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Preparation and recovery method of an ultra-low mercury catalyst with high catalytic activity

A catalytic activity and catalyst technology, applied in the field of fine chemistry, can solve the problems of low conversion selectivity, low yield of vinyl chloride, unsatisfactory catalytic effect of catalyst, and long activation time of hydrogen chloride, so as to shorten the activation time, reduce the dosage and improve the recovery rate. high effect

Active Publication Date: 2018-06-22
李通
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) High mercury content and poor mechanical properties;
[0006] (2) For the synthesis reaction of vinyl chloride, the catalytic effect of the catalyst is not ideal, the catalytic activity is not high, the conversion rate of acetylene, the selectivity of vinyl chloride, and the yield of vinyl chloride are low;
[0007] (3) High unit consumption and large dosage;
[0008] (4) Low catalytic efficiency;
[0010] (6) It is used in the synthesis reaction of vinyl chloride, and the activation time of hydrogen chloride is longer;
[0011] (7) When the catalyst is recovered, the recovery rate of mercuric chloride is low, the purity is low, and the recovered activated carbon has poor performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1 A kind of preparation method of the high ultra-low mercury catalyst of catalytic activity

[0042] Step 1 Selection of activated carbon

[0043] Carbon tetrachloride adsorption 115%, iodine value 1250mg / g, moisture 2.5%, ash 1.8%, mechanical strength 97.9%, bulk density 375g / l, particle size 3.0-3.1mm, specific surface area 1600m 2 / g, the average pore volume is 0.68~0.72 ml / g, and the average pore diameter is 2.4-2.6nm long flame coal activated carbon.

[0044] Step 2 Pretreatment of activated carbon

[0045] Put the activated carbon in 3 times the volume of nitric acid with a concentration of 1.8mol / L, heat and stir until reflux for 3 hours, then wash the activated carbon with distilled water to pH = 7, dry the surface moisture at 50°C, and then vacuum at 80°C Dry to constant weight, place the activated carbon in a 2.8wt% urea solution that is 4.2 times its volume, heat and stir until refluxed for 2.8 hours, filter with suction and dry the surface moist...

Embodiment 2

[0063] Example 2 The above-mentioned catalyst is used in the synthetic reaction of vinyl chloride

[0064] In the reaction that the catalyst of the present invention is used to prepare vinyl chloride by acetylene hydrochlorination, the molar ratio of the reaction feed gas is C 2 h 2 / HCl=1 / 1.08, the space velocity of acetylene is 65h -1 , the reaction temperature is 110°C, and the hydrogen chloride activation time is 20 minutes.

[0065] The reaction tail gas is analyzed by chromatography, and the conversion rate of acetylene is 99.92-99.93%, the selectivity of vinyl chloride is nearly 100%, the yield of vinyl chloride is 94.9-95.0%, and the unit consumption of the catalyst is low, and the unit consumption of the catalyst is 0.0012-0.0013 g / ml vinyl chloride; catalytic efficiency increased by 2-3 m 3 / h; the reaction temperature is reduced to 110°C, and the reaction temperature of the prior art is above 130°C, the amount of catalyst is less, and the amount is reduced by 7-8...

Embodiment 3

[0066] Example 3 A recovery method for an ultra-low mercury catalyst with high catalytic activity

[0067] (1) Separation of activated carbon

[0068] Add 200g of mercuric chloride catalyst into 600ml of water, heat to 200°C, carry out hot-melt pretreatment under stirring, adjust the pH value to 2, and carry out ultrasonic treatment at 200°C, ultrasonic treatment parameters: power 130 W, frequency 300 kHz, processing time 4-5 s, interval time 2-6 s, cycle ultrasonic, filter for 42 minutes, remove activated carbon, and recycle.

[0069] (2) Separation of mercuric chloride

[0070] The filtrate passes through the macroporous sulfhydryl ion exchanger to adsorb mercury ions, and the adsorption flow rate is 3BV / h; then it is eluted with concentrated hydrochloric acid (35%), and the elution process is: elution with concentrated hydrochloric acid (35%) 14BV, Flow rate 3BV / h, then elute 11BV, flow rate 5BV / h; finally elute 6BV, flow rate 3BV / h, collect eluate, remove hydrochloric ac...

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PUM

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Abstract

The present invention provides a preparation method for an ultra-low mercury catalyst with high catalytic activity and a method for recycling it, including the selection of activated carbon, the preparation of adsorption liquid, and adsorption. The adsorption includes gas phase adsorption and liquid phase adsorption; the invention also provides the Catalyst recovery methods. The ultra-low mercury catalyst prepared by the invention contains, in terms of weight percentage, 1.4% mercury chloride, 2% barium chloride, 1.5% potassium chloride, 1.5% ammonium chloride platinum acid, 1% tetraammine platinum dichloride, 0.2% water, mechanical strength 97.3%, particle size 3~6mm (97.8%), bulk density 515g / l; high catalytic activity, acetylene conversion rate reaches 99.92-99.93%, vinyl chloride selectivity is nearly 100%, vinyl chloride The yield reaches 94.9-95.0%; the ultra-low mercury catalyst prepared by the invention has low unit consumption, low dosage and high catalytic efficiency; the catalyst recovery method of the invention has a high mercury chloride recovery rate and high purity.

Description

technical field [0001] The invention relates to the preparation and recovery method of an ultra-low mercury catalyst with high catalytic activity, belonging to the technical field of fine chemistry. Background technique [0002] At present, the industrial acetylene hydrochlorination reaction mainly uses high-mercury catalysts with a loading of mercuric chloride of 12% to 15%, and its consumption of mercury accounts for 60% of the domestic mercury consumption, and it is harmful to the environment and human beings. Serious hazard to health. [0003] In view of the scarcity of mercury resources and the pollution of the environment, as well as the increasingly stringent policies on the prevention and control of mercury pollution at home and abroad, there is an urgent need for breakthroughs in the improvement of the performance of mercury chloride and the research of high-performance and environmentally friendly catalysts to meet the needs of industrial production. At the same t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/18B01J27/13B01J27/10B01J38/72B01J38/74
CPCB01J27/10B01J27/13B01J31/1805B01J38/72B01J38/74B01J35/19
Inventor 李通常炳恩李建平李玉强李庆孙玉梅
Owner 李通
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