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Method for low-mercury catalyst with good heat stability

A low-mercury catalyst and thermal stability technology, applied in the field of fine chemistry, can solve the problems of poor thermal stability, high loss rate of mercuric chloride, poor mechanical properties of the catalyst, etc., and achieve the effect of good thermal stability and low loss rate

Active Publication Date: 2015-12-30
NINGXIA JINHAI CHUANGKE CHEM TECH
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] (1) The mechanical properties of the catalyst itself are poor;
[0005] (2) Poor thermal stability and high loss rate of mercury chloride;
[0006] (3) For the synthesis reaction of vinyl chloride, the conversion rate of acetylene is low, the selectivity of vinyl chloride is low, and the yield of vinyl chloride is low

Method used

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  • Method for low-mercury catalyst with good heat stability

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1 A kind of preparation method of low mercury catalyst with good thermal stability

[0027] Step 1 Preparation of Activated Carbon

[0028] (1) Selection of raw coal

[0029] The raw coal is anthracite, with a moisture content of 6%, an ash content of 8.5%, a volatile matter content of 14.5%, and a fixed carbon content of 71%.

[0030] (2) Deashing of raw coal

[0031] Grind anthracite, pass through a 100-mesh sieve, put the coal powder in 13% HF solution, oscillate ultrasonically at 60°C for 7 hours, filter, wash with distilled water until the filtrate is neutral, then put the washed sample into 40% HCl solution, 75 ° C ultrasonic vibration for 6 hours, filtered, washed with distilled water until the filtrate was neutral; then let it into the 50ppm polyacrylamide solution, first stirred at 5000r / min for 15 minutes, then lowered to 2000r / min Stir at high speed for 8 minutes, filter, and wash with distilled water until the filtrate is neutral.

[0032]...

Embodiment 2

[0055] Embodiment 2 thermal stability test

[0056] Mercury chloride catalyst prepared by the present invention carries out stability test under 260 ℃ of conditions, and measurement result is as follows:

[0057]

[0058] Under the condition of 260℃ for 100h, the content of mercuric chloride is 4.089%, and the loss rate of mercuric chloride is 4.90%.

Embodiment 3

[0059] Embodiment 3 above-mentioned catalyst is used for vinyl chloride synthetic reaction

[0060] 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.

[0061] The reaction tail gas was analyzed by chromatography, and the conversion rate of acetylene was 99.93%, the selectivity of vinyl chloride was nearly 100%, and the yield of vinyl chloride was 95.2%.

[0062] Unless otherwise specified, the percentages used in the present invention are all weight percentages, and the ratios described in the present invention are all mass ratios.

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Abstract

A provided method for low-mercury catalyst with good heat stability comprises preparation of active carbon, preparation of an adsorption solution, and adsorption processing. The adsorption processing steps comprises ultrasonic assisted adsorption, microwave assisted adsorption and vacuum penetration adsorption. The prepared low-mercury catalyst comprises, in percent by weight, 4.3% of mercuric chloride, 8.6% of zinc chloride, 8.6% of palladium chloride, 2.87% of platinum chloride, 2.87% of tetrabutyl ammonium chloride, 2.87% of tripotasium triphenylphosphine-3,3',3''-trisulfonate, and 0.18% of water. The low-mercury catalyst possesses the mechanical strength of 98.6%, the granularity of 3-6 mm (98%), the bulk density of 460 g / L, and the mercuric chloride ignition loss of 0.39%. The prepared low-mercury catalyst is good in heat stability and low in mercuric chloride loss rate. When the low-mercury catalyst is applied to vinyl chloride synthesis reaction, the acetylene conversion rate is 99.93%, the vinyl chloride selectivity is close to 100%, and the vinyl chloride yield is 95.2%.

Description

technical field [0001] The invention relates to a preparation method of a low-mercury catalyst with good thermal stability, belonging to the technical field of fine chemistry. Background technique [0002] Catalysts used in industry include high-mercury catalysts and low-mercury catalysts. The mercury chloride content of high-mercury catalysts is 10-12%, and the mercury chloride content of low-mercury catalysts is 4-6.5%. Due to the high content of mercuric chloride in the high-mercury catalyst, the consumption of mercury is large, and it is now being phased out. The application scale of low-mercury catalyst is gradually expanding. The low-mercury catalyst disclosed in Chinese patent CN200610012455.0 has activated carbon as the carrier, contains 4-6.5% of mercury chloride, and the auxiliary component is zinc chloride. It is prepared by impregnation method and is currently on the market. Most of the low-mercury catalysts used are produced by this company. The composition of...

Claims

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Application Information

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IPC IPC(8): B01J31/24B01J31/30C07C17/08C07C21/06
Inventor 李通常炳恩李建平李玉强李庆孙玉梅
Owner NINGXIA JINHAI CHUANGKE CHEM TECH
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