A porous zirconium boride material, its preparation method and its application in the preparation of vinyl chloride by acetylene hydrochlorination

A technology of zirconium boride and boronizing agent, which is applied in the field of porous catalyst materials and can solve problems such as high price, poor mechanical strength of activated carbon, and environmental pollution

Active Publication Date: 2021-05-18
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] For the above-mentioned acetylene hydrochloride metal catalysts, wherein noble metal catalysts are due to cost problems, their higher price limits the further promotion and application of this type of catalysts; non-noble metal catalysts, such as copper catalysts, are due to the development and application process for catalysts. It is still immature, and is currently undergoing small-scale promotion experiments and further exploration
In addition, due to the poor mechanical strength of activated carbon, the supported carbon-supported catalyst will cause the collapse and sintering of the catalyst pores during the long-term use of the catalyst, resulting in the loss of the catalyst and serious pollution to the environment.

Method used

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  • A porous zirconium boride material, its preparation method and its application in the preparation of vinyl chloride by acetylene hydrochlorination
  • A porous zirconium boride material, its preparation method and its application in the preparation of vinyl chloride by acetylene hydrochlorination
  • A porous zirconium boride material, its preparation method and its application in the preparation of vinyl chloride by acetylene hydrochlorination

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preparation example Construction

[0034] The present invention provides two methods for preparing porous zirconium boride materials described in the above schemes. The first method includes the following steps:

[0035] (1) After mixing the zirconium-containing precursor, boronating agent and solvent A, microwave digestion is carried out to obtain the mixed material;

[0036] (2) leave the mixed material to obtain a gel-like substance;

[0037] (3) drying the gel-like substance, and subjecting the dried material to boronation treatment under X-ray irradiation conditions to obtain a porous zirconium boride material.

[0038] In the invention, the zirconium-containing precursor, the boronating agent and the solvent A are mixed and then subjected to microwave digestion treatment to obtain the mixed material. In the present invention, the zirconium-containing precursor preferably includes zirconium oxide, zirconium chloride, zirconium nitrate, zirconium phosphate, zirconium sulfate, zirconium hydroxide, zirconiu...

Embodiment 1

[0058] (1) Weigh 12.32g of zirconia and 13.92g of boron oxide, add 15mL of ethanol, and use a microwave digestion apparatus to process at a frequency of 300GHz for 0.1h to obtain a mixed material;

[0059] (2) Put the above mixed material at 60°C for 1 hour to make it into a gel-like substance;

[0060] (3) drying the above-mentioned gelatinous substance at 110° C. and 10,000 Pa for 2 hours to obtain a dried material;

[0061] (4) The dry material is irradiated with X-rays under a nitrogen atmosphere, and the frequency of the radiation is 30EHz, so that the internal temperature of the dry material reaches 1100 ° C, and the boronization treatment is carried out for 3 hours;

[0062] (5) The material after the above-mentioned boride treatment is cooled to room temperature, and washed three times with deionized water;

[0063] (6) Dry the zirconium boride material after the above-mentioned washing treatment for later use. The SEM image of the obtained zirconium boride material ...

Embodiment 2

[0067] (1) Weigh 23.3g of zirconium chloride and 8.3g of boron carbide, add 12mL of deionized water, and use a microwave digestion apparatus to process at a frequency of 300MHz for 1.5h to obtain a mixed material;

[0068] (2) Put the above mixed material at 90°C for 1.5h to make it into a gel-like substance;

[0069] (3) drying the above-mentioned gelatinous substance at 80° C. and 1000 Pa for 12 hours to obtain a dried material;

[0070] (4) The dry material is irradiated with X-rays under a nitrogen atmosphere, and the frequency of the radiation is 30PHz, so that the internal temperature of the dry material reaches 1300°C, and the boronization treatment is performed for 2.5 hours;

[0071] (5) The material after the boride treatment is cooled to room temperature, and washed three times with ethanol;

[0072] (6) The porous zirconium boride material after the above washing treatment is dried for subsequent use; the SEM image of the porous zirconium boride material obtained ...

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Abstract

The invention relates to the technical field of porous catalyst materials, and provides a porous zirconium boride material and its preparation method and application. The porous zirconium boride material of the present invention has relatively high specific surface area, rich pore structure (including micropores and mesopores), disordered microscopic surface and dispersed defect sites. The porous zirconium boride material provided by the invention has excellent activity and can be directly used as a catalyst. The preparation method provided by the invention is rich in synthetic raw material resources, cheap in price, green and simple in the preparation process, low in production cost, and less harmful to the environment; It is possible to controllably adjust the physical and chemical properties of materials. The porous zirconium boride material provided by the invention has good catalytic activity for acetylene hydrochlorination reaction in a wide space velocity range.

Description

technical field [0001] The invention relates to the technical field of porous catalyst materials, in particular to a porous zirconium boride material and its preparation method and its application in the preparation of vinyl chloride by acetylene hydrochlorination. Background technique [0002] Polyvinyl chloride (PVC) is the third largest general-purpose plastic, and is generally obtained by polymerization of its monomer vinyl chloride. Due to the energy occurrence characteristics of rich coal, poor oil and little gas in my country, the preparation of vinyl chloride by coal-based calcium carbide method (acetylene hydrochlorination method) is the mainstream process of polyvinyl chloride production in my country. The catalyst used in the existing synthesis of vinyl chloride is mercuric chloride or other mercury-free metal chlorides. Because mercuric chloride will cause serious pollution to the environment, and the polyvinyl chloride synthesized by it contains a small amount ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/04B01J21/06B01J21/18B01J35/10C07C17/08C07C21/06
CPCB01J21/066B01J21/18B01J35/1019B01J35/1023B01J35/1028C01B35/04C01P2004/03C01P2006/12C07C17/08C07C21/06
Inventor 赵佳陆金跃岳玉学李小年王柏林郭伶伶卢春山王赛赛陈志邵淑娟金春晓
Owner ZHEJIANG UNIV OF TECH
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