Method for preparing mercury catalyst by efficiently regenerating waste mercury-containing catalyst

Abstract

The invention relates to a method for preparing a mercury catalyst by efficiently regenerating a waste mercury-containing catalyst, and belongs to the technical field of solid waste recycling. The method comprises seven procedures of directional reconstruction, inert volatilization, negative-pressure circulating absorption, crushing and bonding, inert hot pressing, microwave activation and ultrasonic impregnation, the directional reconstruction is to add an oxidizing agent to convert a complex mercury phase of the waste mercury-containing catalyst into HgCl2, carrier carbon and HgCl2 are efficiently separated under low carbon loss by inert volatilization, HgCl2 flue gas can be completely absorbed by negative-pressure circulating absorption, and the HgCl2 flue gas can be completely absorbed by microwave activation. The step of crushing and bonding comprises the substeps of crushing the mercury-removed activated carbon and then adding a binder for bonding and forming, the step of inert hot pressing comprises the substeps of increasing the strength of the formed carbon, the step of microwave activation comprises the substeps of opening the pore diameter of the carbon, and the step of ultrasonic impregnation comprises the substeps of adding ultrasound in the process of adsorbing the HgCl2 by the activated carbon and strengthening the impregnation of the HgCl2. According to the method, mercury in the waste mercury-containing catalyst can be completely recovered in the form of HgCl2, the recovery rate is 99.8%, the recovery rate of carrier carbon is 99.8%, and the regeneration rate of the mercury catalyst reaches 99.8%.

Description

Technical Field

[0001] The invention relates to a method for efficiently regenerating a discarded mercury-containing catalyst to prepare a mercury catalyst, belonging to the technical field of solid waste recycling. Background Art

[0002] At present, the main method for separating mercury from waste mercury-containing catalysts in China is oxidation distillation, but the distillation temperature is high and the carbon oxidation loss rate is large; the carrier regeneration mostly adopts hydrothermal activation, but the regenerated carbon has a small pore size and a low regeneration rate. Enterprises use high-temperature sublimation technology to separate waste mercury-containing catalyst mercury, and obtain a complex product containing 90% mercuric chloride and 10% elemental mercury, and the distillation temperature needs to reach 450°C; or, by adding calcium oxide, multi-component and multi-phase mercury is pretreated into mercuric oxide, and oxidized and distilled to obtain elemental mercury, but the distillation temperature is as high as 600°C, and the calcium content in the waste activated carbon is 10%, which cannot be recycled; or, the waste activated carbon is regenerated by hydrothermal activation, but the regenerated carbon has a pore size of less than 1.99nm, a process wear loss rate of 10%, and a regeneration rate of less than 20%. Research on the low-temperature separation and regulation of multi-component and multi-phase mercury to prepare mercuric chloride, microwave activation and curing of waste activated carbon is the key to achieving efficient regeneration of waste mercury-containing catalysts.

[0003] Patent CN202211062705.7 discloses a method for recycling waste mercury catalysts, which first uses hydrochloric acid and dodecylphenol polyoxyethylene ether to remove impurity deposits on the surface and in the pores of the waste mercury catalyst, then adds calcium oxide to convert all mercury into mercuric oxide, oxidizes and distills at 700-800°C, and condenses to obtain elemental mercury. Patent CN201810958676.X discloses a method for cleanly and efficiently recycling waste low-mercury catalysts, which adds an organic solvent to the waste mercury catalyst to extract the adsorbed toxic and harmful substances, then places it in a microwave oven, and dry distills and removes mercury at a temperature of 150-800°C and a nitrogen atmosphere. The dry distillation tail gas is condensed to recover mercuric chloride, the residual tail gas after condensation is absorbed, and the carrier carbon is leached to obtain activated carbon and metal chloride salt solution. Patent CN201810442830.8 discloses a high-efficiency recycling process and device for waste mercury catalysts, which places the waste mercury catalysts in a recovery furnace so that the mercuric chloride in the waste mercury catalysts leaves the activated carbon in the form of gas, and uses water not higher than 70°C to dissolve and recover the mercuric chloride liquid. Therefore, none of the existing reports have conducted a directional transformation of the complex mercury phase in the waste mercury-containing catalysts, and no method for activating the carrier carbon is given. Summary of the invention

[0004] In the existing technology of waste mercury-containing catalyst treatment, mercury cannot be completely converted to HgCl 2The invention solves the problems of the inability to recycle the carrier carbon and the inability to regenerate the waste mercury-containing catalyst. The invention provides a method for efficiently regenerating the waste mercury-containing catalyst to prepare a mercury catalyst, including 7 steps of directional reconstruction, inert volatilization, negative pressure circulation absorption, crushing and bonding, inert hot pressing, microwave activation and ultrasonic impregnation. The directional reconstruction is to add an oxidant to convert the complex mercury phase of the waste mercury-containing catalyst into HgCl 2 , inert volatilization to combine the carrier carbon with HgCl at low carbon loss 2 Highly efficient separation and negative pressure circulation absorption can completely absorb HgCl 2 Flue gas, crushing and bonding is to crush the activated carbon after mercury removal and then add a binder to bond and form it, inert hot pressing is to increase the strength of the formed carbon, microwave activation can open the carbon pore size, ultrasonic impregnation is to adsorb HgCl on the activated carbon 2 Ultrasound was added to enhance the HgCl 2 The present invention can realize the complete conversion of mercury in the waste mercury-containing catalyst into HgCl 2 Recycling, the recycling temperature is reduced, the mercury recovery rate exceeds 99%, the carrier carbon recovery rate is 99%, and the mercury catalyst regeneration rate exceeds 99%.

[0005] A method for efficiently regenerating a waste mercury-containing catalyst to prepare a mercury catalyst, the specific steps are as follows:

[0006] (1) Directed reconstruction: Add the waste mercury-containing catalyst and oxidant into a closed light-proof system and mix them evenly to reconstruct the complex mercury phase in the waste mercury-containing catalyst into HgCl 2 A directed reconstructed hybrid system is obtained;

[0007] (2) Inert volatilization: Directed reconstructed mixed system is placed in a protective gas atmosphere and heated to make the carrier carbon and HgCl in the system 2 Efficient separation, the carrier carbon is cooled to room temperature;

[0008] (3) Negative pressure circulation absorption: Turn on the negative pressure circulation and use the hydrochloric acid system to absorb HgCl 2 When the mercuric chloride content in the system is 10-40 g / L, add solid HgCl 2 Prepare HgCl with a concentration of 40 to 80 g / L 2 Solution;

[0009] (4) Crushing and bonding: The carrier carbon is crushed and ball-milled to a particle size of 200-50 mesh, a binder is added and mixed evenly to obtain a mixture, and the mixture is extruded to obtain molded carbon;

[0010] (5) Inert hot pressing: The formed carbon is placed in a protective gas atmosphere and hot pressed to obtain hot pressed carbon;

[0011] (6) Microwave activation: The hot pressed carbon is placed in a microwave and a water vapor-protective gas mixture is introduced for microwave activation to obtain activated carbon;

[0012] (7) Ultrasonic impregnation: Add activated carbon to the HgCl in step (3) 2 The solution is ultrasonically impregnated and dried to obtain a regenerated mercury catalyst.

[0013] Preferably, the waste mercury-containing catalyst in step (1) has a C content of 68.65-91.03%, a Hg content of 0.95-3.31%, a Cl content of 2.12-7.90%, a S content of 0.08-4.45%, and a total content of other elements of 3.46-18.05%; the mercury phase in the waste mercury-containing catalyst includes 56.35-93.76% HgCl 2 4.19~18.89%Hg 2 Cl 2 , 1.65~16.62%Hg, 0.40~8.14%HgS.

[0014] Preferably, the oxidant in step (1) is sodium hypochlorite solution, sodium chlorite solution, sodium chlorate solution or sodium perchlorate solution, the concentration of the oxidant is 4.19-26.53 g / L, the liquid-solid ratio of the oxidant to the waste mercury-containing catalyst is 1:10-5:3, the mixing temperature is 40-80° C., and the mixing time is 1-5 h.

[0015] Preferably, the protective gas in step (2) is CO 2 、N 2 Or Ar, protective gas flow rate is 3~6m 3 / h, the heating temperature is 250-400℃, and the time is 2-5h.

[0016] Preferably, the negative pressure in step (3) is -1000 to -200 Pa, the HCl content in the hydrochloric acid system is 1 to 5 g / L, and the absorption temperature is 50 to 80°C.

[0017] Preferably, the binder in step (4) is a starch / soda ash / bentonite mixture, an asphalt / soda ash / kaolinite mixture or a polyacrylamide / quicklime / bentonite mixture, and the amount of the binder added is 1-5% of the mass of the carrier carbon. The diameter of the formed carbon is 2-3.5 um and the length is 1.2-2 cm.

[0018] More preferably, the mass ratio of starch, soda ash and bentonite in the starch / soda ash / bentonite mixture is 4-6:1-3:6, the mass ratio of asphalt, soda ash and kaolinite in the asphalt / soda ash / kaolinite mixture is 2.5-4.5:1-2.5:4, and the mass ratio of polyacrylamide, quicklime and bentonite in the polyacrylamide / quicklime / bentonite mixture is 3-5:1-2:3.

[0019] Preferably, the protective gas in step (5) is CO 2 、N 2 Or Ar, the hot pressing temperature is 110-150°C, the pressure is 0.6-1.2Mpa, the time is 2-4h, the hot pressed carbon diameter is 1.8-2.5um, and the length is 1-1.5cm.

[0020] Preferably, the protective gas in step (6) is CO 2 、N 2 or Ar, the volume ratio of water vapor to protective gas in the water vapor-protective gas mixture is 1:4~4:1, and the flow rate of the water vapor-protective gas mixture is 1~5m 3 / h.

[0021] More preferably, the microwave power in step (6) is 40 to 80 kW / m 3 The microwave activation temperature is 650-1050°C and the time is 1-5h.

[0022] Preferably, in step (7), HgCl 2 The liquid-to-solid ratio of solution to activated carbon is 1:4-3:2, the ultrasonic frequency is 15-28kHz, and the ultrasonic intensity is 0.28-0.5W / cm 2 The immersion temperature is 60-80℃ and the time is 6-24h.

[0023] In the present invention, the mercury in the discarded mercury-containing catalyst is completely converted to HgCl 2 The recovery rate is 99.1-99.8%, the recovery rate of carrier carbon is 99.1-99.8%, and the regeneration rate of mercury catalyst reaches 99.1-99.8%.

[0024] The beneficial effects of the present invention are:

[0025] (1) The present invention uses phase pre-control to separate the complex high-boiling point phases HgS (volatile temperature 583.5°C) and Hg 2 Cl 2 (volatile temperature 384℃), Hg (volatile temperature 356.7℃) mineral phase transforms into low boiling point phase HgCl 2 (volatilization temperature 302°C), thereby effectively reducing the separation temperature of mercury and carrier carbon to below 310°C, and can be completely returned to the mercury catalyst preparation without further treatment, avoiding the subsequent separation process of recovering mercury; and a circulating negative pressure system is used to avoid the generation of mercuric chloride tail gas, and the mercury recovery rate reaches more than 99%;

[0026] (2) The present invention grinds and solidifies the carrier carbon and then forms it using hot pressing technology. The obtained carrier carbon has higher strength than the original carrier carbon, and is activated by microwaves. Microwaves can induce rapid reaction between water vapor and carbon deposits, and the pore size of the activated carbon is significantly increased, which is conducive to the adsorption of mercuric chloride. The activation rate of waste activated carbon is ≥99%;

[0027] (3) The present invention utilizes the characteristics of ultrasound-enhanced particle vibration to impregnate HgCl in activated carbon. 2 Indirect ultrasound is added during the process to effectively break the balance of the liquid film layer on the surface of the activated carbon particles and strengthen the HgCl 2 The ultrasonic probe can be prevented from directly contacting the activated carbon and impacting the activated carbon surface, causing damage. The immersion time is relatively shortened to 2 hours, and the catalyst regeneration rate exceeds 99%. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is a process flow chart of the present invention. DETAILED DESCRIPTION

[0029] The present invention is further described in detail below in conjunction with specific implementation modes, but the protection scope of the present invention is not limited to the described contents.

[0030] Example 1: The main chemical components and mercury phase distribution of the discarded mercury-containing catalyst in this example are shown in Tables 1.1 and 1.2;

[0031] Table 1.1 Main chemical components of waste mercury-containing catalysts

[0032]

[0033] Table 1.2 Distribution of mercury mass in mercury phases as a percentage of total mercury

[0034]

[0035] A method for efficiently regenerating a waste mercury-containing catalyst to prepare a mercury catalyst (see Figure 1 ), the specific steps are as follows:

[0036] (1) Directed reconstruction: Add the waste mercury-containing catalyst and oxidant (sodium hypochlorite solution) into a closed light-proof system and mix them evenly at 40°C for 1 hour to reconstruct the complex mercury phase in the waste mercury-containing catalyst into HgCl 2 A directional reconstructed mixed system is obtained; the concentration of the oxidant is 26.53 g / L, and the liquid-solid ratio of the oxidant to the waste mercury-containing catalyst is 1:10; the airtight and light-proof system can prevent HgCl 2 Hydrolyzed to Hg 2 Cl 2 ;

[0037] (2) Inert volatilization: Directed reconstruction of the mixed system is placed in a protective gas (CO2 ) atmosphere, heated at 250 ° C for 2 h to make the carrier carbon and HgCl 2 High-efficiency separation achieves inert volatilization, and mercury in the carrier carbon is completely removed. The carrier carbon is cooled to room temperature; the protective gas (CO 2 )Flow rate is 3m 3 / h;

[0038] (3) Negative pressure circulation absorption: Turn on the negative pressure circulation (negative pressure is -1000Pa) and use the hydrochloric acid system with a temperature of 50℃ (HCl content is 1g / L) to absorb HgCl 2 When the mercuric chloride content in the system reaches 10 g / L, solid HgCl 2 Prepare HgCl with a concentration of 40 g / L 2 Solution; the circulating negative pressure system is composed of a buffer tank and a liquid ring vacuum pump;

[0039] (4) Crushing and bonding: The carrier carbon was crushed and ball-milled to a particle size of 200 mesh, and a binder (starch / soda ash / bentonite mixture) of 1% by mass of the carrier carbon was added and mixed evenly for 20 minutes to obtain a mixture, and the mixture was extruded to obtain a molded carbon (diameter 2 μm, length 1.2 cm); the mass ratio of starch, soda ash, and bentonite in the binder (starch / soda ash / bentonite mixture) was 4:1:6;

[0040] (5) Inert hot pressing: The formed carbon is placed in a protective gas (CO 2 ) atmosphere, hot pressed at a temperature of 110°C and a pressure of 0.6 MPa for 2 h to obtain hot pressed carbon (diameter of 1.8 um and length of 1 cm);

[0041] (6) Microwave activation: The hot pressed carbon is placed in a microwave (power 40 kW / m 3 ), the inflow rate is 1m 3 / h water vapor-protective gas (CO 2 ) mixed gas, and microwave activation was performed at a temperature of 650°C for 1 hour to obtain activated carbon; the volume ratio of water vapor to protective gas in the water vapor-protective gas mixed gas was 1:4;

[0042] (7) Ultrasonic impregnation: Add activated carbon to the HgCl in step (3) 2 The solution was ultrasonically immersed at 60°C for 6 hours and hot air dried at 50°C for 3 hours to obtain a regenerated mercury catalyst; the ultrasonic frequency was 15kHz and the intensity was 0.28W / cm 2 ; HgCl 2 The liquid-to-solid ratio of solution to activated carbon mL:g is 1:4;

[0043] In this example, the mercury in the discarded mercury-containing catalyst is completely converted into HgCl 2The recovery rate is 99.1%, the recovery rate of carrier carbon is 99.1%, and the regeneration rate of mercury catalyst reaches 99.1%.

[0044] Example 2: The main chemical components and mercury phase distribution of the discarded mercury-containing catalyst in this example are shown in Tables 2.1 and 2.2;

[0045] Table 2.1 Main chemical components of waste mercury-containing catalysts

[0046]

[0047] Table 2.2 Distribution of mercury mass in mercury phases as a percentage of total mercury

[0048]

[0049] A method for efficiently regenerating a waste mercury-containing catalyst to prepare a mercury catalyst (see Figure 1 ), the specific steps are as follows:

[0050] (1) Directed reconstruction: Add the waste mercury-containing catalyst and oxidant (sodium chlorate solution) into a closed light-proof system and mix them evenly at 60°C for 3 h to reconstruct the complex mercury phase in the waste mercury-containing catalyst into HgCl 2 A directional reconstructed mixed system is obtained; the concentration of the oxidant is 13.92 g / L, and the liquid-solid ratio of the oxidant to the waste mercury-containing catalyst is 2:5; the airtight and light-proof system can prevent HgCl 2 Hydrolyzed to Hg 2 Cl 2 ;

[0051] (2) Inert evaporation: Directed reconstructed mixed system is placed under protective gas (N 2 ) atmosphere, heated at 310 ° C for 3 h to make the carrier carbon and HgCl 2 High-efficiency separation realizes inert volatilization, and mercury in the carrier carbon is completely removed. The carrier carbon is cooled to room temperature; protective gas (N 2 )Flow rate is 4.2m 3 / h;

[0052] (3) Negative pressure circulation absorption: Turn on the negative pressure circulation (negative pressure is -600Pa) and use the hydrochloric acid system with a temperature of 65℃ (HCl content is 3g / L) to absorb HgCl 2 When the mercuric chloride content in the system reaches 20 g / L, solid HgCl 2 Prepare HgCl with a concentration of 60 g / L 2 Solution; the circulating negative pressure system is composed of a buffer tank and a liquid ring vacuum pump;

[0053] (4) Crushing and bonding: The carrier carbon was crushed and ball-milled to a particle size of 80 mesh, and a binder (asphalt / soda ash / kaolinite mixture) of 3% by mass of the carrier carbon was added and mixed evenly for 40 min to obtain a mixture, and the mixture was extruded to obtain a molded carbon (diameter 2.5 μm, length 1.5 cm); the mass ratio of asphalt, soda ash, and kaolinite in the binder (asphalt / soda ash / kaolinite mixture) was 3.5:1.5:4;

[0054] (5) Inert hot pressing: The formed carbon is placed in a protective gas (N 2 ) atmosphere, hot pressed at a temperature of 130°C and a pressure of 1 MPa for 3 h to obtain hot pressed carbon (diameter of 2.2 um and length of 1.2 cm);

[0055] (6) Microwave activation: The hot pressed carbon is placed in a microwave (power 60 kW / m 3 ), the inflow rate is 3m 3 / h water vapor-protective gas (N 2 ) mixed gas, and microwave activation was performed at a temperature of 850°C for 2h to obtain activated carbon; the volume ratio of water vapor to protective gas in the water vapor-protective gas mixed gas was 2:3;

[0056] (7) Ultrasonic impregnation: Add activated carbon to the HgCl in step (3) 2 The solution was ultrasonically immersed at 70°C for 12 hours and hot air dried at 60°C for 5 hours to obtain a regenerated mercury catalyst; the ultrasonic frequency was 20kHz and the intensity was 0.34W / cm 2 ; HgCl 2 The liquid-to-solid ratio of solution to activated carbon was 1:1 in mL:g;

[0057] In this example, the mercury in the discarded mercury-containing catalyst is completely converted into HgCl 2 The recovery rate is 99.5%, the recovery rate of carrier carbon is 99.5%, and the regeneration rate of mercury catalyst reaches 99.5%.

[0058] Example 3: The main chemical components and mercury phase distribution of the discarded mercury-containing catalyst in this example are shown in Tables 3.1 and 3.2;

[0059] Table 3.1 Main chemical components of waste mercury-containing catalysts

[0060]

[0061] Table 3.2 Distribution of mercury mass in mercury phases as a percentage of total mercury

[0062]

[0063] A method for efficiently regenerating a waste mercury-containing catalyst to prepare a mercury catalyst (see Figure 1 ), the specific steps are as follows:

[0064] (1) Directed reconstruction: Add the waste mercury-containing catalyst and oxidant (sodium perchlorate solution) into a closed light-proof system and mix them evenly at 80°C for 5 h to reconstruct the complex mercury phase in the waste mercury-containing catalyst into HgCl 2 A directional reconstructed mixed system is obtained; the oxidant concentration is 4.19 g / L, and the liquid-solid ratio of the oxidant to the waste mercury-containing catalyst is 5:3 in mL:g; the airtight and light-proof system can prevent HgCl 2 Hydrolyzed to Hg 2 Cl 2 ;

[0065] (2) Inert volatilization: The directional reconstructed mixed system was placed in a protective gas (Ar) atmosphere and heated at 400 °C for 5 h to evaporate the carrier carbon and HgCl in the system. 2 High-efficiency separation achieves inert volatilization, and mercury in the carrier carbon is completely removed. The carrier carbon is cooled to room temperature; the protective gas (Ar) flow rate is 6m 3 / h;

[0066] (3) Negative pressure circulation absorption: Turn on the negative pressure circulation (negative pressure is -200Pa) and use the hydrochloric acid system with a temperature of 80℃ (HCl content is 5g / L) to absorb HgCl 2 When the mercuric chloride content in the system reaches 40g / L, solid HgCl 2 Prepare HgCl with a concentration of 80 g / L 2 Solution; the circulating negative pressure system is composed of a buffer tank and a liquid ring vacuum pump;

[0067] (4) Crushing and bonding: The carrier carbon was crushed and ball-milled to a particle size of 50 mesh, and a binder (polyacrylamide / quicklime / bentonite mixture) of 5% by mass of the carrier carbon was added and mixed evenly for 60 minutes to obtain a mixture, and the mixture was extruded to obtain a molded carbon (diameter 3.3 μm, length 2 cm); the mass ratio of the polyacrylamide, quicklime, and bentonite mixture in the binder (polyacrylamide / quicklime / bentonite mixture) was 5:2:3;

[0068] (5) Inert hot pressing: The molded carbon was placed in a protective gas (Ar) atmosphere and hot pressed at a temperature of 150 °C and a pressure of 1.2 MPa for 4 h to obtain hot pressed carbon (diameter 2.5 μm, length 1.5 cm);

[0069] (6) Microwave activation: The hot pressed carbon is placed in a microwave (power 80 kW / m 3 ), the inflow rate is 5m 3 / h of water vapor-protective gas (Ar) mixture, and microwave activation at a temperature of 1050°C for 5h to obtain activated carbon; the volume ratio of water vapor to protective gas in the water vapor-protective gas mixture is 4:1;

[0070] (7) Ultrasonic impregnation: Add activated carbon to the HgCl in step (3) 2 The solution was ultrasonically immersed at 80°C for 24 hours and hot air dried at 70°C for 8 hours to obtain a regenerated mercury catalyst; the ultrasonic frequency was 28 kHz and the intensity was 0.5 W / cm 2 ; HgCl 2 The liquid-to-solid ratio of solution to activated carbon was 3:2 in mL:g;

[0071] In this example, the mercury in the discarded mercury-containing catalyst is completely converted into HgCl 2 The recovery rate is 99.8%, the recovery rate of carrier carbon is 99.8%, and the regeneration rate of mercury catalyst reaches 99.8%.

[0072] The specific implementation modes of the present invention are described in detail above, but the present invention is not limited to the above implementation modes, and various changes can be made within the knowledge scope of ordinary technicians in this field without departing from the purpose of the present invention.

Claims

1. A method for efficiently regenerating a waste mercury-containing catalyst to prepare a mercury catalyst, characterized in that: The specific steps are as follows: (1) Directed reconstruction: Add the waste mercury-containing catalyst and the oxidant into a closed light-proof system and mix them evenly to directionally reconstruct the complex mercury phase in the waste mercury-containing catalyst into HgCl2 to obtain a directed reconstructed mixed system; (2) Inert volatilization: The directional reconstructed mixed system is placed in a protective gas atmosphere and heated to efficiently separate the carrier carbon and HgCl2 in the system, and the carrier carbon is cooled to room temperature; (3) Negative pressure circulation absorption: Turn on the negative pressure circulation, use the hydrochloric acid system to absorb HgCl2 until the mercuric chloride content in the system is 10-40 g / L, and then add solid HgCl2 to prepare a HgCl2 solution with a concentration of 40-80 g / L; (4) Crushing and bonding: The carrier carbon is crushed and ball-milled to a particle size of 200-50 mesh, a binder is added and mixed evenly to obtain a mixture, and the mixture is extruded to obtain molded carbon; (5) Inert hot pressing: The formed carbon is placed in a protective gas atmosphere and hot pressed to obtain hot pressed carbon; (6) Microwave activation: The hot pressed carbon is placed in a microwave and a water vapor-protective gas mixture is introduced for microwave activation to obtain activated carbon; (7) Ultrasonic impregnation: The activated carbon is added to the HgCl2 solution of step (3) for ultrasonic impregnation, and then dried to obtain a regenerated mercury catalyst.

2. The method for efficiently regenerating a waste mercury-containing catalyst to prepare a mercury catalyst according to claim 1, characterized in that: The waste mercury-containing catalyst in step (1) has a C content of 68.65-91.03%, a Hg content of 0.95-3.31%, a Cl content of 2.12-7.90%, a S content of 0.08-4.45%, and a total content of other elements of 3.46-18.05%; the mercury phase in the waste mercury-containing catalyst comprises 56.35-93.76% HgCl2, 4.19-18.89% Hg2Cl2, 1.65-16.62% Hg, and 0.40-8.14% HgS.

3. The method for efficiently regenerating a waste mercury-containing catalyst to prepare a mercury catalyst according to claim 1, characterized in that: The oxidant in step (1) is sodium hypochlorite solution, sodium chlorite solution, sodium chlorate solution or sodium perchlorate solution, the concentration of the oxidant is 4.19-26.53 g / L, the liquid-solid ratio of the oxidant to the waste mercury-containing catalyst is 1:10-5:3, the mixing temperature is 40-80° C., and the mixing time is 1-5 h.

4. The method for efficiently regenerating a waste mercury-containing catalyst to prepare a mercury catalyst according to claim 1, characterized in that: Step (2) The protective gas is CO2, N2 or Ar, and the protective gas flow rate is 3-6m 3 / h, the heating temperature is 250-400℃, and the time is 2-5h.

5. The method for efficiently regenerating a waste mercury-containing catalyst to prepare a mercury catalyst according to claim 1, characterized in that: The negative pressure in step (3) is -1000 to -200 Pa, the HCl content in the hydrochloric acid system is 1 to 5 g / L, and the absorption temperature is 50 to 80°C.

6. The method for efficiently regenerating a waste mercury-containing catalyst to prepare a mercury catalyst according to claim 1, characterized in that: The binder in step (4) is a starch / soda ash / bentonite mixture, an asphalt / soda ash / kaolinite mixture or a polyacrylamide / quicklime / bentonite mixture, and the amount of the binder added is 1-5% of the mass of the carrier carbon. The diameter of the formed carbon is 2-3.5um and the length is 1.2-2cm.

7. The method for efficiently regenerating a waste mercury-containing catalyst to prepare a mercury catalyst according to claim 1, characterized in that: In step (5), the protective gas is CO2, N2 or Ar, the hot pressing temperature is 110-150°C, the pressure is 0.6-1.2 MPa, the time is 2-4 hours, the hot pressed carbon diameter is 1.8-2.5 um, and the length is 1-1.5 cm.

8. The method for efficiently regenerating a waste mercury-containing catalyst to prepare a mercury catalyst according to claim 1, characterized in that: Step (6) The protective gas is CO2, N2 or Ar, the volume ratio of water vapor to protective gas in the water vapor-protective gas mixture is 1:4 to 4:1, and the flow rate of the water vapor-protective gas mixture is 1 to 5 m 3 / h.

9. The method for efficiently regenerating a waste mercury-containing catalyst to prepare a mercury catalyst according to claim 8, characterized in that: The microwave power in step (6) is 40-80 kW / m 3 The microwave activation temperature is 650-1050°C and the time is 1-5h.

10. The method for efficiently regenerating a waste mercury-containing catalyst to prepare a mercury catalyst according to claim 1, characterized in that: Step (7) The liquid-to-solid ratio of HgCl2 solution to activated carbon is 1:4 to 3:2, the ultrasonic frequency is 15 to 28 kHz, and the ultrasonic intensity is 0.28 to 0.5 W / cm 2 The immersion temperature is 60-80℃ and the time is 6-24h.

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