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Ruthenium catalyst for producing vinyl chloride, and preparation method thereof

A ruthenium catalyst and catalyst technology are applied in the directions of catalyst activation/preparation, hydrogen halide addition preparation, chemical instruments and methods, etc., can solve problems such as sublimation loss of ruthenium catalyst, achieve good economy and industrial application value, convenient operation, The effect of enhancing stability

Active Publication Date: 2018-03-16
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The purpose of the present invention is to fundamentally solve the problem of ruthenium catalyst sublimation and loss in the reaction of acetylene hydrochlorination to vinyl chloride, and to provide a ruthenium-based catalyst for acetylene hydrochlorination with good stability and high reactivity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Select columnar activated carbon as the carrier, its particle size is 40 mesh, the ash content is 3.0wt%, and the specific surface area is 800m 2 / g, pore volume 0.6ml / g, and treated with 200ml of 10wt% hydrochloric acid at 25°C for 3.5h. Dry at 110°C for 10 hours and set aside. 50ml of RuCl 3 The solution (wherein the Ru content is 0.002g / ml) is mixed with 5g of 1-butyl-3-methylimidazolium chloride salt, and the mixed solution is added dropwise on the 100g activated carbon carrier under the action of ultrasonic waves at 30°C. The soaking time is 8 hours. Then at 30°C, add 10ml of Na to the above system dropwise under the action of ultrasound. 2 S solution (wherein the S content is 0.01g / ml), and soaked for 10 hours under the action of ultrasonic waves. The impregnated catalyst was vacuum-dried at 110°C for 6 hours to obtain catalyst A, wherein the Ru loading (relative to the mass of the support) was 0.1wt%, the S loading (relative to the mass of the support) was 0....

Embodiment 2

[0055] Select columnar carbon nanotubes as the carrier, the particle size is 50 mesh, the ash content is 3.0wt%, and the specific surface area is 200m 2 / g, the pore volume is 0.66ml / g. Mix 12.5ml of ammonium hexachlororuthenate solution (wherein the Ru content is 0.08g / ml) and 20g of tributylethylphosphine bromide, and add the mixed solution dropwise to 100g of carbon nanotubes under ultrasonic action at 40°C On the carrier, the impregnation time is 5 hours under the action of ultrasonic waves. Then, at 40°C, 10ml of KHS solution (in which the S content is 0.5g / ml) and 43.5ml of deionized water were added dropwise to the above system under the action of ultrasonic waves, and immersed for 6 hours under the action of ultrasonic waves. The impregnated catalyst was vacuum-dried at 100°C for 8 hours to obtain catalyst B, in which the Ru loading (relative to the mass of the support) was 1 wt%, the S loading (relative to the mass of the support) was 5 wt%, and the loading of the io...

Embodiment 3

[0058] Select columnar graphene as the carrier, its particle size is 80 mesh, the ash content is 2.1wt%, and the specific surface area is 2630m 2 / g, the pore volume is 1.5ml / g. Mix 100ml of potassium pentachlororuthenate (III) solution (wherein the Ru content is 0.004g / ml) and 10g of tributylmethylammonium chloride, and add the mixed solution dropwise to 100g of graphene carrier under the action of ultrasonic waves at 20°C On, the immersion time is 4 hours under the action of ultrasonic waves. Then at 20°C, add 20ml of (NH 4 ) 2 S 2 o 3 solution (wherein the S content is 0.2g / ml) and 30ml deionized water, and soaked for 8 hours under the action of ultrasonic waves. The impregnated catalyst was vacuum-dried at 90°C for 9 hours to obtain catalyst C, in which the Ru loading (relative to the mass of the support) was 0.4wt%, the S loading (relative to the mass of the support) was 4wt%, and the loading of the ionic liquid was 10wt%. .

[0059] Take 2g of this catalyst and appl...

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Abstract

The invention discloses a supported ionic liquid-promoted ruthenium catalyst. A preparation method of the ruthenium catalyst comprises the following steps: mixing a prepared ruthenium-containing solution with an ionic liquid to obtain a mixed solution; dropwise adding the mixed solution to a porous solid carrier under the action of ultrasonic waves at 20-60 DEG C, and performing impregnation underthe action of the ultrasonic waves for 0.5-6 h; dropwise adding an inorganic salt solution to the mixed solution-impregnated porous solid carrier under the action of the ultrasonic waves, and performing impregnation under the action of the ultrasonic waves for 1-20 h; and performing vacuum drying at 60-120 DEG C for 6-30 h to obtain the supported ionic liquid-promoted ruthenium catalyst. The catalyst has the advantages of low load capacity, high activity and good stability when used in acetylene hydrochlorination for synthesizing vinyl chloride, and has a great economical efficiency and greatindustrial application values.

Description

Background technique [0001] Polyvinyl chloride (PVC) is the third most commonly used plastic, which is obtained by polymerization of monomer vinyl chloride. Due to the energy occurrence characteristics of rich coal, poor oil and little gas in my country, the preparation of vinyl chloride by coal-based calcium carbide acetylene method is the mainstream process of polyvinyl chloride production in my country. Mercury chloride is currently used as a catalyst for the synthesis of vinyl chloride in the industry. Because it causes serious pollution to the environment, and the synthesized polyvinyl chloride contains a small amount of mercury, the application of polyvinyl chloride is limited. Therefore, mercuric chloride catalysts will be gradually eliminated, and the synthesis of vinyl chloride under non-mercury catalyst conditions will become the main direction for the sustainable development of calcium carbide PVC in the future. The reported mercury-free catalysts mainly use metal ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28C07C17/08C07C21/06
CPCB01J31/0292B01J31/28B01J37/024B01J37/343B01J2231/32C07C17/08C07C21/06
Inventor 赵佳李小年狄淑霞翟媛媛王柏林岳玉学盛刚锋吕井辉卢春山姚楠马磊江大好倪珺
Owner ZHEJIANG UNIV OF TECH
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