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Application of composite carrier ruthenium-based catalyst in acetylene hydrochlorination reaction

A technology of acetylene hydrochlorination and ruthenium-based catalyst, applied in the field of catalysis, can solve the problems of low activity and poor stability of ruthenium-based catalyst, and achieve the effects of slowing down the rate of carbon deposition, reducing the content, and avoiding agglomeration and side reactions.

Active Publication Date: 2020-09-11
XINJIANG CORPS MODERN GREEN CHLOR ALKALI CHEM ENG RES CENT LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the problem of mercury pollution in the process of synthesizing vinyl chloride by acetylene hydrochlorination, the invention provides a composite carrier ruthenium-based catalyst used in acetylene hydrochlorination to solve the problems of low activity and poor stability of low-content ruthenium-based catalysts

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Select 30g of columnar coal-based activated carbon carrier, wash with water, remove ash and dry before use. Weigh 0.0153g of zirconium chloride and dissolve it in 80ml of cold water, pour it into activated carbon and stir thoroughly, and then soak for 2 hours; weigh 0.0645g of phosphoric acid and dilute it with 10ml of water, then add it drop by drop into activated carbon, white flocs are formed, and keep stirring until After adding phosphoric acid dropwise, let it stand for 6 hours, stir evenly, pour out the impregnating solution, wash with distilled water for 2 times and dry, and then roast at 300°C for 4 hours under a nitrogen atmosphere to obtain the catalyst carrier.

[0020] Weigh 0.0924g of ruthenium trichloride and add 60ml of water to dissolve it, pour it into the activated carbon treated in the previous step and stir thoroughly, place it at room temperature for 6 hours, then dry it in an oven at 80°C for about 6 hours until there is no obvious impregnating solu...

Embodiment 2

[0023] Select 30g of columnar wooden activated carbon carrier, wash with water, remove ash and dry for later use. Weigh 0.0530g of zirconium oxychloride and dissolve it in 80ml of water, pour it into activated carbon and fully stir and impregnate for 3 hours; weigh 0.0508g of hydroxyethylidene diphosphonic acid and disperse and dilute it with 10ml of water, then add it drop by drop into activated carbon, and keep stirring until the phosphine After adding the acid dropwise, let it stand for 4 hours, stir evenly, pour out the impregnating solution, wash it with distilled water twice and dry it, and then bake it at 300°C for 4 hours under a nitrogen atmosphere to obtain the catalyst carrier.

[0024] Weigh 0.1231g of ruthenium trichloride and add 60ml of water to dissolve it, pour it into the activated carbon treated in the previous step and stir thoroughly, after standing at room temperature for 5 hours, dry it in an oven at 70°C for about 7 hours until there is no obvious impreg...

Embodiment 3

[0027] Select 30g of powdered coconut shell activated carbon carrier, wash with water, remove ash and dry before use. Weigh 0.1360g of zirconium carbonate and dissolve it in 70ml of water, pour it into activated carbon and fully stir and impregnate for 2h; weigh 0.1967g of aminotrimethylene phosphonic acid, disperse and dilute it with 10ml of water, then add it drop by drop to the activated carbon, and keep stirring until the phosphonic acid is added dropwise. After standing for 3 hours, stir evenly and pour the impregnating solution, then wash with distilled water for 3 times and dry, and then roast at 300°C for 4 hours under a nitrogen atmosphere to obtain the catalyst carrier.

[0028] Weigh 0.1847g of ruthenium trichloride and add 60ml of water to dissolve it, pour it into the activated carbon treated in the previous step and stir thoroughly, after standing at room temperature for 4 hours, dry it in an oven at 60°C for about 7 hours until there is no obvious impregnating li...

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PUM

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Abstract

The invention discloses an application of a composite carrier ruthenium-based catalyst in acetylene hydrochlorination reaction. A composite carrier of the catalyst is formed by dipping and loading phosphorus / zirconium phosphonate on activated carbon, and the main preparation process comprises the following steps: dissolving a zirconium precursor with water, adding ash-removed and dried activated carbon, fully stirring and dipping the precursor and activated carbon, dropwise adding a phosphorus / phosphonic acid solution, fully stirring and standing the mixture, washing the mixture with water, and drying and roasting the mixture to prepare the catalyst. The carrier is impregnated and loaded with any one of ruthenium trichloride, ruthenium acetate and terpyridyl ruthenium chloride to prepare the mercury-free ruthenium-based catalyst for acetylene hydrochlorination reaction. The catalyst prepared by the invention has the characteristics of high activity, good selectivity, simple productionmethod, environmental friendliness and the like, and new power is further added for the mercury-free industrial process of the calcium carbide method polyvinyl chloride industry.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to the preparation of a phosphorus / zirconium phosphonate composite carrier ruthenium-based catalyst and its application in acetylene hydrochlorination. Background technique [0002] Polyvinyl chloride is one of the five major synthetic resins in the world, widely used in important fields of the national economy such as industry, agriculture, and building materials. The synthesis methods mainly include calcium carbide acetylene method, ethylene method, dichloroethane cracking method, ethane oxychlorination method, etc. my country's energy structure determines that the production process of calcium carbide polyvinyl chloride has long occupied a dominant position. [0003] Vinyl chloride is made from acetylene and hydrogen chloride, HgCl 2 / AC is synthesized by catalyst reaction. Mercury chloride is volatile and highly toxic, which has a negative impact on the environm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/02B01J27/16B01J35/10B01J27/185B01J31/02B01J31/38B01J31/22B01J31/04C07C17/08C07C21/06
CPCB01J37/0201B01J27/16B01J27/1856B01J31/0267B01J31/0269B01J31/1815B01J31/2239B01J31/04C07C17/08B01J35/61C07C21/06
Inventor 王小艳宋晓玲周军李国栋陈万银李静张学鲁郑伟玲庞晓东赵忠峰司江坤夏锐周佳王伟夏轮超
Owner XINJIANG CORPS MODERN GREEN CHLOR ALKALI CHEM ENG RES CENT LTD
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