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Ruthenium complex catalyst for acetylene hydrochlorination reaction

A ruthenium complex and catalyst technology, applied in the field of ruthenium complex catalysts, can solve the problems of low activity of supported non-precious metal catalysts, poor stability of supported noble metal catalysts, easy sublimation and deactivation of mercury catalysts, etc., and achieve long running time and difficult sublimation , the effect of convenient operation

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

[0005] The purpose of the present invention is to: overcome the problems of easy sublimation and deactivation of mercury catalysts and serious environmental pollution, low activity of supported non-precious metal catalysts, poor stability and high cost of supported noble metal catalysts in the gas-solid reaction of acetylene hydrochlorination synthesis of vinyl chloride The problem is to provide a supported ruthenium complex catalyst and its application in the synthesis of vinyl chloride by acetylene hydrochlorination. The catalyst is cheap, has high acetylene conversion rate and vinyl chloride selectivity, and good stability

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Ruthenium complex (ImH) 2 [RuImCl 5 ], the synthesis of amine and imine ruthenium complexes is used as an example to further illustrate the present invention. It should be pointed out that the synthesis of such ruthenium complexes proposed in this patent is only for clearer , clearly explain the present invention, but cannot be construed as limiting the protection scope of the present invention, and the present invention is not limited thereto in any way.

[0044] (ImH) 2 [RuImCl 5 ] Synthesis: 4.4 g RuCl 3 Dissolve in a mixed solvent of 100mL ethanol and 100mL water, and reflux for 2h. Concentrate to 50 mL, add dropwise to 20 mL of 6M HCl aqueous solution containing 10 g of imidazole, stir the clear dark red solution for 3 minutes, concentrate to 40 mL, add 1.8 mL of 8M HCl, and heat to 85°C. After cooling to room temperature, red crystals were obtained after about 30 minutes, washed with ethanol, and dried in vacuum.

[0045] Select columnar activated carbon as ...

Embodiment 2

[0048] (ImH) 2 [RuImCl 5 ] Synthesis: 4.4 g RuCl 3 Dissolve in a mixed solvent of 100mL ethanol and 100mL water, and reflux for 2h. Concentrate to 50 mL, add dropwise to 20 mL of 6M HCl aqueous solution containing 10 g of imidazole, stir the clear dark red solution for 3 minutes, concentrate to 40 mL, add 1.8 mL of 8M HCl, and heat to 85°C. After cooling to room temperature, red crystals were obtained after about 30 minutes, washed with ethanol, and dried in vacuum.

[0049] 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, with a pore volume of 0.6ml / g, and treated with 300mL of 10wt% hydrochloric acid at 25°C for 3h. Dry at 110°C for 12 hours and set aside. 20mL of (ImH) 2 [RuImCl 5 ] solution (wherein the Ru content is 0.1g / mL) and BaCl 2 After mixing 30 mL of the solution (wherein the Ba content is 0.1 g / mL), after mixing, 15 g of phosphine-containing ionic liquid (t...

Embodiment 3

[0052] (ImH) 2 [RuImCl 5 ] Synthesis: 4.4 g RuCl 3 Dissolve in a mixed solvent of 100mL ethanol and 100mL water, and reflux for 2h. Concentrate to 50 mL, add dropwise to 20 mL of 6M HCl aqueous solution containing 10 g of imidazole, stir the clear dark red solution for 3 minutes, concentrate to 40 mL, add 1.8 mL of 8M HCl, and heat to 85°C. After cooling to room temperature, red crystals were obtained after about 30 minutes, washed with ethanol, and dried in vacuum.

[0053] 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, with a pore volume of 0.6ml / g, and treated with 300mL of 10wt% hydrochloric acid at 25°C for 3h. Dry at 200°C for 0.5h and set aside. 20mL of (ImH) 2 [RuImCl 5 ] solution (wherein the Ru content is 0.0005g / mL) and CaCl 2 After mixing 10 mL of the solution (in which the Ca content is 0.001 g / mL) and mixing, add 1 g of phosphine-containing ionic liquid ...

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Abstract

The invention discloses a supported ruthenium complex catalyst. The supported ruthenium complex catalyst comprises a porous solid carrier, and a ruthenium complex, a metal assistant and a nonmetal assistant which are supported on the surface of the carrier, and the ruthenium complex is one or more of a polypyridine ruthenium complex, a ruthenium porphyrin ruthenium complex, an aromatic hydrocarbonruthenium complex, a cyclic metal ruthenium complex, a DMSO ruthenium complex, an amine ruthenium complex and an imine ruthenium complex; the metal assistant is salt of one or more of In, Bi, Ba, Sr,Fe, Mn, Zn, Cs, Ca and Sn; the nonmetal assistant is an ionic liquid; and a ratio of the mass of the porous solid carrier to the theoretic mass of ruthenium in the ruthenium complex to the mass of the metal in the metal assistant to the mass of the nonmetal assistant is 100:(0.01-2):(0.01-3):(1-30). The catalyst has a very high stability in an acetylene hydrochlorination reaction, no obvious lossof the ruthenium is detected after the catalyst runs for 8000 h, the highest acetylene conversion rate reaches 99.95% or more, and the highest vinyl chloride selectivity reaches 99.95% or more.

Description

(1) Technical field [0001] The invention belongs to the technical field of catalysts, in particular to a ruthenium complex catalyst used for acetylene hydrochlorination. (2) Background technology [0002] Polyvinyl chloride is a very versatile plastic that is polymerized from vinyl chloride. The industrial synthesis of vinyl chloride in my country mainly uses acetylene and hydrogen chloride as raw materials and mercuric chloride as a catalyst. However, with the increase of mercury usage, my country's mercury resources are gradually depleted; in addition, mercury chloride is easy to sublimate and cause catalyst deactivation, and highly toxic mercury chloride will cause serious environmental pollution and endanger human health. Therefore, the development of non-mercury catalysts that can replace mercury is very necessary for the sustainable development of the PVC industry. [0003] In recent years, there have been many public reports on the hydrochlorination of acetylene cat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J31/26B01J31/38C07C17/08C07C21/06
CPCB01J31/0292B01J31/1691B01J31/1815B01J31/26B01J31/38B01J2231/32B01J2531/821C07C17/08C07C21/06
Inventor 李小年赵佳张群峰丰枫杨倩邓雅琴赖慧霞余祎
Owner ZHEJIANG UNIV OF TECH
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