A kind of synthetic method of vinyl chloride

A synthesis method, vinyl chloride technology, applied in chemical instruments and methods, hydrogen halide addition preparation, organic compound/hydride/coordination complex catalyst, etc., can solve the problem of cationic metal catalyst deactivation, etc., to reduce poisoning and deactivation, good effect, high mechanical strength

Active Publication Date: 2021-12-21
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, in the surface functional groups of activated carbon after acid treatment, the content of carboxyl groups accounts for more than 80% of the total surface functional groups, and the strong reducibility of carboxyl functional groups on the surface of activated carbon will instead reduce metal cations to zero-valent metals, resulting in the deactivation of cationic metal catalysts. (See literature Applied Catalysis B: Environmental, 2013, 142-143, 234-240; Catalysis Letters. 2008, 124, 165-167; Journal of Catalysis. 2013, 297, 128-136)

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  • A kind of synthetic method of vinyl chloride
  • A kind of synthetic method of vinyl chloride
  • A kind of synthetic method of vinyl chloride

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preparation example Construction

[0061] In the present invention, the preparation method of the carrier activated carbon fiber preferably comprises the following steps:

[0062] After the carbonaceous precursor and the activator are mixed, carbonization treatment is carried out to obtain activated carbon fibers.

[0063] In the present invention, the carbonaceous precursor preferably includes one or more of viscose-based fibers, polyacrylonitrile-based fibers, pitch-based fibers, phenolic-based fibers and palm fibers, when the carbonaceous precursor When multiple substances are preferred, the mass of each substance is preferably equal. In the present invention, the activator preferably includes ammonia water, phosphoric acid, diammonium hydrogen phosphate, ammonium chloride, ammonium phosphate, sodium thiosulfate, 1-(3-dimethylaminopropyl)-3-ethylcarbodi One or more of imine hydrochloride, N-hydroxysuccinimide and ethanol. When the activator is preferably multiple of the above substances, the mass of each su...

Embodiment 1

[0080] The viscose-based fibers were immersed in ammonia water with a concentration of 20wt% for 10 hours. The amount ratio of the ammonia water and viscose-based fibers was 40mL:100g. After vacuum drying, they were placed in a tube furnace. Heating at a heating rate of 5°C / min to the set temperature of 800°C, and keeping at this temperature for 3 hours for carbonization, cooling to room temperature naturally, cleaning with deionized water under ultrasonic vibration until the pH of the solution is 7, and cleaning the sample Put it into a vacuum oven for drying to obtain activated carbon fibers.

[0081] Activated carbon fiber is used as the carrier, the surface oxygen-containing groups (hydroxyl content 430μmol / g, carboxyl content 20μmol / g), ash content 1.0wt%, specific surface area 1300m 2 / g, pore volume 0.6mL / g. 4 mL of HAuCl 4 solution (where the Au content is 0.025g / mL), 6mL of CaCl 2 The solution (wherein the Ca content is 0.25g / mL) and 50mL deionized water are mixed ...

Embodiment 2

[0084] The polyacrylonitrile-based fibers are immersed in phosphoric acid with a concentration of 65wt% for 3 hours. The dosage ratio of the phosphoric acid and polyacrylonitrile-based fibers is 100mL:100g. , heated to a set temperature of 1000°C at a heating rate of 12°C / min, and kept at this temperature for 3.5 hours for carbonization, cooled naturally to room temperature, cleaned with deionized water under ultrasonic vibration until the pH of the solution = 7, and cleaned The processed samples were dried in a vacuum oven to obtain activated carbon fibers.

[0085] Activated carbon fiber is used as the carrier, the surface oxygen-containing groups (hydroxyl content 430μmol / g, carboxyl content 20μmol / g), ash content 1.0wt%, specific surface area 1300m 2 / g, pore volume 0.6mL / g. 4mL of RuCl 3 solution (in which the Ru content is 0.10g / mL), 1g of 1-butyl-3-methylimidazolium chloride salt and 54mL of ethanol are mixed to obtain an impregnation solution, and the impregnation so...

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Abstract

The invention provides a catalyst for synthesizing vinyl chloride, a preparation method thereof and a synthesis method of vinyl chloride, belonging to the field of organic synthesis. The catalyst provided by the invention includes an active center, an auxiliary agent and a carrier; the active center is one or more of a gold compound, a ruthenium compound, a palladium compound and a copper compound; the carrier is activated carbon fiber; the auxiliary agent includes Metallic and / or non-metallic additives. The catalyst provided by the invention has higher catalytic activity and stability. The results of the examples show that the catalyst provided by the present invention has a better effect. At the initial stage of the reaction, the conversion rate of acetylene is 63.35% to 99.97%, and the selectivity of vinyl chloride is 100%. After 6000 hours of reaction, the conversion rate of acetylene is 62.56% to 99.85%. The vinyl chloride selectivity is 99.9%.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a catalyst for synthesizing vinyl chloride, a preparation method thereof and a synthesis method of vinyl chloride. Background technique [0002] At present, the main method of producing vinyl chloride is acetylene hydrochlorination, and in the foreseeable next few decades, acetylene hydrochlorination will still be the main production process of vinyl chloride. At present, the industrial catalyst for the synthesis of vinyl chloride by the acetylene method is the activated carbon carrier loaded with HgCl pretreated by strong acid. 2 (See literature Science. 2017, 355, 1399-1403; Journal of the American Chemical Society. 2015, 137, 14548-14557; Journal of Catalysis. 2013, 297, 128-136). In the synthesis of vinyl chloride by acetylene hydrochlorination, acetylene, as a strong reducing agent, will deactivate active metal cations by reducing them to zero-valent metals, but the surface...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28B01J23/644B01J23/66B01J35/10C07C17/08C07C21/06
CPCB01J31/28B01J23/6447B01J23/66B01J35/1028C07C17/08C07C21/06
Inventor 李小年赵佳张群峰丰枫赖慧霞
Owner ZHEJIANG UNIV OF TECH
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