A load type [pdscl x ] x- Catalyst and its preparation and application in the synthesis of vinyl chloride

A catalyst and supported technology, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, catalytic reactions, etc., can solve problems such as sublimation loss, and achieve simple preparation, convenient operation, and high activity and stability effects

Active Publication Date: 2020-10-09
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The object of the present invention is to overcome the shortcoming that palladium catalyst sublimates and loses in the synthetic vinyl chloride reaction of acetylene hydrochlorination, provides a kind of [PdSCl that the loading type ionic liquid of good stability, high reactivity promotes. x ] x- Composite catalyst (where x=1, 2 or 3) and its application in acetylene hydrochlorination

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Spherical activated carbon was selected as the carrier, with a particle size of 30 mesh, an ash content of 4.6wt%, and a specific surface area of ​​900 m 2 / g, pore volume 1.1mL / g, and treated with 500ml of nitric acid with a concentration of 10wt% at 20°C for 20h, dried at 100°C for 20h, and set aside. 50ml of K 2 PdCl 4 solution (in which the Pd content is 0.001g / ml), 10ml of (NH 4 ) 2 S solution (in which the S content is 0.01g / ml) and 2.5g of the chloride salt of N-hexylpyridine are mixed, and an appropriate amount of deionized water is added to make the volume to 110ml; at 20°C, the mixture is added dropwise under the action of ultrasound onto 100g of spherical activated carbon, and impregnated under vacuum conditions and ultrasonic waves for 0.5 hours; then vacuum-dried at 60°C for 30 hours to obtain the supported ionic liquid-promoted [PdSCl x ] x- A composite catalyst, wherein the Pd loading (relative to the mass of the support) is 0.05wt%, the loading of t...

Embodiment 2

[0050] Select columnar carbon nanotubes as the carrier, the particle size is 80 mesh, the ash content is 2.4wt%, and the specific surface area is 500m 2 / g, pore volume 0.85mL / g. 20ml of (NH 4 ) 2 PdCl 4 solution (wherein the Pd content is 0.05g / ml), 10ml of NaHSO 3 solution (wherein the S content is 0.5g / ml) and 25g of N-butyl-N-methylpyrrolidone chloride salt are mixed, and an appropriate amount of deionized water is added to make the volume to 85ml; at 60°C, the mixed Droplets were added to 100g columnar carbon nanotubes, and impregnated under vacuum conditions and ultrasonic waves for 8 hours; then vacuum-dried at 120°C for 2 hours to obtain the supported ionic liquid-promoted [PdSCl x ] x-A composite catalyst, wherein the Pd loading (relative to the mass of the carrier) is 1 wt%, the loading of the S element (relative to the mass of the carrier) is 5 wt%, and the loading of the ionic liquid (relative to the mass of the carrier) is 25 wt%.

[0051] Take 2g of this ca...

Embodiment 3

[0053] Select columnar SiO 2 As a carrier, its particle size is 50 mesh and its specific surface area is 300m 2 / g, pore volume 0.7mL / g. 20ml of H 2 PdCl 4 solution (wherein the Pd content is 0.01g / ml), 30ml of KHSO 3 Solution (wherein the S content is 0.008g / ml) and the chloride salt of 20g 1-butyl-3-methylimidazole are mixed, and add appropriate amount of deionized water to make it to 70ml; At 50 ℃, under the action of ultrasonic The mixture was added dropwise to 100g columnar SiO 2 , and impregnated under vacuum conditions and ultrasonic waves for 7 hours; then vacuum-dried at 100°C for 8 hours to obtain the supported ionic liquid-promoted [PdSCl x ] x- Composite catalyst, wherein the Pd loading (relative carrier mass) is 0.2wt%, the S element loading (relative carrier mass) is 0.24wt%, and the ionic liquid loading (relative carrier mass) is 20wt%.

[0054] Take 2g of this catalyst and apply it to the hydrochlorination of acetylene in a fixed bed reactor. The reactio...

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Abstract

The invention discloses a supported type ionic liquid promoted [PdSCl<x>]<x> compound catalyst. The supported type ionic liquid promoted [PdSCl<x>]<x> compound catalyst is composed of a porous solid carrier, and ionic liquid and a [PdSCl<x>]<x> compound which are loaded onto the surface of the porous solid carrier, wherein x=1, 2, or 3, the [PdSCl<x>]<x> ionic compound is formed via taking Pd as the core via bonding of S and Cl with Pd through ionic bonds; the anion of the ionic liquid is chloride ion, and the cation is one or a plurality of ions selected from iminazole, quaternary ammonium, quaternary phosphonium, or pyrrolidine ionic liquid. The ionic liquid load capacity is controlled to be 2.5 to 25wt% based on the mass of the carrier, the load capacity of Pd is controlled to be 0.05 to 1wt%, the load capacity of S is controlled to be 0.1 to 5wt%. The supported type ionic liquid promoted [PdSCl<x>]<x> compound catalyst possesses relatively high ethyne hydrochlorination reaction activity, and excellent stability; after operation of 2000h, no obvious palladium loss is detected, the highest conversion rate of ethyne is 100%, and the highest vinyl chloride selectivity is 100%.

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, the preparation of vinyl chloride by calcium carbide acetylene method is still the mainstream process of polyvinyl chloride production in my country. In industry, the catalyst currently used for synthesizing vinyl chloride is mercuric chloride, because it causes serious pollution to the environment, and the synthesized polyvinyl chloride contains a small amount of mercury, which affects the application of polyvinyl chloride. 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 best catalytic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28C07C17/08C07C21/06
CPCB01J31/0292B01J31/28B01J2231/32C07C17/08C07C21/06
Inventor 李小年赵佳丰枫岳玉学张群峰许孝良
Owner ZHEJIANG UNIV OF TECH
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