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Preparation method of 1, 1, 1, 3-tetrachloropropane

A technology of tetrachloropropane and carbon tetrachloride, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, catalyst activation/preparation, etc., can solve problems such as easy oxidation, easy agglomeration of iron powder, and increase of iron specific surface area , to achieve the effect of increasing the contact area, good catalytic effect and large specific surface area

Pending Publication Date: 2022-08-02
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] According to one aspect of the present application, a preparation method of 1,1,1,3-tetrachloropropane is provided. The preparation method uses a supported iron main catalyst, which can significantly improve the problem that commercially available iron powder is easy to agglomerate, and at the same time increase The specific surface area of ​​iron is increased, and the second nano-metal component is added at the same time, which effectively solves the problem that the freshly prepared nano-iron catalyst is easily oxidized when exposed to air, and is conducive to the reaction.

Method used

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  • Preparation method of 1, 1, 1, 3-tetrachloropropane

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preparation example Construction

[0067] In another preferred embodiment, the preparation method of the catalyst comprises the steps:

[0068] (i) Using a metal salt (FeSO4) with a carrier (organic bentonite) 4 ·7H 2 O) ethanol-aqueous solution with reducing agent (NaBH) 4 ) solution to carry out reduction reaction, thereby obtaining the nano-zero valent iron supported by organobentonite; continue to add the second metal component (PdCl 2 ); continue the reduction reaction; the Pd content in the obtained catalyst is: 0.04%. Suction filtration, vacuum drying oven drying. During the whole reaction process, nitrogen gas was continuously introduced to isolate the air.

[0069] In another preferred embodiment, the metal salt is FeCl 2 ·4H 2 O.

[0070] In another preferred embodiment, the carrier is modified activated carbon.

[0071] In another preferred embodiment, the reducing agent is KBH 4 .

[0072] In another preferred embodiment, the second metal component is K 2 PdCl 6 .

[0073] In another pr...

Embodiment 1

[0104] The preparation of embodiment 1 catalyst

[0105] Add 5g of organic bentonite to 250mL, 0.054mol / L FeSO 4 ·7H 2 O solution, stir for 6h; adjust PH4 The aqueous solution was dropped into the above solution, stirred for 2 hours, and the whole process was vented with nitrogen to isolate the air to prevent the nano-zero valent iron from being oxidized by oxygen in the air. Filter, wash with deionized water and alcohol. Dry in a vacuum oven.

Embodiment 2

[0106] The preparation of embodiment 2 catalyst

[0107] Add 5g of organic bentonite to 250mL, 0.054mol / L FeCl 2 ·4H 2 O solution, stir for 6h; adjust PH4 The aqueous solution was dropped into the above solution, stirred for 2 hours, and the whole process was vented with nitrogen to isolate the air to prevent the nano-zero valent iron from being oxidized by oxygen in the air. Filter, wash with deionized water and alcohol. Dry in a vacuum oven.

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Abstract

The invention discloses a preparation method of 1, 1, 1, 3-tetrachloropropane, which comprises the following steps: in the presence of a first catalyst and a second catalyst, reacting raw materials containing carbon tetrachloride and ethylene to obtain the 1, 1, 1, 3-tetrachloropropane, the first catalyst comprises a carrier and an active component loaded on the carrier; the active component comprises nano zero-valent iron; the second catalyst comprises an ester compound. According to the preparation method, the supported iron catalyst is adopted, so that the problem of easy agglomeration when pure commercially available iron powder is used as the catalyst can be remarkably improved, the specific surface area of iron is increased, and the reaction is facilitated.

Description

technical field [0001] The application relates to a preparation method of 1,1,1,3-tetrachloropropane, which belongs to the technical field of chemical industry. Background technique [0002] Carbon tetrachloride is a by-product of a methane chloride plant. Carbon tetrachloride is a controlled substance that depletes the ozone layer under the Montreal Protocol, abbreviated as CTC. Completely stop the production and consumption of CTC except for raw material use, reagent use and special exempted use. In recent years, China's methane chloride has developed rapidly. Depending on the raw material market, it is difficult to digest and produce CTC. The cost of incinerating carbon tetrachloride is about 3,000 to 4,000 yuan per ton. Therefore, the comprehensive utilization of CTC has very important practical significance, which is related to the survival and safety of the entire industry chain. [0003] The metals and cocatalysts reported in literature reports mainly include: organ...

Claims

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Application Information

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IPC IPC(8): C07C17/275C07C19/01B01J31/02B01J23/745B01J23/89B01J37/16B01J37/02
CPCC07C17/275B01J23/745B01J23/8906B01J37/16B01J37/0201B01J31/0258B01J31/0259B01J2231/341B01J35/23B01J35/61C07C19/01
Inventor 张业新邓艳艳张建陈慧
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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