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Method for recycling waste mercury catalyst from polyvinyl chloride production based on calcium carbide method

A waste mercury catalyst, polyvinyl chloride technology, applied in chemical recovery, chemical instruments and methods, mercury halide and other directions, can solve the problems of low recovery rate, pollute the environment, high energy consumption, etc., achieve simple operation, reduced energy consumption, The effect of low heating temperature

Active Publication Date: 2017-05-17
HWASU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, recovery of waste mercury catalysts is usually done by steaming waste mercury catalysts together with lime water to convert mercuric chloride into mercuric oxide, and then turn mercuric oxide into elemental mercury at a high temperature of 700-800°C. The recovery rate of this method is low. It is only about 57%, and the energy consumption is large; there are also poisonous chlorine gas reclaimed mercury and mercuric chloride in the heating process, and the final dry distillation tail gas is treated to regenerate mercury-containing wastewater and pollute the environment; Adsorbed organic substances and hydrogen chloride acidic substances are effectively removed, affecting the quality of recovered substances

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A method for recovering waste mercury catalysts in the production of calcium carbide polyvinyl chloride, comprising the steps of:

[0020] (1) First 100g of waste mercury catalyst is pulverized to a fineness of 40 meshes, and the waste mercury catalyst refers to a deactivated catalyst with 2% mercuric chloride, 1% hydrogen chloride and 0.4% vinyl chloride adsorbed on the activated carbon;

[0021] (2) Extract the above-mentioned crushed waste mercury catalyst with 150ml carbon disulfide to remove vinyl chloride, and filter to obtain the filter residue;

[0022] (3) The above filter residue was heated to 90°C under dark conditions, sublimated for 120 minutes to obtain mercuric chloride vapor, and then condensed and recovered at 18°C ​​to obtain 1.92g of mercuric chloride solid with a purity of 99.5%, with a recovery rate of 96%;

[0023] (4) Treat the remaining filter residue after the above recovery of mercuric chloride with 120g of 20% sodium hydroxide aqueous solution...

Embodiment 2

[0025] A method for recovering waste mercury catalysts in the production of calcium carbide polyvinyl chloride, comprising the steps of:

[0026] (1) First 100g of waste mercury catalyst is pulverized to a fineness of 80 meshes, and the waste mercury catalyst refers to an inactivated catalyst with 3.8% mercuric chloride, 0.5% hydrogen chloride and 0.1% vinyl chloride adsorbed on the activated carbon;

[0027] (2) Extract the above-mentioned crushed waste mercury catalyst with 300ml carbon disulfide to remove vinyl chloride, and filter to obtain filter residue;

[0028] (3) The above filter residue was heated to 120°C under dark conditions, sublimated for 30 minutes to obtain mercuric chloride vapor, and then condensed and recovered at 10°C to obtain 3.69g of mercuric chloride solid with a purity of 99.6%, with a recovery rate of 97%;

[0029] (4) Treat the remaining filter residue after the above recovery of mercuric chloride with 80 g of 54% sodium hydroxide aqueous solution,...

Embodiment 3

[0031] A method for recovering waste mercury catalysts in the production of calcium carbide polyvinyl chloride, comprising the steps of:

[0032] (1) First 100g of waste mercury catalyst is pulverized to a fineness of 60 meshes, and the waste mercury catalyst refers to an inactivated catalyst with 2.9% mercuric chloride, 0.7% hydrogen chloride and 0.2% vinyl chloride adsorbed on the activated carbon;

[0033] (2) Extract the above-mentioned crushed waste mercury catalyst with 220ml carbon disulfide to remove vinyl chloride, and filter to obtain the filter residue;

[0034] (3) The above filter residue was heated to 105°C under dark conditions, sublimated for 75 minutes to obtain mercuric chloride vapor, and then condensed and recovered at 25°C to obtain 2.76g of mercuric chloride solid with a purity of 99.5%, with a recovery rate of 95%;

[0035] (4) Treat the remaining filter residue after the above recovery of mercuric chloride with 105 g of 35% sodium hydroxide aqueous solu...

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Abstract

The invention provides a method for recycling a waste mercury catalyst from polyvinyl chloride production based on a calcium carbide method. The method comprises the following steps: smashing the waste mercury catalyst with mercuric chloride, hydrogen chloride and vinyl chloride attached to activated carbon into certain fineness; extracting with carbon disulfide and filtering, thereby acquiring filter residues; heating and then condensing the filter residues under a light-shielding condition to recycle mercuric chloride; treating the filter residues with alkali, neutralizing the absorbed hydrogen chloride, filtering, drying and recycling the activated carbon. The recycling method provided by the invention has the advantages that the heating temperature for recycling the mercuric chloride is low, the recycling of the mercuric chloride can be carried out only at 90-120 DEG C, the recovery rate reaches up to 95% and the purity reaches up to 99.5%; after the recycled activated carbon is treated, the purity is high, the recovery rate reaches up to 92%, the absorption activity is recovered, the micro-pore surface area is recovered to 1000-1200m<2> / g and the pore volume is recovered to 0.3-0.6ml / g; besides, according to the method, the operation is simple, the energy consumption is low, the environment-friendly and pollution-free effects are achieved; the organic substances, such as chloroethylene, and the hydrogen chloride acidic material can be effectively removed.

Description

technical field [0001] The invention relates to the field of catalyst recovery, in particular to a method for recovering waste mercury catalysts in the production of calcium carbide polyvinyl chloride. Background technique [0002] In the production process of polyvinyl chloride by calcium carbide method, acetylene and hydrogen chloride are used as raw materials, mercuric chloride and activated carbon are used as catalysts to carry out catalytic reaction to synthesize vinyl chloride monomer, and then the vinyl chloride monomer is polymerized to form polyvinyl chloride. With the progress of the catalytic reaction, the content of mercuric chloride which is easy to sublimate in the activated carbon is reduced to less than 4%. At the same time, the catalyst is gradually deactivated due to the adsorption of excess raw hydrogen chloride gas and product vinyl chloride in the pores of the activated carbon. As my country's environmental protection requirements are becoming increasing...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G13/04C01B32/354C01B32/36B01J20/20B01J20/28
CPCY02P20/584C01G13/04B01J20/20B01J20/28066B01J20/28073B01J2220/4893C01P2006/12C01P2006/14C01P2006/80
Inventor 李毅丘永桂魏昭辉王明建陈群涛
Owner HWASU
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