CN109261120B - Method for preparing iron-loaded activated carbon by using waste mercury catalyst - Google Patents

Method for preparing iron-loaded activated carbon by using waste mercury catalyst Download PDF

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CN109261120B
CN109261120B CN201811019195.9A CN201811019195A CN109261120B CN 109261120 B CN109261120 B CN 109261120B CN 201811019195 A CN201811019195 A CN 201811019195A CN 109261120 B CN109261120 B CN 109261120B
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mixture
steam
activated carbon
mercury catalyst
mercury
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CN109261120A (en
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张利波
杨坤
李世伟
彭金辉
朱霏
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Kunming University of Science and Technology
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • 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
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/745—Iron
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B43/00—Obtaining mercury

Abstract

The invention relates to a method for preparing iron-loaded activated carbon by using a waste mercury catalyst, belonging to the technical field of waste resource utilization. Uniformly mixing a waste mercury catalyst, ammonium chloride and ferric chloride to obtain a mixture A, adding an oxidant impregnating solution into the mixture A, carrying out impregnating treatment at the temperature of 20-70 ℃ and reacting for 15-120 min, and reacting for 10-120 min under the conditions of ultrasonic waves and ozone atmosphere to obtain a mixture B; performing microwave drying on the mixture B at the microwave power of 500-900W until no gas exists to obtain a mixture C and steam A, and condensing the steam A and collecting mercury; roasting the mixture C at the low temperature of 200-400 ℃ for 10-90 min to obtain steam B and calcine, and performing dust removal, purification, condensation and refining on the steam B to obtain high-purity mercury; soaking and washing the roasted product by dilute hydrochloric acid, and drying to obtain the iron-loaded activated carbon. The invention adopts ultrasonic wave and ozone to perform solid waste treatment in a synergistic and reinforced way, changes the solid waste into a functional material by a one-step method, and has the advantages of short flow, high regeneration efficiency and good economic benefit.

Description

Method for preparing iron-loaded activated carbon by using waste mercury catalyst
Technical Field
The invention relates to a method for preparing iron-loaded activated carbon by using a waste mercury catalyst, belonging to the technical field of resource utilization and environment.
Background
With the increasing expansion and development of VCM synthesized by the acetylene method in China, the demand of mercury chloride is increasing, the amount of the generated waste mercury catalyst is correspondingly increased, and the amount of the currently generated waste mercury catalyst is about 1.3 ten thousand t/a. The environmental protection system of China is increasingly strict, and people are increasingly more conscious of environmental protection. How to effectively control and reduce the pollution of the waste mercury catalyst to the environment, and establish a mercury recycling economic system, which can ensure the sufficient supply and the stable price of the mercury catalyst, is also of great concern.
At present, two methods are mainly used for recycling the waste mercury catalyst: the regenerated mercury is recovered by using the waste catalyst and pyrometallurgy, and the regenerated mercury catalyst is produced by chemical activation and recovery. However, both recovery methods have certain limitations, and pyrometallurgical smelting can generate a large amount of waste gas in the combustion process, and has high energy consumption, high pollution, low recovery rate and difficult purification and separation. Chemical activation method the treatment time is slightly longer, and agglomeration and mercury soot are easily generated.
Disclosure of Invention
Aiming at the problems and the defects existing in the prior art of waste mercury catalyst recovery, the invention provides the method for preparing the iron-loaded activated carbon by using the waste mercury catalyst, and the method has the advantages of high treatment efficiency, environmental friendliness and capability of directly and efficiently recycling the waste mercury catalyst.
A method for preparing iron-loaded activated carbon by using a waste mercury catalyst comprises the following specific steps:
(1) uniformly mixing the waste mercury catalyst, ammonium chloride and ferric chloride to obtain a mixture A, adding an oxidant impregnating solution into the mixture A, carrying out impregnating treatment at the temperature of 20-70 ℃ and reacting for 15-120 min, and then reacting for 10-120 min under the conditions of ultrasonic waves and ozone atmosphere to obtain a mixture B; wherein the content of the mercuric chloride in the waste mercury catalyst is 2-20% by mass percent;
(2) performing microwave drying on the mixture obtained in the step (1) at the microwave power of 500-900W until no gas exists to obtain a mixture C and steam A, and condensing the steam A and collecting mercury;
(3) roasting the mixture C obtained in the step (2) at a low temperature of 200-400 ℃ for 10-90 min to obtain steam B and roasted sand, and performing dust removal, purification, condensation and refining on the steam B to obtain high-purity mercury;
(4) soaking and washing the roasted product in the step (3) by using dilute hydrochloric acid, and drying to obtain iron-loaded activated carbon;
the mass ratio of the waste mercury catalyst, the ammonium chloride and the ferric chloride in the step (1) is 100: 0.1-5: 0.1-1;
in the step (1), the concentration of the oxidant impregnating solution is 5-15%, and the oxidant impregnating solution and the mixture are mixedThe liquid-solid ratio mL of the substance A is 2-15: 1, and the oxidant is H2O2Sodium hypochlorite and/or ammonium persulfate;
in the step (1), the ultrasonic power is 200-2000 w, and the flow of ozone is 0.01-0.5 mL/min;
the concentration of the dilute hydrochloric acid in the step (4) is 2-15%, the drying temperature is 50-110 ℃, and the drying time is 30-120 min.
The invention has the beneficial effects that:
(1) in the use process of the mercury catalyst, the mercury chloride is lost, the mercury chloride reacts with impurity elements to generate mercury subchloride, mercury sulfide or mercury simple substance, especially free carbon and high-boiling organic matters generated by side reactions such as cracking and the like are deposited on the surface of the mercury chloride or block an active carbon channel, so that the mercury chloride catalyst is inactivated and scrapped to form the waste mercury catalyst2And the organic matters are decomposed and removed more completely, the aperture and the specific surface area of the regenerated active carbon are increased, and the surface adsorption activity of the active carbon is improved;
(2) the regenerated activated carbon obtained by the method has large aperture and specific surface area, high surface adsorption activity and high adsorption rate to impurity ions;
(3) the method has the advantages of high recovery rate of the waste mercury catalyst, simple operation and less pollution; the iron-doped active carbon can be directly used for treating As, Pb, Fe and other wastewater.
Detailed Description
The present invention will be further described with reference to the following embodiments.
Example 1: a method for preparing iron-loaded activated carbon by using a waste mercury catalyst comprises the following specific steps:
(1) mixing waste mercury catalyst, ammonium chloride and ferric chloride uniformly to obtain a mixture A, and adding an oxidant impregnating solution (H) into the mixture A2O2Solution), performing infiltration treatment at the temperature of 20 ℃, reacting for 15min, and reacting for 10min under the conditions of ultrasonic waves and ozone atmosphere to obtain a mixture B; wherein at leastThe content of mercuric chloride in the waste mercury catalyst is 2 percent by mass percent; the mass ratio of the waste mercury catalyst, the ammonium chloride and the ferric chloride is 100: 0.1: 0.1; oxidant impregnating solution (H)2O2Solution) is 5 percent, and the liquid-solid ratio mL of the oxidant impregnating solution to the mixture A is 2: 1; the ultrasonic power is 200w, and the flow of ozone is 0.01 mL/min;
(2) performing microwave drying on the mixture obtained in the step (1) at the microwave power of 500W until no gas exists to obtain a mixture C and steam A, and condensing the steam A and collecting mercury;
(3) roasting the mixture C obtained in the step (2) at the low temperature of 200 ℃ for 10min to obtain steam B and roasted sand, and performing dust removal, purification, condensation and refining on the steam B to obtain high-purity mercury;
(4) soaking and washing the roasted product in the step (3) by using dilute hydrochloric acid, and drying to obtain iron-loaded activated carbon; wherein the concentration of the dilute hydrochloric acid is 2%, the drying temperature is 50 ℃, and the drying time is 30 min;
in this example, the recovery rate of mercury is 88.12%, and the iron-doped regenerated catalyst contains 100 mg/L Na2HAsO4The adsorption rate of the wastewater was 86.76%.
Example 2: a method for preparing iron-loaded activated carbon by using a waste mercury catalyst comprises the following specific steps:
(1) mixing waste mercury catalyst, ammonium chloride and ferric chloride uniformly to obtain a mixture A, and adding an oxidant impregnating solution (H) into the mixture A2O2Solution), performing infiltration treatment at the temperature of 50 ℃ and reacting for 60min, and reacting for 60min under the conditions of ultrasonic waves and ozone atmosphere to obtain a mixture B; wherein, the content of mercuric chloride in the waste mercury catalyst is 10 percent by mass percent; the mass ratio of the waste mercury catalyst to the ammonium chloride to the ferric chloride is 100: 2: 0.5; oxidant impregnating solution (H)2O2Solution) is 10 percent, and the liquid-solid ratio mL of the oxidant impregnating solution to the mixture A is 8: 1; the ultrasonic power is 1000w, and the flow of ozone is 0.1 mL/min;
(2) performing microwave drying on the mixture obtained in the step (1) at the microwave power of 700W until no gas exists to obtain a mixture C and steam A, and performing condensation treatment on the steam A and collecting mercury;
(3) roasting the mixture C obtained in the step (2) at the low temperature of 300 ℃ for 50min to obtain steam B and calcine, and performing dust removal, purification, condensation and refining on the steam B to obtain high-purity mercury;
(4) soaking and washing the roasted product in the step (3) by using dilute hydrochloric acid, and drying to obtain iron-loaded activated carbon; wherein the concentration of the dilute hydrochloric acid is 5%, the drying temperature is 80 ℃, and the drying time is 75 min;
in this example, the recovery rate of mercury is 90.08%, and the iron-doped regenerated catalyst contains 100 mg/L Na2HAsO4The adsorption rate of the wastewater was 88.12%.
Example 3: a method for preparing iron-loaded activated carbon by using a waste mercury catalyst comprises the following specific steps:
(1) mixing waste mercury catalyst, ammonium chloride and ferric chloride uniformly to obtain a mixture A, and adding an oxidant impregnating solution (H) into the mixture A2O2Solution), performing infiltration treatment at the temperature of 70 ℃, reacting for 120min, and reacting for 120min under the conditions of ultrasonic waves and ozone atmosphere to obtain a mixture B; wherein, the content of mercuric chloride in the waste mercury catalyst is 20 percent by mass percent; the mass ratio of the waste mercury catalyst to the ammonium chloride to the ferric chloride is 100:5: 1; oxidant impregnating solution (H)2O2Solution) is 15 percent, and the liquid-solid ratio mL of the oxidant impregnating solution to the mixture A is 15: 1; the ultrasonic power is 2000w, and the flow of ozone is 0.5 mL/min;
(2) performing microwave drying on the mixture obtained in the step (1) at the microwave power of 900W until no gas exists to obtain a mixture C and steam A, and condensing the steam A and collecting mercury;
(3) roasting the mixture C obtained in the step (2) at the temperature of 400 ℃ for 90min to obtain steam B and calcine, and performing dust removal, purification, condensation and refining on the steam B to obtain high-purity mercury;
(4) soaking and washing the roasted product in the step (3) by using dilute hydrochloric acid, and drying to obtain iron-loaded activated carbon; wherein the concentration of the dilute hydrochloric acid is 15%, the drying temperature is 110 ℃, and the drying time is 120 min;
in this example, the recovery rate of mercury was 91.29%, and the iron was doped againThe raw catalyst pair contains 100 mg/L Na2HAsO4The adsorption rate of the wastewater was 92.12%.
Example 4: a method for preparing iron-loaded activated carbon by using a waste mercury catalyst comprises the following specific steps:
(1) uniformly mixing the waste mercury catalyst, ammonium chloride and ferric chloride to obtain a mixture A, adding an oxidant impregnating solution (sodium hypochlorite solution) into the mixture A, carrying out impregnating treatment at the temperature of 50 ℃ and reacting for 60min, and reacting for 30min under the conditions of ultrasonic waves and ozone atmosphere to obtain a mixture B; wherein, the content of mercuric chloride in the waste mercury catalyst is 10 percent by mass percent; the mass ratio of the waste mercury catalyst to the ammonium chloride to the ferric chloride is 100: 2: 0.5; the concentration of the oxidant impregnating solution (sodium hypochlorite solution) is 10%, and the liquid-solid ratio mL of the oxidant impregnating solution to the mixture A is 8: 1; the ultrasonic power is 1000w, and the flow of ozone is 0.1 mL/min;
(2) performing microwave drying on the mixture obtained in the step (1) at the microwave power of 700W until no gas exists to obtain a mixture C and steam A, and performing condensation treatment on the steam A and collecting mercury;
(3) roasting the mixture C obtained in the step (2) at the low temperature of 300 ℃ for 50min to obtain steam B and calcine, and performing dust removal, purification, condensation and refining on the steam B to obtain high-purity mercury;
(4) soaking and washing the roasted product in the step (3) by using dilute hydrochloric acid, and drying to obtain iron-loaded activated carbon; wherein the concentration of the dilute hydrochloric acid is 2%, the drying temperature is 80 ℃, and the drying time is 75 min;
in this example, the recovery rate of mercury is 88.29%, and the iron-doped regenerated catalyst contains 100 mg/L Na2HAsO4The adsorption rate of the wastewater was 87.28%.
Example 5: a method for preparing iron-loaded activated carbon by using a waste mercury catalyst comprises the following specific steps:
(1) uniformly mixing the waste mercury catalyst, ammonium chloride and ferric chloride to obtain a mixture A, adding an oxidant impregnating solution (ammonium persulfate solution) into the mixture A, carrying out impregnating treatment at the temperature of 50 ℃ and reacting for 60min, and reacting for 90min under the conditions of ultrasonic waves and ozone atmosphere to obtain a mixture B; wherein, the content of mercuric chloride in the waste mercury catalyst is 10 percent by mass percent; the mass ratio of the waste mercury catalyst to the ammonium chloride to the ferric chloride is 100: 2: 0.5; the concentration of the oxidant impregnating solution (ammonium persulfate solution) is 10%, and the liquid-solid ratio mL of the oxidant impregnating solution to the mixture A is 8: 1; the ultrasonic power is 1000w, and the flow of ozone is 0.1 mL/min;
(2) performing microwave drying on the mixture obtained in the step (1) at the microwave power of 700W until no gas exists to obtain a mixture C and steam A, and performing condensation treatment on the steam A and collecting mercury;
(3) roasting the mixture C obtained in the step (2) at the low temperature of 300 ℃ for 50min to obtain steam B and calcine, and performing dust removal, purification, condensation and refining on the steam B to obtain high-purity mercury;
(4) soaking and washing the roasted product in the step (3) by using dilute hydrochloric acid, and drying to obtain iron-loaded activated carbon; wherein the concentration of the dilute hydrochloric acid is 2%, the drying temperature is 80 ℃, and the drying time is 75 min;
the recovery rate of mercury in this example is 80.09%, and the iron-doped regenerated catalyst contains 100 mg/L Na2HAsO4The adsorption rate of the wastewater was 89.36%.
While the present invention has been described in detail with reference to the specific embodiments thereof, the present invention is not limited to the embodiments described above, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.

Claims (5)

1. A method for preparing iron-loaded activated carbon by using a waste mercury catalyst is characterized by comprising the following specific steps:
(1) uniformly mixing the waste mercury catalyst, ammonium chloride and ferric chloride to obtain a mixture A, adding an oxidant impregnating solution into the mixture A, carrying out impregnating treatment at the temperature of 20-70 ℃ and reacting for 15-120 min, and then reacting for 10-120 min under the conditions of ultrasonic waves and ozone atmosphere to obtain a mixture B; wherein the content of the mercuric chloride in the waste mercury catalyst is 2-20% by mass percent;
(2) performing microwave drying on the mixture obtained in the step (1) at the microwave power of 500-900W until no gas exists to obtain a mixture C and steam A, and condensing the steam A and collecting mercury;
(3) roasting the mixture C obtained in the step (2) at a low temperature of 200-400 ℃ for 10-90 min to obtain steam B and roasted sand, and performing dust removal, purification, condensation and refining on the steam B to obtain high-purity mercury;
(4) and (4) soaking and washing the roasted product in the step (3) by using dilute hydrochloric acid, and drying to obtain the iron-loaded activated carbon.
2. The method for preparing iron-loaded activated carbon using spent mercury catalyst as claimed in claim 1, wherein: the mass ratio of the waste mercury catalyst, the ammonium chloride and the ferric chloride in the step (1) is 100: 0.1-5: 0.1-1.
3. The method for preparing iron-loaded activated carbon using spent mercury catalyst as claimed in claim 1, wherein: in the step (1), the concentration of the oxidant impregnating solution is 5-15%, the liquid-solid ratio mL of the oxidant impregnating solution to the mixture A is 2-15: 1, and the oxidant is H2O2Sodium hypochlorite and/or ammonium persulfate.
4. The method for preparing iron-loaded activated carbon using spent mercury catalyst as claimed in claim 1, wherein: in the step (1), the ultrasonic power is 200-2000 w, and the flow rate of ozone is 0.01-0.5 mL/min.
5. The method for preparing iron-loaded activated carbon using spent mercury catalyst as claimed in claim 1, wherein: the concentration of the dilute hydrochloric acid in the step (4) is 2-15%, the drying temperature is 50-110 ℃, and the drying time is 30-120 min.
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