CN110605106A - Regeneration method of waste mercury catalyst activated carbon after harmless treatment - Google Patents
Regeneration method of waste mercury catalyst activated carbon after harmless treatment Download PDFInfo
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- CN110605106A CN110605106A CN201910857119.3A CN201910857119A CN110605106A CN 110605106 A CN110605106 A CN 110605106A CN 201910857119 A CN201910857119 A CN 201910857119A CN 110605106 A CN110605106 A CN 110605106A
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- activated carbon
- hydrochloric acid
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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
- B01J20/30—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
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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
- B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
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Abstract
The invention discloses a method for regenerating activated carbon of a waste mercury catalyst after innocent treatment, which belongs to the technical field of recycling of the waste mercury catalyst.A hydrochloric acid solution is put into the activated carbon in the waste mercury catalyst after innocent treatment for oscillation, the concentration of the hydrochloric acid solution is 0.2 ~.8 mol/L, the oscillation time is 0.5 ~ h, the activated carbon is put into an oxygen-isolated environment after being filtered and heated to 650 ~ ℃ for 0.5 ~ h, and the regenerated activated carbon is obtained after cooling.
Description
Technical Field
The invention belongs to the technical field of recycling of waste mercury catalysts, and particularly relates to a regeneration method of harmless treated waste mercury catalyst activated carbon.
Background
The mercury catalyst is an indispensable part for producing polyvinyl chloride (PVC) by a calcium carbide method, and is used as a catalyst for synthesizing Vinyl Chloride (VCM) by acetylene and hydrogen chloride gas in PVC production. The mercury catalyst is produced by taking activated carbon as a carrier and mercuric chloride as an active substance, and loading the mercuric chloride on the surface of the activated carbon. After the mercury catalyst is used for a certain period of time, the activity of the mercury catalyst is reduced and the mercury catalyst needs to be replaced, and the replaced waste mercury catalyst still contains about 2-5% of mercuric chloride. The mercuric chloride is extremely toxic, extremely volatile and easily soluble in water, and if the replaced mercury catalyst is directly discarded or stacked, serious mercury pollution is caused, and great potential safety hazards are generated. According to the "treatment and disposal method for waste mercury catalyst" (GB/T36382-2008), distillation and oxygen-controlled dry distillation are mainly adopted for the harmless treatment of the waste mercury catalyst at present. The distillation method is characterized in that quicklime, sodium hydroxide and the like are added to convert mercury in each valence state in the waste mercury catalyst into similar substances (most of which are mercury oxide) which are easy to decompose, volatilize and collect and have similar physical and chemical properties, the mercury oxide is heated and decomposed into elemental mercury and oxygen, and elemental mercury vapor is quenched to realize the recovery of mercury in the waste mercury catalyst.
Although the method realizes harmless treatment of the waste mercury catalyst and recovery of mercury, activation and regeneration of activated carbon are not realized, and substances such as quicklime, sodium hydroxide and the like are introduced in a pretreatment process, so that a large amount of calcium carbonate, calcium oxide, sodium carbonate and other powder are attached to the surface of the waste mercury catalyst after a distillation process, the activated carbon is seriously inactivated, and the activated carbon is difficult to reuse. Although the waste mercury catalyst can be treated as general waste in principle after being subjected to harmless treatment of recovered mercury, people always worry about whether the mercury content of a certain batch of activated carbon exceeds the identification standard of hazardous waste. Moreover, the active carbon cannot be recycled, so that serious resource waste is caused, and the production cost of enterprises is increased.
Disclosure of Invention
In order to realize high-value utilization of the waste activated carbon after harmless treatment of the waste mercury catalyst, the invention aims to provide the method for regenerating the waste mercury catalyst activated carbon, which has low cost, simple flow and good effect. The invention utilizes the method of combining the chemical regeneration and the thermal regeneration of the hydrochloric acid to remove calcium carbonate, sodium carbonate, calcium oxide, residual PVC and other substances existing on the surface and inside of the hydrochloric acid, and recovers the adsorption capacity of the activated carbon, thereby realizing the aim of regeneration.
The purpose of the invention is realized by the following technical scheme: a regeneration method of waste mercury catalyst activated carbon after innocent treatment comprises the following steps:
(1) placing the harmlessly treated waste mercury catalyst activated carbon into a hydrochloric acid solution with the concentration of 0.2 ~ 0.8.8 mol/L, and oscillating by using an oscillator for 0.5 ~ 4 h;
(2) filtering and separating the mixed solution obtained in the step (1) to obtain filtrate and activated carbon, and returning the filtrate to the step (1) for recycling;
(3) putting the filtered activated carbon product into a temperature programmed heating furnace, heating to 650 ~ 850 ℃ under the condition of oxygen isolation, keeping the temperature for activation and regeneration for 0.5 ~ 4 h;
(4) and closing the heating furnace for cooling to obtain the regenerated activated carbon.
In the invention, in the step (1), the mass ratio of the activated carbon to the hydrochloric acid is 1:5 ~ 1: 10.
In the invention, in the step (1), the concentration of the hydrochloric acid is 0.4 ~ 0.8.8 mol/L, and the oscillation time is 0.5 h.
In the invention, in the step (1), the oscillator is a turnover type oscillator with the frequency of 20 ~ 50 rpm.
In the invention, in the step (2), firstly, a polypropylene or polytetrafluoroethylene corrosion-resistant filter plate is adopted to separate the active carbon from the hydrochloric acid solution, then dilute sulfuric acid is added into the waste hydrochloric acid solution to remove calcium chloride generated by the reaction, the calcium chloride is separated again, and finally the filtered hydrochloric acid solution is returned to the step (1) to realize the reuse.
In the invention, in the step (3), the temperature is 700 ~ 750 ℃, the regeneration time is 2 ~ 2.5.5 h, and the heating is carried out in a closed oxygen-insulated environment to avoid the loss of the active carbon.
Compared with the prior art, the invention has the following advantages:
1. the method realizes the regeneration of the waste mercury catalyst activated carbon after harmless treatment by adopting a mode of combining chemical regeneration and thermal regeneration, and has the characteristics of good effect, low cost, simple equipment and the like compared with a single activated carbon regeneration method;
2. in the chemical regeneration process, hydrochloric acid is adopted under the oscillation action of an oscillator, substances such as calcium carbonate, sodium carbonate, calcium oxide and the like remained on the surface of the waste mercury catalyst activated carbon can be quickly removed in a short time, and the adsorption capacity of the activated carbon is improved;
3. the method adopts a thermal regeneration mode to regenerate the harmlessly treated waste mercury catalyst activated carbon, quickly removes residual adsorption substances in the activated carbon, and remarkably recovers the adsorption capacity of the harmlessly treated waste mercury catalyst activated carbon.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples. These examples are given solely for the purpose of illustration and are not intended to limit the scope of the invention.
And (3) process screening test:
1. screening of hydrochloric acid concentration and oscillation time
(1) Averagely dividing the harmless treated waste mercury catalyst activated carbon into 20 parts, placing the 20 parts in hydrochloric acid solutions with different concentrations (0.2 mol/L, 0.4 mol/L, 0.6mol/L and 0.8 mol/L), oscillating for a certain time (0.5 h, 1 h, 1.5 h and 2 h), closing the equipment, filtering and drying to obtain the regenerated activated carbon treated under the conditions of different hydrochloric acid concentrations and oscillation time.
(2) The iodine adsorption value and the methylene blue adsorption value of the regenerated activated carbon obtained under different treatment conditions in the step (1) are detected, and the result shows that the regeneration time is constant, when the hydrochloric acid concentration value is increased from 0.2 mol/L to 0.4 mol/L, the iodine adsorption value and the methylene blue adsorption value are both greatly increased, but are not obviously increased after the hydrochloric acid concentration value exceeds 0.6mol/L, when the hydrochloric acid concentration value is in the range of 0.4 ~ 0.8mol/L, the influence of the oscillation time on the adsorption performance of the regenerated activated carbon is small, and the oscillation time of 0.5 h is enough, so that the hydrochloric acid concentration is preferably 0.4 ~ 0.8.8 mol/L, the oscillation time is 0.5 h, the optimum condition is that the hydrochloric acid concentration value is 0.6mol/L, and the oscillation time is 0.5 h.
2. Screening of thermal regeneration temperature and time
(1) Averagely dividing the activated carbon treated under the conditions that the concentration value of hydrochloric acid is 0.6mol/L and the oscillation time is 0.5 h into 12 parts, putting the activated carbon into a temperature programming furnace, setting the temperature to be 650 ℃, 750 ℃ and 850 ℃, treating the activated carbon in an oxygen-isolated environment, keeping the treatment time to be 0.5 h, 1 h, 1.5 h and 2 h, closing equipment after the treatment is finished, and cooling to obtain the regenerated activated carbon treated under different thermal regeneration temperature and time conditions.
(2) The iodine adsorption value and the methylene blue adsorption value of the regenerated activated carbon obtained under different treatment conditions in the step (1) are detected, and the result shows that the adsorption performance of the regenerated activated carbon is firstly increased and then decreased along with the increase of the temperature when the heat regeneration time is fixed, the effect is optimal when the temperature is 750 ℃, the adsorption performance of the activated carbon is increased along with the increase of the retention time when the heat treatment temperature is fixed, the increase amplitude is lower after the retention time is increased and exceeds 2 hours, and the optimal retention time is 2 hours when the time cost and the energy consumption are considered, so that the heat regeneration temperature is 650 ~ 850 ℃, the regeneration time is 0.5 ~ 4 hours, the heat regeneration temperature is preferably 700 ~ 750 ℃, the regeneration time is 2 ~ 2.5.5 hours, and the optimal heat regeneration temperature is 750 ℃ and the retention time is 2 hours.
Example 1
A regeneration method of waste mercury catalyst activated carbon after harmless treatment comprises the following specific steps:
(1) putting 20 g of harmless treated waste mercury catalyst activated carbon into 0.7 mol/L hydrochloric acid solution, wherein the putting mass ratio of the activated carbon to the hydrochloric acid is 1:5, and taking down the activated carbon after 2 hours of oscillation by using a turnover type oscillator with the oscillation frequency of 30 rpm;
(2) separating the activated carbon and the hydrochloric acid solution in the step (1) by adopting a filter plate made of corrosion-resistant materials such as polypropylene or polytetrafluoroethylene, adding a proper amount of dilute sulfuric acid into the waste hydrochloric acid solution to remove calcium chloride generated by the reaction, separating again, and returning the filtered hydrochloric acid solution to the step (1) for reuse;
(3) putting the filtered activated carbon product into a temperature programmed heating furnace, and heating for 3 h under the conditions of nitrogen atmosphere, gas flow of 0.5L/min and 650 ℃ to ensure a closed oxygen-insulated environment;
(4) and closing the heating furnace for cooling to obtain the regenerated activated carbon.
In the embodiment, the iodine adsorption value and the methylene blue adsorption value are determined according to GB/T7702.7-2008 and GB/T7702.6-2008, the iodine adsorption values before and after regeneration of the activated carbon are respectively 10 mg/g and 943 mg/g, the methylene blue adsorption values are respectively 1.5 mg/g and 152 mg/g, and the regenerated harmless treated waste mercury catalyst activated carbon recovers higher adsorption capacity.
Example 2
(1) Putting 20 g of harmless treated waste mercury catalyst activated carbon into 0.6mol/L hydrochloric acid solution, wherein the adding mass ratio of the activated carbon to the hydrochloric acid is 1:6, and taking down the waste mercury catalyst activated carbon after oscillation for 0.5 h by using a turnover type oscillator with the oscillation frequency of 30 rpm;
(2) separating the activated carbon and the hydrochloric acid solution in the step (1) by adopting a filter plate made of corrosion-resistant materials such as polypropylene or polytetrafluoroethylene, adding a proper amount of dilute sulfuric acid into the waste hydrochloric acid solution to remove calcium chloride generated by the reaction, separating again, and returning the filtered hydrochloric acid solution to the step (1) for reuse;
(3) putting the filtered activated carbon product into a temperature programmed heating furnace, and heating for 2 hours under the conditions of nitrogen atmosphere, gas flow of 0.5L/min and 750 ℃ to ensure a closed oxygen-insulating environment;
(4) and closing the heating furnace for cooling to obtain the regenerated activated carbon.
In this embodiment, iodine adsorption values and methylene blue adsorption values are determined according to GB/T7702.7-2008 and GB/T7702.6-2008, the iodine adsorption values before and after regeneration of the activated carbon are 10 mg/g and 1005 mg/g, respectively, and the methylene blue adsorption values are 1.5 mg/g and 159 mg/g, respectively, and the regenerated harmless treated waste mercury catalytic activated carbon recovers a higher adsorption capacity.
Example 3
(1) Putting 20 g of harmless treated waste mercury catalyst activated carbon into 0.5 mol/L hydrochloric acid solution, wherein the adding mass ratio of the activated carbon to the hydrochloric acid is 1:7, and taking down the waste mercury catalyst activated carbon after oscillation for 0.5 h by using a turnover type oscillator with the oscillation frequency of 30 rpm;
(2) separating the activated carbon and the hydrochloric acid solution in the step (1) by using a filter plate made of corrosion-resistant materials such as polypropylene or polytetrafluoroethylene, adding a proper amount of dilute sulfuric acid into the waste hydrochloric acid solution to remove calcium chloride generated by the reaction, separating again, and returning the filtered hydrochloric acid solution to the step (1) for reuse;
(3) putting the filtered activated carbon product into a temperature programmed heating furnace, and heating for 2 hours at 850 ℃ in a nitrogen atmosphere at the gas flow of 0.5L/min to ensure a closed oxygen-insulated environment;
(4) and closing the heating furnace for cooling to obtain the regenerated activated carbon.
In this example, the iodine adsorption value and the methylene blue adsorption value are determined according to GB/T7702.7-2008 and GB/T7702.6-2008, the iodine adsorption values before and after regeneration of the activated carbon are respectively 10 mg/g and 965 mg/g, the methylene blue adsorption values are respectively 1.5 mg/g and 149 mg/g, and the regenerated harmless treated waste mercury catalyst activated carbon recovers higher adsorption capacity.
Example 4
(1) Putting 50 g of harmless treated waste mercury catalyst activated carbon into 0.8mol/L hydrochloric acid solution, wherein the putting mass ratio of the activated carbon to the hydrochloric acid is 1:10, and taking down the waste mercury catalyst activated carbon by using a turnover type oscillator with the oscillation frequency of 30 rpm and oscillation for 4 hours;
(2) separating the activated carbon and the hydrochloric acid solution in the step (1) by adopting a filter plate made of corrosion-resistant materials such as polypropylene or polytetrafluoroethylene, adding a proper amount of dilute sulfuric acid into the waste hydrochloric acid solution to remove calcium chloride generated by the reaction, separating again, and returning the filtered hydrochloric acid solution to the step (1) for reuse;
(3) putting the filtered activated carbon product into a temperature programmed heating furnace, and heating for 0.5 h at 850 ℃ in a nitrogen atmosphere at the gas flow of 0.5L/min to ensure a closed oxygen-insulated environment;
(4) and closing the heating furnace for cooling to obtain the regenerated activated carbon.
In this embodiment, iodine adsorption values and methylene blue adsorption values are determined according to GB/T7702.7-2008 and GB/T7702.6-2008, the iodine adsorption values before and after regeneration of the activated carbon are 10 mg/g and 987 mg/g, respectively, and the methylene blue adsorption values are 1.5 mg/g and 151 mg/g, respectively, and the regenerated harmless treated waste mercury catalyst activated carbon recovers a higher adsorption capacity.
Example 5
(1) Putting 1 kg of harmless treated waste mercury catalyst activated carbon into 0.4 mol/L hydrochloric acid solution, wherein the adding mass ratio of the activated carbon to the hydrochloric acid is 1:9, and using a turnover type oscillator, wherein the oscillation frequency is 30 rpm, and the activated carbon is taken down after oscillation for 3 hours;
(2) separating the activated carbon and the hydrochloric acid solution in the step (1) by adopting a filter plate made of corrosion-resistant materials such as polypropylene or polytetrafluoroethylene, adding a proper amount of dilute sulfuric acid into the waste hydrochloric acid solution to remove calcium chloride generated by the reaction, separating again, and returning the filtered hydrochloric acid solution to the step (1) for reuse;
(3) putting the filtered activated carbon product into a temperature programmed heating furnace, and heating for 4 hours at 750 ℃ in a nitrogen atmosphere at the gas flow of 5L/min to ensure a closed oxygen-insulating environment;
(4) and closing the heating furnace for cooling to obtain the regenerated activated carbon.
In this embodiment, iodine adsorption values and methylene blue adsorption values are determined according to GB/T7702.7-2008 and GB/T7702.6-2008, the iodine adsorption values before and after regeneration of the activated carbon are 10 mg/g and 998 mg/g, respectively, and the methylene blue adsorption values are 1.5 mg/g and 153 mg/g, respectively, and the regenerated harmless treated waste mercury catalyst activated carbon recovers a higher adsorption capacity.
Claims (6)
1. A regeneration method of waste mercury catalyst activated carbon after innocent treatment is characterized by comprising the following steps:
(1) placing the harmlessly treated waste mercury catalyst activated carbon into a hydrochloric acid solution with the concentration of 0.2 ~ 0.8.8 mol/L, and oscillating by using an oscillator for 0.5 ~ 4 h;
(2) filtering and separating the mixed solution obtained in the step (1) to obtain filtrate and activated carbon, and returning the filtrate to the step (1) for recycling;
(3) putting the filtered activated carbon product into a temperature programmed heating furnace, heating to 650 ~ 850 ℃ under the condition of oxygen isolation, keeping the temperature for activation and regeneration for 0.5 ~ 4 h;
(4) and closing the heating furnace for cooling to obtain the regenerated activated carbon.
2. The method for regenerating the harmlessly treated waste mercury-catalyzed activated carbon as claimed in claim 1, wherein in the step (1), the mass ratio of activated carbon to hydrochloric acid is 1:5 ~ 1: 10.
3. The method for regenerating the harmlessly treated waste mercury-catalyzed activated carbon as claimed in claim 1, wherein the hydrochloric acid concentration in the step (1) is 0.4 ~ 0.8.8 mol/L, and the oscillation time is 0.5 h.
4. The method for regenerating the harmlessly treated waste mercury-catalyzed activated carbon as claimed in claim 1, wherein in the step (1), the oscillator is a roll-over oscillator with a frequency of 20 ~ 50 rpm.
5. The regeneration method of the harmlessly treated waste mercury-catalyzed activated carbon according to claim 1, wherein in the step (2), the activated carbon is separated from the hydrochloric acid solution by using a polypropylene or polytetrafluoroethylene corrosion-resistant filter plate, then dilute sulfuric acid is added into the waste hydrochloric acid solution to remove calcium chloride generated by the reaction, the calcium chloride is separated again, and finally the filtered hydrochloric acid solution is returned to the step (1) for reuse.
6. The method for regenerating the harmlessly treated waste mercury-catalyzed activated carbon as claimed in claim 1, wherein the temperature in the step (3) is 700 ~ 750 ℃, and the regeneration time is 2 ~ 2.5.5 h.
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Cited By (2)
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| CN111321428A (en) * | 2020-03-04 | 2020-06-23 | 中南大学 | Method for waste mercuric chloride catalyst molten salt electrolysis regeneration and mercury recovery |
| CN114229843A (en) * | 2021-12-24 | 2022-03-25 | 贵州重力科技环保有限公司 | Method for activating and regenerating waste activated carbon after harmless treatment of waste mercury catalyst |
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