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
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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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Abstract
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