Method for preparing low mercury catalyst by using activated carbon with high carbon tetrachloride adsorption value

A technology for the preparation of activated carbon and low-mercury catalysts, applied in the field of fine chemistry, can solve the problems of poor mechanical properties of catalysts, low yield of vinyl chloride, low conversion rate of acetylene, etc., and achieve the effect of improving catalytic efficiency

Active Publication Date: 2016-03-23
NINGXIA JINHAI CHUANGKE CHEM TECH
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  • Abstract
  • Description
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Problems solved by technology

[0006] (1) The mechanical properties of the catalyst itself are poor;
[0007] (2) Used in the synthesis reaction of vinyl chloride, the conversion rate o

Method used

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Experimental program
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Embodiment 1

[0033] Embodiment 1 A kind of method adopting high carbon tetrachloride adsorption value gac to prepare low mercury catalyst

[0034] Step 1. Selection of activated carbon

[0035] The carbon tetrachloride adsorption value of described gac is 135%, iodine value 1550mg / g, methylene blue value 135mg / g, moisture content 2%, ash content 0.7%, mechanical strength 99.5%, bulk density 416g / L, specific surface area is 1780m 2 / g, the average pore diameter is 3.1-3.2nm.

[0036] Step 2, treatment of activated carbon

[0037] The activated carbon prepared by the present invention is placed in 5 times the volume of nitric acid with a concentration of 2.6 mol / L, heated and stirred to reflux for 2 hours, then the activated carbon is washed with distilled water to pH=6.9, and the surface moisture is dried at 55° C., and then Vacuum dry at 92°C to constant weight; place the activated carbon in a urea solution with a concentration 5 times its volume of 3.5wt%, heat and stir until ref...

Embodiment 2

[0054] Embodiment 2 above-mentioned catalyst is used for synthetic reaction of vinyl chloride

[0055] In the reaction that the catalyst of the present invention is used to prepare vinyl chloride by hydrochlorination of acetylene, the molar ratio of the reaction feed gas is C 2 h 2 / HCl=1 / 1.1, the space velocity of acetylene is 70h -1 , the reaction temperature is 112°C, and the hydrogen chloride activation time is 20 minutes.

[0056] The reaction tail gas is analyzed by chromatography, and the conversion rate of acetylene is 99.98%, and the yield of vinyl chloride is 97.3%; the activation time of hydrogen chloride is shortened; the sublimation amount of mercuric chloride is small in the reaction process, and after 6000 hours, the accumulation of mercuric chloride The sublimation amount is 0.86%; the catalytic efficiency is high, and the catalytic efficiency is increased by 5.6m 3 / h.

[0057] Unless otherwise specified, the percentages used in the present invention are...

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Abstract

The present invention provides a method for preparing a low mercury catalyst by using activated carbon with a high carbon tetrachloride adsorption value. The method comprises gas phase adsorption, absorption solution preparation and microwave absorption. The microwave absorption comprises first-stage microwave absorption. The first-stage microwave absorption is performed at the temperature of 60 DEG C, the microwave wavelength is 139 mm, the frequency is 2650 MHz, the power is 310 w, and the adsorption treatment lasts for 10 minutes. The method has the beneficial effects that the low mercury catalyst prepared by the method provided by the present invention comprises the following components in percentages by weight: 4.91% of chlorinated mercury, 4% of zinc chloride, 2% of palladium chloride, 2% of platinum chloride, 2% of tetrabutyl ammonium chloride, 2% of triphenylphosphine sulfonic acid potassium and 0.20% of water; the mechanical strength is 99.6%, the particle size is 3-6 mm (99.8%), and the bulk density is 516 g/L; and In the synthesis reaction of vinyl chloride, the conversion rate of acetylene reaches 99.98%, and the yield of the vinyl chloride reaches 97.3%.

Description

technical field [0001] The invention relates to a method for preparing a low-mercury catalyst by using activated carbon with a high carbon tetrachloride adsorption value, and belongs to the technical field of fine chemistry. Background technique [0002] In the reaction of acetylene hydrochlorination to prepare vinyl chloride, it has been reported at home and abroad that noble metals such as platinum, palladium, and gold are used as the main catalytic components. Although the activity is high, the stability is not as good as that of high mercury catalysts, and the cost is too high to be Realize industrial production, and when using tin, bismuth, copper, zinc and other base metal compounds as main catalyst components, the loss of its active components is more serious. [0003] The mercury chloride content of high-mercury catalysts is 10-12%. Due to the high mercury chloride content of high-mercury catalysts and high mercury consumption, they are now being phased out, and the ...

Claims

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Application Information

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IPC IPC(8): B01J27/138B01J37/34B01J37/00
CPCB01J27/138B01J37/00B01J37/346
Inventor 李玉强常炳恩李建平李通李庆孙玉梅
Owner NINGXIA JINHAI CHUANGKE CHEM TECH
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