阅读说明：本技术 一种氯乙烯合成用超低汞催化剂制备方法 (Preparation method of ultralow-mercury catalyst for vinyl chloride synthesis ) 是由 吴云和 于 2019-12-02 设计创作，主要内容包括：本申请公开的氯乙烯合成用超低汞催化剂制备方法,与现有技术相比,包括以下步骤：获取原料煤；脱灰处理原料煤；碳化处理；活化处理；处理活性炭获得载体；配置盐酸溶液；吸附剂制备；吸附处理：将吸附剂粉体置于浓度为70％的乙醇溶液中1000rpm搅拌30min得到吸附液；再将活性炭置于吸附床内,先用氮气吹扫系统,排出氧气、二氧化碳等杂质气体；开启循环系统,同时,开启超声波辅助系统,同时通入压缩氮气,循环吸附4～5h；然后取出活性炭用离心机甩干,并放置在82～86℃的温度条件蒸干至含水量在0.15～0.3％,获得超低汞催化剂。本发明涉及的氯乙烯合成用超低汞催化剂制备方法,其能够制备出氯乙烯合成用的超低汞催化剂,避免使用高毒性汞催化剂所带来的环境污染问题。(Compared with the prior art, the preparation method of the ultralow-mercury catalyst for vinyl chloride synthesis disclosed by the application comprises the following steps of: obtaining raw material coal; deashing raw material coal; carbonizing treatment; activating treatment; treating the activated carbon to obtain a carrier; preparing a hydrochloric acid solution; preparing an adsorbent; adsorption treatment: placing the adsorbent powder in 70% ethanol solution, stirring at 1000rpm for 30min to obtain adsorption solution; then placing the activated carbon in an adsorption bed, firstly purging the system by using nitrogen to discharge impurity gases such as oxygen, carbon dioxide and the like; starting a circulating system, simultaneously starting an ultrasonic auxiliary system, introducing compressed nitrogen, and circularly adsorbing for 4-5 hours; and then taking out the activated carbon, spin-drying the activated carbon by using a centrifuge, and placing the activated carbon at the temperature of 82-86 ℃ for drying by distillation until the water content is 0.15-0.3%, thereby obtaining the ultra-low mercury catalyst. The preparation method of the ultralow-mercury catalyst for vinyl chloride synthesis can prepare the ultralow-mercury catalyst for vinyl chloride synthesis, and avoids the problem of environmental pollution caused by the use of a high-toxicity mercury catalyst.)

1. The preparation method of the ultralow-mercury catalyst for vinyl chloride synthesis is characterized by comprising the following steps of:

obtaining raw material coal;

deashing raw material coal: grinding anthracite coal into coal powder, putting the coal powder into 30ppm polyaluminium chloride solution, strongly stirring at the rotating speed of 4800-5200 r/min, reducing the rotating speed to 450-550/min after 1.5-2.5 minutes, and filtering after stirring for 8-12 minutes; washing with distilled water until the filtrate is neutral; adding a polyacrylamide solution, stirring for 8-12 minutes at a polyacrylamide concentration of 0.5ppm and a rotation speed of 380-420 r/min, then filtering, washing with distilled water until the filtrate is neutral, and the ash content after deashing is 1.5%;

carbonizing treatment;

activation treatment: carrying out acid dipping treatment on the carbonized coal powder, wherein the mass ratio of acid to fixed carbon in the coal powder is 3:1, and washing and drying after soaking for 4-6 hours; placing the dried coal powder into a mixed solution of a secondary activating agent, soaking for 2 hours, wherein the mass ratio of the secondary activating agent to fixed carbon is 1:0.8, and then activating for 2 hours at 480 ℃ under the condition of nitrogen flow of 10ml/mim to obtain an activated material;

treating activated carbon to obtain a carrier: cooling the activated material to room temperature, soaking the activated material in a hydrochloric acid solution with the mass percentage of 3-4.8% for 12 hours, washing the activated material to be neutral by distilled water, and drying the activated material to obtain activated carbon;

preparing a hydrochloric acid solution, soaking activated carbon in the prepared hydrochloric acid solution for 28-32 minutes, enabling the hydrochloric acid solution to continuously flow by using a circulating pump during the soaking, taking out the solution for filtering or carrying out spin-drying dehydration and drying by using a centrifugal machine, and drying at the temperature of 200 ℃ until the water content is below 3% to obtain an activated carbon carrier;

preparing an adsorbent: mixing the active component and the accelerator according to the mass ratio of 2:1, and dry-grinding for 6 hours under the protection of nitrogen to obtain adsorbent powder with the fineness of 800 meshes;

adsorption treatment: obtaining an adsorption solution, namely placing the adsorbent powder into an ethanol solution with the concentration of 70%, and stirring for 30min at 1000rpm to obtain the adsorption solution; placing the activated carbon in an adsorption bed, firstly purging a system by using nitrogen to discharge impurity gases such as oxygen, carbon dioxide and the like;

starting an ultrasonic auxiliary system while circulating the adsorption liquid through the adsorption bed, wherein the ultrasonic frequency is 50-54 KHz, compressed nitrogen is introduced at the same time, the air pressure of the air flow is 0.8-1.2 MPa, the introduction amount of the nitrogen air flow is 18-22 kg/min, and the adsorption is circulated for 4-5 hours; and then taking out the activated carbon, spin-drying the activated carbon by using a centrifuge, and placing the activated carbon at the temperature of 82-86 ℃ for drying by distillation until the water content is 0.15-0.3%, thereby obtaining the ultra-low mercury catalyst.

2. The method for preparing the ultra-low mercury catalyst for vinyl chloride synthesis according to claim 1, wherein the deashing raw material coal is specifically: grinding anthracite, sieving with a 100-mesh sieve, putting the coal powder into 30ppm polyaluminium chloride solution, strongly stirring at the rotation speed of 5000r/min for 2 minutes, reducing the rotation speed to 500r/min, stirring for 10 minutes, filtering, and washing with distilled water until the filtrate is neutral; adding into polyacrylamide solution with a polyacrylic acid concentration of 0.5ppm and a rotation speed of 400r/min, stirring for 10 min, filtering, washing with distilled water until the filtrate is neutral, and deashing to obtain an ash content of 1.5%.

3. The method for preparing the ultra-low mercury catalyst for vinyl chloride synthesis according to claim 2, wherein the carbonization treatment specifically comprises: carbonizing the deashed coal powder under the protection of nitrogen flow of 20ml/mim, wherein the initial temperature of the carbonization temperature is 280 ℃, the temperature is increased to 380-420 ℃ at the heating rate of 2 ℃/min, and the carbonization time is 2-3 hours, so that the carbonized material is obtained.

4. The method for preparing the ultra-low mercury catalyst for vinyl chloride synthesis according to claim 3, wherein the coal dust carbonized by acid dipping in the activation treatment is specifically: impregnating carbonized coal powder with acid, wherein the acid comprises: phosphoric acid, tartaric acid and stearic acid in a mass ratio of 3:1:2, wherein the mass ratio of the acid to the fixed carbon in the coal powder is 3:1, soaking for 5 hours, washing with water and drying.

5. The method for preparing the ultra-low mercury catalyst for vinyl chloride synthesis according to claim 4, wherein the secondary activator is zinc chloride, bismuth chloride, magnesium chloride and lead nitrate in a mass ratio of 3:2:1: 1.

6. The method for preparing the ultra-low mercury catalyst for vinyl chloride synthesis according to claim 1, wherein the active components comprise tin iodide, bismuth oxide, copper chloride and tin dioxide in a mass ratio of 4:2:1: 3.

7. The method for preparing the ultra-low mercury catalyst for vinyl chloride synthesis according to claim 1, wherein the promoter component comprises ferric trichloride, magnesium chloride, calcium chloride, p-chlorobenzoic acid and aluminum triacetylacetonate in a mass ratio of 1:3:2:1: 1.

8. The preparation method of the ultralow-mercury catalyst for vinyl chloride synthesis according to claim 1, wherein an ultrasonic auxiliary system is started, the ultrasonic frequency is 50-54 KHz, compressed nitrogen is introduced, and the air pressure of the air flow is specifically as follows: under the pressure of 1.1MPa, the introduction amount of nitrogen gas flow is specifically 21.5kg/min, and the cyclic adsorption is carried out for 4.5 h; and then taking out the activated carbon, spin-drying the activated carbon by using a centrifuge, and placing the activated carbon at 85 ℃ for drying until the water content is 0.15-0.3%.

Technical Field

The application relates to the technical field of catalysts, in particular to a preparation method of an ultralow-mercury catalyst for vinyl chloride synthesis.

Background

At present, the industrial production method of vinyl chloride mainly comprises an ethylene equilibrium oxychlorination method and an acetylene hydrochlorination method, wherein the specific gravity of the vinyl chloride synthesized by the coal-based acetylene hydrochlorination method in the polyvinyl chloride industry in China is close to 80%, the industrial catalyst used in the method is an activated carbon-loaded mercury chloride catalyst (HgCl2/AC), the mercury catalyst is easy to sublimate and run off to cause environmental pollution, the toxicity of HgCl2 threatens the safety of the environment and human beings, the problem of mercury pollution in the acetylene hydrochlorination method process is solved, and the development of an environment-friendly ultralow-mercury catalyst is urgently needed.

Therefore, how to provide a method for preparing an ultra-low mercury catalyst for vinyl chloride synthesis, which can avoid the problem of environmental pollution caused by using a highly toxic mercury catalyst, has become a technical problem to be solved by those skilled in the art.

Disclosure of Invention

In order to solve the technical problems, the application provides a preparation method of an ultralow-mercury catalyst for vinyl chloride synthesis, which can avoid the problem of environmental pollution caused by the use of a high-toxicity mercury catalyst.

The technical scheme provided by the application is as follows:

the application provides a preparation method of an ultralow-mercury catalyst for vinyl chloride synthesis, which comprises the following steps: obtaining raw material coal;

deashing raw material coal: grinding anthracite coal into coal powder, putting the coal powder into 30ppm polyaluminium chloride solution, strongly stirring at the rotating speed of 4800-5200 r/min, reducing the rotating speed to 450-550/min after 1.5-2.5 minutes, stirring for 8-12 minutes, filtering, and washing with distilled water until filtrate is neutral; adding a polyacrylamide solution, wherein the concentration of the polyacrylamide is 0.5ppm, the rotating speed is 380-420 r/min, stirring for 8-12 minutes, filtering, washing with distilled water until the filtrate is neutral, and the ash content after deashing is 1.5%;

carbonizing treatment;

activation treatment: carrying out acid dipping treatment on the carbonized coal powder, wherein the mass ratio of acid to fixed carbon in the coal powder is 3:1, and washing and drying after soaking for 4-6 hours; placing the dried coal powder into a mixed solution of a secondary activating agent, soaking for 2 hours, wherein the mass ratio of the secondary activating agent to fixed carbon is 1:0.8, and then activating for 2 hours at 480 ℃ under the condition of nitrogen flow of 10ml/mim to obtain an activated material;

treating activated carbon to obtain a carrier: cooling the activated material to room temperature, soaking the activated material in a hydrochloric acid solution with the mass percentage of 3-4.8% for 12 hours, washing the activated material to be neutral by distilled water, and drying the activated material to obtain activated carbon;

preparing a hydrochloric acid solution, soaking activated carbon in the prepared hydrochloric acid solution for 28-32 minutes, enabling the hydrochloric acid solution to continuously flow by using a circulating pump during the soaking, taking out the solution for filtering or carrying out spin-drying dehydration and drying by using a centrifugal machine, and drying at the temperature of 200 ℃ until the water content is below 3% to obtain an activated carbon carrier;

preparing an adsorbent: mixing the active component and the accelerator according to the mass ratio of 2:1, and dry-grinding for 6 hours under the protection of nitrogen to obtain adsorbent powder with the fineness of 800 meshes;

adsorption treatment: placing the adsorbent powder in 70% ethanol solution, stirring at 1000rpm for 30min to obtain adsorption solution; then placing the activated carbon in an adsorption bed, firstly purging the system by using nitrogen to discharge impurity gases such as oxygen, carbon dioxide and the like;

starting a circulating system to enable the adsorption liquid to circularly pass through the adsorption bed, simultaneously starting an ultrasonic auxiliary system, simultaneously introducing compressed nitrogen with the ultrasonic frequency of 50-54 KHz, wherein the air pressure of the air flow is 0.8-1.2 MPa, the introduction amount of the nitrogen air flow is 18-22 kg/min, and circularly adsorbing for 4-5 h; and then taking out the activated carbon, spin-drying the activated carbon by using a centrifuge, and placing the activated carbon at the temperature of 82-86 ℃ for drying by distillation until the water content is 0.15-0.3%, thereby obtaining the ultra-low mercury catalyst.

Further, in a preferred embodiment of the present invention, the deashing-treated raw material coal is specifically: grinding anthracite, sieving with a 100-mesh sieve, putting the coal powder into 30ppm polyaluminium chloride solution, strongly stirring at the rotation speed of 5000r/min for 2 minutes, reducing the rotation speed to 500r/min, stirring for 10 minutes, filtering, and washing with distilled water until the filtrate is neutral; adding into polyacrylamide solution with a polyacrylic acid concentration of 0.5ppm and a rotation speed of 400r/min, stirring for 10 min, filtering, washing with distilled water until the filtrate is neutral, and deashing to obtain an ash content of 1.5%.

Further, in a preferred embodiment of the present invention, the carbonization treatment specifically includes: carbonizing the deashed coal powder under the protection of nitrogen flow of 20ml/mim, wherein the initial temperature of the carbonization temperature is 280 ℃, the temperature is increased to 380-420 ℃ at the heating rate of 2 ℃/min, and the carbonization time is 2-3 hours to obtain a carbonized material;

further, in a preferred embodiment of the present invention, the coal dust carbonized by the acid dipping treatment in the activation treatment specifically includes: impregnating carbonized coal powder with acid, wherein the acid comprises: phosphoric acid, tartaric acid and stearic acid in a mass ratio of 3:1:2, wherein the mass ratio of the acid to the fixed carbon in the coal powder is 3:1, soaking for 5 hours, washing with water and drying.

Further, in a preferred mode of the invention, the secondary activating agent is zinc chloride, bismuth chloride, magnesium chloride and lead nitrate, and the mass ratio is 3:2:1: 1.

Further, in a preferred mode of the present invention, the active component is tin iodide, bismuth oxide, copper chloride, and tin dioxide, and the mass ratio is 4:2:1: 3.

Further, in a preferred mode of the invention, the promoter components are ferric trichloride, magnesium chloride, calcium chloride, p-chlorobenzoic acid and aluminum triacetylacetonate in a mass ratio of 1:3:2:1: 1.

Further, in a preferred mode of the present invention, the ultrasonic auxiliary system is started, the ultrasonic frequency is 50 to 54KHz, and compressed nitrogen is introduced, wherein the air pressure of the air flow specifically is: under the pressure of 1.1MPa, the introduction amount of nitrogen gas flow is specifically 21.5kg/min, and the cyclic adsorption is carried out for 4.5 h; and then taking out the activated carbon, spin-drying the activated carbon by using a centrifuge, and placing the activated carbon at 85 ℃ for drying until the water content is 0.15-0.3%.

Compared with the prior art, the preparation method of the ultralow-mercury catalyst for vinyl chloride synthesis provided by the invention comprises the following steps: obtaining raw material coal; deashing raw material coal: grinding anthracite coal into coal powder, putting the coal powder into 30ppm polyaluminium chloride solution, strongly stirring at the rotating speed of 4800-5200 r/min, reducing the rotating speed to 450-550/min after 1.5-2.5 minutes, stirring for 8-12 minutes, filtering, and washing with distilled water until filtrate is neutral; adding a polyacrylamide solution, wherein the concentration of the polyacrylamide is 0.5ppm, the rotating speed is 380-420 r/min, stirring for 8-12 minutes, filtering, washing with distilled water until the filtrate is neutral, and the ash content after deashing is 1.5%; carbonizing treatment; activation treatment: carrying out acid dipping treatment on the carbonized coal powder, wherein the mass ratio of acid to fixed carbon in the coal powder is 3:1, and washing and drying after soaking for 4-6 hours; placing the dried coal powder into a mixed solution of a secondary activating agent, soaking for 2 hours, wherein the mass ratio of the secondary activating agent to fixed carbon is 1:0.8, and then activating for 2 hours at 480 ℃ under the condition of nitrogen flow of 10ml/mim to obtain an activated material; treating activated carbon to obtain a carrier: cooling the activated material to room temperature, soaking the activated material in a hydrochloric acid solution with the mass percentage of 3-4.8% for 12 hours, washing the activated material to be neutral by distilled water, and drying the activated material to obtain activated carbon; preparing a hydrochloric acid solution, soaking activated carbon in the prepared hydrochloric acid solution for 28-32 minutes, enabling the hydrochloric acid solution to continuously flow by using a circulating pump during the soaking, taking out the solution for filtering or carrying out spin-drying dehydration and drying by using a centrifugal machine, and drying at the temperature of 200 ℃ until the water content is below 3% to obtain an activated carbon carrier; preparing an adsorbent: mixing the active component and the accelerator according to the mass ratio of 2:1, and dry-grinding for 6 hours under the protection of nitrogen to obtain adsorbent powder with the fineness of 800 meshes; adsorption treatment: placing the adsorbent powder in 70% ethanol solution, stirring at 1000rpm for 30min to obtain adsorption solution; then placing the activated carbon in an adsorption bed, firstly purging the system by using nitrogen to discharge impurity gases such as oxygen, carbon dioxide and the like; starting a circulating system to enable the adsorption liquid to circularly pass through the adsorption bed, simultaneously starting an ultrasonic auxiliary system, simultaneously introducing compressed nitrogen with the ultrasonic frequency of 50-54 KHz, wherein the air pressure of the air flow is 0.8-1.2 MPa, the introduction amount of the nitrogen air flow is 18-22 kg/min, and circularly adsorbing for 4-5 h; and then taking out the activated carbon, spin-drying the activated carbon by using a centrifuge, and placing the activated carbon at the temperature of 82-86 ℃ for drying by distillation until the water content is 0.15-0.3%, thereby obtaining the ultra-low mercury catalyst. The preparation method of the ultralow-mercury catalyst for vinyl chloride synthesis can prepare the ultralow-mercury catalyst for vinyl chloride synthesis, and can avoid the problem of environmental pollution caused by the use of a high-toxicity mercury catalyst.

Detailed Description

In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.

It will be understood that the terms "length," "width," "upper," "lower," "front," "rear," "first," "second," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like, as used herein, refer to an orientation or positional relationship indicated for convenience and simplicity of description, and do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and is therefore not to be considered as limiting.

Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, the meaning of a plurality of or a plurality of is two or more unless specifically limited otherwise.

The preparation method of the ultralow-mercury catalyst for vinyl chloride synthesis provided by the embodiment of the application comprises the following steps: deashing raw material coal: grinding anthracite coal into coal powder, putting the coal powder into 30ppm polyaluminium chloride solution, strongly stirring at the rotating speed of 4800-5200 r/min, reducing the rotating speed to 450-550/min after 1.5-2.5 minutes, stirring for 8-12 minutes, filtering, and washing with distilled water until filtrate is neutral; adding a polyacrylamide solution, wherein the concentration of the polyacrylamide is 0.5ppm, the rotating speed is 380-420 r/min, stirring for 8-12 minutes, filtering, washing with distilled water until the filtrate is neutral, and the ash content after deashing is 1.5%;

carbonizing treatment;

activation treatment: carrying out acid dipping treatment on the carbonized coal powder, wherein the mass ratio of acid to fixed carbon in the coal powder is 3:1, and washing and drying after soaking for 4-6 hours; placing the dried coal powder into a mixed solution of a secondary activating agent, soaking for 2 hours, wherein the mass ratio of the secondary activating agent to fixed carbon is 1:0.8, and then activating for 2 hours at 480 ℃ under the condition of nitrogen flow of 10ml/mim to obtain an activated material;

treating activated carbon to obtain a carrier: cooling the activated material to room temperature, soaking the activated material in a hydrochloric acid solution with the mass percentage of 3-4.8% for 12 hours, washing the activated material to be neutral by distilled water, and drying the activated material to obtain activated carbon;

preparing a hydrochloric acid solution, soaking activated carbon in the prepared hydrochloric acid solution for 28-32 minutes, enabling the hydrochloric acid solution to continuously flow by using a circulating pump during the soaking, taking out the solution for filtering or carrying out spin-drying dehydration and drying by using a centrifugal machine, and drying at the temperature of 200 ℃ until the water content is below 3% to obtain an activated carbon carrier;

preparing an adsorbent: mixing the active component and the accelerator according to the mass ratio of 2:1, and dry-grinding for 6 hours under the protection of nitrogen to obtain adsorbent powder with the fineness of 800 meshes;

adsorption treatment: placing the adsorbent powder in 70% ethanol solution, stirring at 1000rpm for 30min to obtain adsorption solution; then placing the activated carbon in an adsorption bed, firstly purging the system by using nitrogen to discharge impurity gases such as oxygen, carbon dioxide and the like;

starting a circulating system to enable the adsorption liquid to circularly pass through the adsorption bed, simultaneously starting an ultrasonic auxiliary system, simultaneously introducing compressed nitrogen with the ultrasonic frequency of 50-54 KHz, wherein the air pressure of the air flow is 0.8-1.2 MPa, the introduction amount of the nitrogen air flow is 18-22 kg/min, and circularly adsorbing for 4-5 h; and then taking out the activated carbon, spin-drying the activated carbon by using a centrifuge, and placing the activated carbon at the temperature of 82-86 ℃ for drying by distillation until the water content is 0.15-0.3%, thereby obtaining the ultra-low mercury catalyst.

The embodiment of the invention provides a preparation method of an ultralow-mercury catalyst for vinyl chloride synthesis, which specifically comprises the following steps: obtaining raw material coal; deashing raw material coal: grinding anthracite coal into coal powder, putting the coal powder into 30ppm polyaluminium chloride solution, strongly stirring at the rotating speed of 4800-5200 r/min, reducing the rotating speed to 450-550/min after 1.5-2.5 minutes, stirring for 8-12 minutes, filtering, and washing with distilled water until filtrate is neutral; adding a polyacrylamide solution, wherein the concentration of the polyacrylamide is 0.5ppm, the rotating speed is 380-420 r/min, stirring for 8-12 minutes, filtering, washing with distilled water until the filtrate is neutral, and the ash content after deashing is 1.5%; carbonizing treatment; activation treatment: carrying out acid dipping treatment on the carbonized coal powder, wherein the mass ratio of acid to fixed carbon in the coal powder is 3:1, and washing and drying after soaking for 4-6 hours; placing the dried coal powder into a mixed solution of a secondary activating agent, soaking for 2 hours, wherein the mass ratio of the secondary activating agent to fixed carbon is 1:0.8, and then activating for 2 hours at 480 ℃ under the condition of nitrogen flow of 10ml/mim to obtain an activated material; treating activated carbon to obtain a carrier: cooling the activated material to room temperature, soaking the activated material in a hydrochloric acid solution with the mass percentage of 3-4.8% for 12 hours, washing the activated material to be neutral by distilled water, and drying the activated material to obtain activated carbon; preparing a hydrochloric acid solution, soaking activated carbon in the prepared hydrochloric acid solution for 28-32 minutes, enabling the hydrochloric acid solution to continuously flow by using a circulating pump during the soaking, taking out the solution for filtering or carrying out spin-drying dehydration and drying by using a centrifugal machine, and drying at the temperature of 200 ℃ until the water content is below 3% to obtain an activated carbon carrier; preparing an adsorbent: mixing the active component and the accelerator according to the mass ratio of 2:1, and dry-grinding for 6 hours under the protection of nitrogen to obtain adsorbent powder with the fineness of 800 meshes; adsorption treatment: placing the adsorbent powder in 70% ethanol solution, stirring at 1000rpm for 30min to obtain adsorption solution; then placing the activated carbon in an adsorption bed, firstly purging the system by using nitrogen to discharge impurity gases such as oxygen, carbon dioxide and the like; starting a circulating system to enable the adsorption liquid to circularly pass through the adsorption bed, simultaneously starting an ultrasonic auxiliary system, simultaneously introducing compressed nitrogen with the ultrasonic frequency of 50-54 KHz, wherein the air pressure of the air flow is 0.8-1.2 MPa, the introduction amount of the nitrogen air flow is 18-22 kg/min, and circularly adsorbing for 4-5 h; and then taking out the activated carbon, spin-drying the activated carbon by using a centrifuge, and placing the activated carbon at the temperature of 82-86 ℃ for drying by distillation until the water content is 0.15-0.3%, thereby obtaining the ultra-low mercury catalyst. The preparation method of the ultralow-mercury catalyst for vinyl chloride synthesis can prepare the ultralow-mercury catalyst for vinyl chloride synthesis, and can avoid the problem of environmental pollution caused by the use of a high-toxicity mercury catalyst.

Specifically, in the embodiment of the present invention, the raw material coal for deliming treatment specifically includes: grinding anthracite, sieving with a 100-mesh sieve, putting the coal powder into 30ppm polyaluminium chloride solution, strongly stirring at the rotation speed of 5000r/min for 2 minutes, reducing the rotation speed to 500r/min, stirring for 10 minutes, filtering, and washing with distilled water until the filtrate is neutral; adding into polyacrylamide solution with a polyacrylic acid concentration of 0.5ppm and a rotation speed of 400r/min, stirring for 10 min, filtering, washing with distilled water until the filtrate is neutral, and deashing to obtain an ash content of 1.5%.

Specifically, in the embodiment of the present invention, the carbonization treatment specifically includes: carbonizing the deashed coal powder under the protection of nitrogen flow of 20ml/mim, wherein the initial temperature of the carbonization temperature is 280 ℃, the temperature is increased to 380-420 ℃ at the heating rate of 2 ℃/min, and the carbonization time is 2-3 hours to obtain a carbonized material;

specifically, in the embodiment of the present invention, the coal dust carbonized by acid immersion in the activation treatment specifically includes: impregnating carbonized coal powder with acid, wherein the acid comprises: phosphoric acid, tartaric acid and stearic acid in a mass ratio of 3:1:2, wherein the mass ratio of the acid to the fixed carbon in the coal powder is 3:1, soaking for 5 hours, washing with water and drying.

Specifically, in the embodiment of the invention, the secondary activating agent is zinc chloride, bismuth chloride, magnesium chloride and lead nitrate, and the mass ratio is 3:2:1: 1.

Specifically, in the embodiment of the invention, the active components are tin iodide, bismuth oxide, copper chloride and tin dioxide, and the mass ratio is 4:2:1: 3.

Specifically, in the embodiment of the invention, the promoter components comprise ferric trichloride, magnesium chloride, calcium chloride, p-chlorobenzoic acid and aluminum triacetylacetone in a mass ratio of 1:3:2:1: 1.

Specifically, in the embodiment of the present invention, the ultrasonic auxiliary system is started, the ultrasonic frequency is 50 to 54KHz, compressed nitrogen is introduced, and the air pressure of the air flow specifically is: under the pressure of 1.1MPa, the introduction amount of nitrogen gas flow is specifically 21.5kg/min, and the cyclic adsorption is carried out for 4.5 h; and then taking out the activated carbon, spin-drying the activated carbon by using a centrifuge, and placing the activated carbon at 85 ℃ for drying until the water content is 0.15-0.3%.

The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.