Vulcanized ionic liquid complex palladium catalyst, and preparation method and applications thereof

A technology of ionic liquid and palladium catalyst, which is applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, catalytic reaction, etc., can solve the problem that is not suitable for improving the deactivation and large-scale The limitations of the industrial application of production equipment, and the problems that have not been fundamentally resolved, have achieved good economics, industrial application value, high stability, and low load.

Active Publication Date: 2018-02-23
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Chinese patent application (CN 102357336 A) discloses using molecular sieves such as HZSM-5, NaZSM-5, and zeolite as carriers to support PdCl 2 The prepared catalyst, at the feed gas ratio V (HCl) /V (C2H2) Under the condition of =1.15, the acetylene hydrochlorination reaction performance test was carried out at 160 °C, and the reaction tail gas was analyzed. The initial conversion rate of acetylene of the catalyst was 89.78%, and the selectivity of vinyl chloride was 98.62%. The catalyst activity was low and did not meet the requirements of industrialization
Chinese patent CN101716528 discloses an ionic liquid dissolving metal chlorides such as gold, platinum, palladium, tin, mercury, copper or rhodium as a catalyst system, which is applied to acetylene hydrochlorination, but the reaction system belongs to a gas-liquid reaction system, and there is The mass transfer efficiency of reactants and products is low, stirring or pneumatic stirring is easy to cause t

Method used

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  • Vulcanized ionic liquid complex palladium catalyst, and preparation method and applications thereof
  • Vulcanized ionic liquid complex palladium catalyst, and preparation method and applications thereof
  • Vulcanized ionic liquid complex palladium catalyst, and preparation method and applications thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0066] 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 950m 2 / g, the pore volume is 0.45mL / g, and treated with 300ml of 10wt% hydrochloric acid at 25°C for 3h. The treated carrier was washed with deionized water until neutral, dried at 110° C. for 12 hours, and then ready for use.

[0067] Synthesis of sulfide ionic liquid A:

[0068] Mix the ionic liquid 1-butyl-3-methylimidazolium chloride and sulfur powder at a mass ratio of 1:0.5, stir in a water bath at 40°C for 10 minutes, then add acetonitrile solution, dissolve, and stir at 40°C for 12 hours, Stir the above mixture evenly, then filter to remove unreacted sulfur powder, dry the obtained filtrate at 110°C, then dissolve the sample obtained after drying in dichloromethane, add an appropriate amount of Ionized water and sodium bicarbonate solution were used to further remove impurities in the solution. Finally, the above mixed sol...

Embodiment 2

[0072] The main difference between this example and Example 1 is that the types of ionic liquids are different, and its influence on the catalytic performance of the catalyst is studied.

[0073] Synthesis of sulfide ionic liquid B:

[0074] Mix ionic liquid 1-propyl-3-methylimidazolium tetrafluoroborate and sulfur powder according to the mass ratio of 1:0.5, stir in a water bath at 40°C for 10 minutes, then add acetonitrile solution, dissolve, and stir at 40°C After 12 hours, stir the above mixture evenly, then filter to remove unreacted sulfur powder, and dry the obtained filtrate at 110°C, then dissolve the sample obtained after drying into dichloromethane, add Appropriate amount of deionized water and sodium bicarbonate solution to further remove impurities in the solution, and finally, dry the above mixed solution at 110°C for 16 hours, and then recrystallize at room temperature to obtain the desired sulfide ionic liquid b.

[0075] Select columnar activated carbon as t...

Embodiment 3

[0079] 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 950m 2 / g, pore volume 0.6mL / g, and treated with 300ml of 10wt% hydrochloric acid at 25°C for 3h. The treated carrier was washed with deionized water until neutral, dried at 110° C. for 12 hours, and then ready for use.

[0080] Synthesis of sulfide ionic liquid A:

[0081] Mix the ionic liquid 1-butyl-3-methylimidazolium chloride and sulfur powder at a mass ratio of 1:0.5, stir in a water bath at 40°C for 10 minutes, then add acetonitrile solution, dissolve, and stir at 40°C for 12 hours, Stir the above mixture evenly, then filter to remove unreacted sulfur powder, dry the obtained filtrate at 110°C, then dissolve the sample obtained after drying in dichloromethane, add an appropriate amount of Ionized water and sodium bicarbonate solution were used to further remove impurities in the solution. Finally, the above mixed solution wa...

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Abstract

The invention discloses a vulcanized ionic liquid complex palladium catalyst, and a preparation method and applications thereof. According to the preparation method, an ionic liquid is subjected to sulfuration modification to introduce sulfur containing groups, and the treated ionic liquid is loaded with PdCl2 precursor so as to form a Pd-S-IL system with a special structure, and increase both thereaction activity and the stability of the palladium catalyst. The supported ionic liquid promoted palladium catalyst possesses relatively high stability in ethyne hydrochlorination, after 6000h of operation, no palladium loss is detected, the highest ethyne conversion rate is 99.8%, and the highest vinyl chloride selectivity is 99.95%.

Description

Background technique [0001] Polyvinyl chloride (PVC) is an important general-purpose plastic. Due to the energy storage characteristics of rich coal, poor oil and little gas in my country, the preparation of vinyl chloride by 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, the mercury chloride catalyst will be gradually eliminated, and the synthesis of vinyl chloride under the condition of mercury-free catalyst will become the main direction for the future sustainable development of calcium carbide method PVC. Mercury-free catalysts mainly use metal chlorides as active components, among which noble metal chlorides exhibit the bes...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J31/26C07C17/08C07C21/06
CPCB01J31/226B01J31/26B01J2231/32B01J2531/824C07C17/08C07C21/06
Inventor 李小年赵佳张群峰丰枫
Owner ZHEJIANG UNIV OF TECH
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