Method for catalyzing ethyne hydrochlorination reaction by utilizing metal nanoparticle/ionic liquid system

A metal nanoparticle, acetylene hydrochlorination technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc. The problem of the loss of active components of the catalyst, to achieve the effect of low vapor pressure, reduced volatility, high activity and high stability of catalysis

Active Publication Date: 2015-10-28
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these two types of ionic liquids are relatively low in terms of conversion rate, and there is still a certain gap with industrial reactions.
[0007] The Chinese patent documents whose publication numbers are CN104086351A and CN104109076A respectively disclose the method for preparing vinyl chloride by hydrochlorination of acetylene using nitrogen heterocyclic protonic acid ionic liquid and quaternary phosphonium long-chain anion functionalized ionic liquid as medium. Dissolved in ionic liquids for catalytic reactions, among which nitrogen heterocyclic protonic acid ionic liquids are easy to prepare, have great economic advantages, and the conversion rate can reach more than 70%, while the conversion rate of acetylene in quaternary phosphonium long-chain anion functionalized ionic liquids can reach 80% % to 98%, but the metal salt has a certain volatility. During the high-temperature hydrochlorination reaction of acetylene, it is easy to lose the active components of the catalyst due to volatilization, resulting in catalyst deactivation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] To 20ml surface active ionic liquid tetrabutyl phosphopalmitate [P 4444 ][C 15 COO], add 0.04mol / L catalyst precursor platinum chloride PtCl 2 , the nano-platinum / ionic liquid system can be prepared in situ by feeding hydrogen gas at 60°C for 2 hours.

[0048] Pre-flow hydrogen chloride at a temperature of 60°C for 3 hours to activate the catalytic system. Then heat up to the reaction temperature of 200°C, control the flow rate of acetylene to 5ml / min, and react with the volume-to-molecular flow rate ratio of hydrogen chloride and acetylene at 1:1. The reaction tail gas is deacidified, dried, and then passed to gas chromatography for analysis. The conversion rate of acetylene in the nano-platinum / ionic liquid system can reach 96%, the selectivity of vinyl chloride is greater than 99.5%, the catalytic activity does not decrease after 120 hours of reaction, and the catalytic system is very stable.

Embodiment 2

[0050] Add 0.05mol / L of catalyst precursor palladium chloride PdCl to 20ml of surface-active ionic liquid 1-ethyl-3-methylimidazolium diisooctyl sulfosuccinate [Emim][AOT] 2 and 0.5 mol / L sodium borohydride, mixed and stirred at 25° C. for 2 hours, and the nano-palladium / ionic liquid system can be prepared in situ.

[0051] Pre-flow hydrogen chloride at a temperature of 120°C for 1 h to activate the catalytic system. Then the temperature was raised to the reaction temperature of 180°C, the flow rate of acetylene was controlled to be 5ml / min, and the molar ratio of hydrogen chloride to acetylene was 1.15:1 for the reaction. The conversion rate of acetylene in the nano-palladium / ionic liquid system can reach 90%, the selectivity of vinyl chloride is greater than 99.5%, no decline in catalytic activity is seen after 120 hours of reaction, and the catalytic system is very stable.

Embodiment 3

[0053] To 20ml surface active ionic liquid 1-octyl-3-methylimidazolium trifluoromethanesulfonate [Omim][CF 3 SO 3 ], add 0.01mol / L catalyst precursor chloroauric acid HAuCl 4 4H 2 O, mixing and stirring at 120°C for 1 h, the nano-gold / ionic liquid system can be prepared in situ.

[0054] At a temperature of 80°C, pass hydrogen chloride for 2 hours in advance to activate the catalytic system. Then the temperature was raised to the reaction temperature of 160°C, the flow rate of acetylene was controlled to be 5ml / min, and the molar ratio of hydrogen chloride to acetylene was 1.2:1 for the reaction. The conversion rate of acetylene in the nano-gold / ionic liquid system can reach 85%, the selectivity of vinyl chloride is greater than 99.5%, the catalytic activity does not decrease after 40 hours of reaction, and the catalytic system is very stable.

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PUM

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Abstract

The invention discloses a method for catalyzing ethyne hydrochlorination reaction by utilizing a metal nanoparticle / ionic liquid system. The method comprises the steps that a metal nanoparticle / ionic liquid phase catalytic system is prepared, ionic liquid is surface activity ionic liquid, under the temperature ranging from 60 DEG C to 120 DEG C, hydrogen chloride is pumped into the metal nanoparticle / ionic liquid phase catalytic system, activation is carried out, warming is carried out until the temperature ranges from 140 DEG C to 220 DEG C, ethyne and the hydrogen chloride are pumped, the reaction is carried out, and after processing is carried out, a chloroethylene product gas is obtained. The special surface activity ionic liquid and a metal nanoparticle are subjected to in-situ reaction or compounding, the metal nanoparticle / ionic liquid system is obtained, the metal nanoparticle / ionic liquid system is utilized to catalyze the ethyne hydrochlorination reaction, the ethyne converting rate can reach up to 99% in a maximum mode, the chloroethylene selectivity is larger than 99.5%, and the catalytic system has the best cycling stability.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for catalyzing acetylene hydrochlorination by using a metal nanoparticle / ionic liquid system. Background technique [0002] Vinyl chloride (VCM) is a colorless, liquefied gas at room temperature, and is an important chemical raw material for the synthesis of polyvinyl chloride resin (PVC). As one of the five most widely used general-purpose plastics, PVC is widely used in various industries such as medical supplies, building materials, and clothing because of its properties such as wear resistance, heat resistance, corrosion resistance, high mechanical strength, and good insulation. At present, the synthesis methods of vinyl chloride are mainly divided into the acetylene method and the ethylene method. Most foreign companies use the ethylene method with petroleum as the raw material. Hydrochlorination has become the main source of vinyl chloride production in m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/06C07C17/08B01J31/02B01J31/04
Inventor 邢华斌胡静逸任其龙杨启炜苏宝根张治国杨亦文鲍宗必
Owner ZHEJIANG UNIV
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