbon to be desulfurized is 100g, the active carbon is loaded into an active carbon regeneration tower, the microwave generation time is set to be 60min, the output power is 800w, the temperature of the active carbon is controlled to be 80 ℃, the concentration of hydrogen peroxide is 10%, and the waste desulfurized active carbon is regenerated.
Example 2
The difference between the embodiment and the embodiment 1 is that the weight of the active carbon to be desulfurized is 100g, the active carbon is loaded into an active carbon regeneration tower, the microwave generation time is set to be 120min, the output power is 600w, and the temperature of the active carbon is controlled to be 200 ℃; the concentration of hydrogen peroxide is 20%, and the waste desulfurization activated carbon is regenerated.
The saturated sulfur capacity of the regenerated active carbon obtained in the example 1 and the regenerated active carbon obtained in the example 2 are measured, wherein the saturated sulfur capacity of the regenerated active carbon in the example 1 reaches 150mg/g and reaches 42.9% of the original saturated sulfur capacity; the saturated sulfur capacity of the regenerated active carbon in the example 2 reaches 188mg/g and reaches 53.7% of the original saturated sulfur capacity.
Finally, it is noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the present invention, which is intended to be covered by the claims of the present invention.
Claims (6)
1. A desulfurization activated carbon regeneration method by utilizing microwave coupling hydrogen peroxide is characterized in that: regenerating the desulfurization activated carbon by adopting a desulfurization activated carbon regeneration system utilizing microwave coupling hydrogen peroxide;
the desulfurization activated carbon regeneration system utilizing the microwave coupling hydrogen peroxide comprises an activated carbon regeneration tower, a microwave generator and a spraying device, wherein the spraying device is used for spraying a solution into the activated carbon regeneration tower; the active carbon regeneration tower is also connected with a purging pipeline, a drainage pipeline and a tail gas discharge pipeline; the spraying device comprises a hydrogen peroxide storage tank, a potassium dichromate storage tank and a plurality of nozzles, wherein the nozzles are arranged at the top of the active carbon regeneration tower and are respectively communicated with the hydrogen peroxide storage tank and the potassium dichromate storage tank through pipelines; the connecting pipelines between the nozzle and the hydrogen peroxide storage tank and between the nozzle and the potassium dichromate storage tank are respectively provided with a regulating valve and a cut-off valve;
the purging pipeline, the drainage pipeline and the tail gas discharge pipeline are respectively provided with a cut-off valve, and the purging pipeline and the tail gas discharge pipeline are respectively provided with an air valve;
the output power of the microwave generator is 250-1000W, and the emission time is 60-9999 min;
the regeneration method comprises the following steps:
1) Acquiring the weight of the active carbon to be regenerated, and setting heating parameters of a microwave generator according to the weight; meanwhile, adding the hydrogen peroxide with the set concentration into a hydrogen peroxide storage tank;
2) The method comprises the steps of presetting the required output power and the emission time of a microwave generator according to the weight of active carbon to be regenerated;
3) Closing a purging pipeline, a drainage pipeline and a tail gas discharge pipeline, and starting a microwave generator to heat the activated carbon; after heating to a set temperature, opening a hydrogen peroxide storage tank, controlling the flow of hydrogen peroxide through a regulating valve, spraying hydrogen peroxide into an activated carbon regeneration tower through a nozzle, and removing sulfur adsorbed in activated carbon by oxidizing elemental sulfur with hydrogen peroxide;
4) After the emission time is over, closing the microwave generator and the spraying device, opening a drainage pipeline, and discharging the generated solution;
5) Opening a potassium dichromate storage tank, introducing a potassium dichromate solution into the activated carbon regeneration tower through a nozzle, removing elemental sulfur remained on the activated carbon, enabling the activated carbon to adsorb chromium elements, and enabling the chromium elements remained on the activated carbon to participate in a desulfurization process after the activated carbon is regenerated, so as to play a role in catalysis; then a drainage pipeline is opened to drain the generated solution;
6) After the solution is discharged, closing the drainage pipeline, opening the purging pipeline and the tail gas discharge pipeline, blowing inert gas into the activated carbon regeneration tower through the purging pipeline, purging, discharging residual gas in the activated carbon regeneration tower from the tail gas discharge pipeline, and completing the regeneration of the activated carbon.
2. The desulfurization activated carbon regeneration method using microwave-coupled hydrogen peroxide according to claim 1, wherein the method comprises the following steps: the concentration of the hydrogen peroxide solution in the hydrogen peroxide storage tank is 1-30%.
3. The desulfurization activated carbon regeneration method using microwave-coupled hydrogen peroxide according to claim 1, wherein the method comprises the following steps: the ratio of the emission time of the microwave generator to the mass of the active carbon is (0.5:1) - (2:1), and the temperature of the active carbon is controlled to be 80-600 ℃; wherein, the emission time unit is minutes, and the mass unit of the activated carbon is grams.
4. The desulfurization activated carbon regeneration method using microwave-coupled hydrogen peroxide according to claim 1, wherein the method comprises the following steps: the inert gas is argon.
5. The desulfurization activated carbon regeneration method using microwave-coupled hydrogen peroxide according to claim 1, wherein the method comprises the following steps: controlling the flow of the inert gas to be 1-5L/min, wherein the ratio of the purging time to the mass of the activated carbon is (1:1) - (5:1); wherein the purging time unit is minutes, and the mass unit of the activated carbon is grams.
6. The desulfurization activated carbon regeneration method using microwave-coupled hydrogen peroxide according to claim 1, wherein the method comprises the following steps: the activated carbon is one or more of coal activated carbon and biomass activated carbon.
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| CN101643205A (en) * | 2008-08-06 | 2010-02-10 | 王庆凯 | Equipment and method for active carbon microwave activation |
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| CN101643205A (en) * | 2008-08-06 | 2010-02-10 | 王庆凯 | Equipment and method for active carbon microwave activation |
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