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Hydrogen chloride resistant basic catalyst, preparation method and application

A catalyst and alkaline technology, which is applied in the field of hydrogen chloride-resistant alkaline catalyst and its preparation and application, and can solve the problems that gas-phase dehydrochlorination catalysts cannot meet the requirements of industrial production, low selectivity of vinylidene chloride, and short service life of catalysts, etc. , to achieve excellent resistance to hydrogen chloride, broad industrialization prospects, and high conversion rate

Inactive Publication Date: 2018-11-20
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] ① The activity of the catalyst is poor, and the conversion rate of most trichloroethanes is lower than 50%;
[0009] ②The selectivity of vinylidene chloride is low;
[0010] ③ The service life of the catalyst is short;
[0011] Existing gas-phase dehydrochlorination catalysts cannot meet the requirements of industrial production

Method used

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  • Hydrogen chloride resistant basic catalyst, preparation method and application
  • Hydrogen chloride resistant basic catalyst, preparation method and application
  • Hydrogen chloride resistant basic catalyst, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Dissolve the chloromethyltriphenylphosphorous chloride in absolute ethanol, the chloromethyltriphenylphosphorous chloride accounts for 1% of the mass of ethanol, and stir evenly with a stirring device.

[0046] (2) Use 0.1mol / L nitric acid to dissolve γ-Al 2 o 3 After soaking for 12 hours, soak the soaked γ-Al with deionized water 2 o 3 Wash to neutral. Washed γ-Al 2 o 3 Put it in a blast oven, dry at 200°C for 5 hours, and dry the γ-Al 2 o 3 Put it into a muffle furnace and bake at 800°C for 2 hours. The baked carrier is taken out for later use.

[0047] (3) The γ-Al obtained in (2) 2 o 3 Added to the solution of (1), γ-Al 2 o 3 Accounting for 10% of the mass of the solution, use a stirring device to stir evenly. Chloromethyltriphenylphosphonium chloride in γ-Al 2 o 3 The loading of the surface is 40%.

[0048] (4) Put the treated mixture in (3) in an ultrasonic cleaner for 4 hours. It was left to stand in an environment of 10° C. for 6 hours.

[...

Embodiment 2

[0052] (1) Dissolve tetraphenylphosphorus chloride in absolute ethanol, wherein tetraphenylphosphorus chloride accounts for 1% of the mass of absolute ethanol, and stir evenly with a stirring device.

[0053] (2) Use 4mol / L nitric acid to soak the activated carbon for 0.5 hour, and wash the soaked activated carbon to neutral with deionized water. The washed activated carbon was dried in a blast oven at 80°C for 10 hours, and the dried activated carbon was roasted in a tube furnace at 400°C under a nitrogen atmosphere for 12 hours, and the roasted carrier was taken out for use.

[0054] (3) Add the activated carbon obtained in (2) into the solution of (1), the activated carbon accounts for 25% of the solution mass, and use a stirring device to stir well. The loading of tetraphenylphosphine chloride on the surface of activated carbon is 4%.

[0055] (4) Put the treated mixture in (3) in an ultrasonic cleaning machine for 0.5 hours. It was left to stand in an environment of 40°...

Embodiment 3

[0059] (1) Dissolve trityltriphenylphosphorus chloride in absolute ethanol, wherein trityltriphenylphosphorus chloride accounts for 10% of the mass of absolute ethanol, and stir evenly with a stirring device.

[0060] (2) Use 4mol / L nitric acid to dissolve SiO 2 After soaking for 0.5 hours, the pickled SiO 2 Wash to neutral. Wash the SiO in a blast oven at 80°C 2 After drying for 5 hours, the dried SiO 2 Roast for 5 hours. The catalyst carrier that has been calcined is taken out for use.

[0061] (3) SiO obtained in (2) 2 Added to the solution of (1), SiO 2 Accounting for 60% of the solution mass, use a stirring device to stir evenly. Trityltriphenylphosphonium chloride on SiO 2 The load on it is 40%.

[0062] (4) Put the treated mixture in (3) in an ultrasonic cleaner for 4 hours. Post-processing is the same as (4) in embodiment 3.

[0063] (5) Dry the treated mixture in (4) for 24 hours in a blast oven at 80°C.

[0064] (6) The obtained catalyst is stored for fut...

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PUM

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Abstract

The invention discloses a hydrogen chloride resistant basic catalyst, a preparation method and application. The basic catalyst comprises a carrier and an active component loaded on the carrier, wherein the carrier is selected from one in SiO2, gamma-Al2O3, SBA-15, active carbon, ZSM-5, MCM-22 and silica aerogel; the active component is selected from one or a combination of more in ionic liquid taking chloride ion as anion; the loading amount of the ionic liquid is 0.1 to 40 percent. The invention provides application of the basic catalyst to reaction in which vinylidene chloride is prepared from 1. 1.2-methyl chloroform gas phase dehydrochlorination. The basic catalyst has the advantages of long service life and high activity.

Description

(1) Technical field [0001] The invention relates to a basic catalyst with anti-hydrogen chloride properties, its preparation method and its application in the reaction of 1.1.2-trichloroethane gas-phase dehydrochlorination to prepare vinylidene chloride. (2) Background technology [0002] Basic catalysts are often used in the catalytic reaction process of dehalogenation of halogenated alkanes to unsaturated hydrocarbons, but the released hydrogen halide is a strongly acidic substance, which is easy to form a strong reaction with the basic active center on the surface of the catalyst. Interaction, poisoning the alkaline active center of the catalyst. During the design of basic catalysts, the resistance to poisoning by hydrogen halide species must be considered. [0003] Vinylidene chloride is a polymerized monomer used to produce polyvinylidene chloride (PVDC), which can produce polyvinylidene chloride and various polymers. Compared with other polymers, polyvinylidene chlor...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J37/02C07C21/08C07C17/25
CPCB01J31/0298B01J37/0207C07C17/25C07C21/08Y02P20/54
Inventor 李小年张朋泽蒋肇彬张群峰丰枫
Owner ZHEJIANG UNIV OF TECH
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