Method for preparing vinyl chloride by hydrochlorinating acetylene through using quaternary phosphonium long-chain ionic liquid as medium

A technology for producing vinyl chloride and ionic liquids by chlorination, which is applied in hydrogen halide addition preparation, organic chemistry and other directions, can solve problems such as low conversion rate, and achieve the effects of avoiding local overheating, avoiding environmental pollution, and being environmentally friendly.

Active Publication Date: 2014-10-22
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 o...

Method used

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Embodiment 1

[0031] Equivalent molar amount of octanoic acid [P 4444 ][OH](40% aqueous solution) was stirred and reacted in a round bottom flask at a temperature of 318.15K for 24h to obtain an aqueous solution of the target ionic liquid. Then the ionic liquid aqueous solution is decompressed and rotated to remove water at 323.15K, and then dried under high vacuum for 48h to obtain tetrabutylphosphine octanoate ionic liquid [P 4444 ][C 7 COO].

[0032] Tetrabutylphosphine octanoate ionic liquid [P 4444 ][C 7 Characterization of physical properties of COO]: 1H NMR (500MHz, DMSO-d6, δ / ppm relative to TMS): 0.85(3H, t; COO-CH 3 ),0.92(12H,t; P-CH 3),1.17-1.27(8H,m; COO-(C) 2 -(CH 2 ) 4 ),1.36-1.49(18H,m; P-C-(CH 2 ) 2 and COO-C-CH 2 ), 1.74(2H,t; COO-CH 2 ), and2.20-2.26(8H,m; P-CH 2 ).13C NMR (500MHz, DMSO-d6, δ / ppm relative to TMS) 175.15, 39.55, 31.91, 30.06, 29.40, 27.26, 23.92, 23.80, 23.18, 23.15, 22.63, 17.59, 14.44, 13.74.

[0033] Get 20ml synthetic quaternary phosphoni...

Embodiment 2

[0035] Prepare tributylhexylphosphine palmitate ionic liquid by the method in embodiment 1 [P 6444 ][C 15 COO], and the physical properties were characterized.

[0036] Get the synthetic quaternary phosphonium type ionic liquid tributylhexylphosphine palmitate ionic liquid of 20ml [P 6444 ][C 15 COO], to which 268.90 mg of copper chloride CuCl was added 2 Catalyst, the molar concentration of the catalyst in the ionic liquid is 0.1mol / L, fully mixed and dissolved at a temperature of 140° C. for 40 minutes, and then moved to the reaction device. Pre-pass hydrogen chloride for 1 h to activate the catalytic system before the reaction, then raise the reaction temperature to 180°C for reaction, the flow rate of acetylene is 5ml / min, the molar ratio of reactant hydrogen chloride to acetylene is 0.8:1, the reaction tail gas is deacidified and dried analyzed by gas chromatography. According to gas chromatography analysis, the conversion rate after the reaction is stable can reach ...

Embodiment 3

[0038] Prepare tributyloctylphosphine laurate ionic liquid [P by the method in embodiment 1 8444 ][C 11 COO], and the physical properties were characterized.

[0039] Get 20ml synthetic quaternary phosphonium type ionic liquid tributyloctylphosphine laurate ionic liquid [P 8444 ][C 11 COO], to which was added 207.17 mg of chloroplatinic acid H 2 PtCl 6 ·6H 2 O catalyst, the molar concentration of the catalyst in the ionic liquid is 0.02mol / L, fully mixed and dissolved at a temperature of 120°C for 40min and then moved to the reaction device. Pre-pass hydrogen chloride for 1 hour to activate the catalytic system before the reaction, then raise the reaction temperature to 160°C for reaction, the flow rate of acetylene is 5ml / min, the molar ratio of reactant hydrogen chloride to acetylene is 1:1, and the reaction tail gas is deacidified and dried analyzed by gas chromatography. According to gas chromatography analysis, the conversion rate after the reaction is stable can r...

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Abstract

The invention discloses a method for preparing vinyl chloride by hydrochlorinating acetylene through using a quaternary phosphonium long-chain ionic liquid as a medium. The method comprises the following steps: dissolving a catalyst in a quaternary phosphonium long-chain anion functional ionic liquid medium to prepare a catalysis system, activating the catalysis system by introducing hydrogen chloride in advance, and introducing acetylene and hydrogen chloride to carry out a reaction. The method using the ionic liquid as the reaction medium and a mercury-free compound as the catalyst realizes the green and environmentally-friendly liquid phase reaction of acetylene hydrochlorination, has a very good catalysis efficiency, and makes the acetylene conversion rate reach 80-98% and the vinyl chloride selectivity reach above 99.5%.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing vinyl chloride by hydrochlorination of acetylene using a quaternary phosphonium long-chain anion ionic liquid as a medium. Background technique [0002] Polyvinyl chloride (PVC) is widely used in our lives as a plastic material, which is produced by polymerization of vinyl chloride monomer (VCM). At present, there are two main methods for the preparation of vinyl chloride monomer in industry, one is the acetylene method derived from the coal chemical industry route, and the other is the ethylene method derived from the petrochemical route. In my country, coal resources are abundant and oil resources are relatively scarce, so the acetylene hydrochlorination reaction derived from the coal chemical industry route is the main production process for the synthesis of vinyl chloride monomer in my country, accounting for more than 70% of vinyl chloride pr...

Claims

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Application Information

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IPC IPC(8): C07C17/08C07C21/06
Inventor 邢华斌胡静逸任其龙杨启炜苏宝根张志国杨亦文鲍宗必
Owner ZHEJIANG UNIV
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