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Preparation method of 2-chloro-1, 1-difluoroethane

A technology of difluoroethane and fluorination, which is applied in the field of preparation of 2-chloro-1,1-difluoroethane, can solve the problems of long synthesis route, complex process, harsh reaction conditions, etc. Simple, high reaction yield effect

Pending Publication Date: 2022-08-05
SHANDONG HUAAN NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The object of the present invention is to provide a synthetic route with simple process and high product yield in view of the problems of long synthetic route, complex process and harsh reaction conditions in the preparation method of 2-chloro-1,1-difluoroethane in the prior art. A new method for the preparation of 2-chloro-1,1-difluoroethane with high yield and high purity and continuous industrial production

Method used

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  • Preparation method of 2-chloro-1, 1-difluoroethane

Examples

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Embodiment 1

[0038] (1) Preparation of isomerization catalyst: weigh 300 g of activated alumina, fill it into a SUS-316 reaction tube with an inner diameter of 30 mm and a length of 100 mm, and set it in a tubular electric furnace. The temperature was raised to 400°C at 2-5°C / min, and kept at 400°C for 10-20 h for dehydration. Then 20L / h of nitrogen / HF mixed gas of 5 / 1 (volume / volume) was passed through, and the alumina catalyst was fluorinated and circulated for 24 hours, and the bed temperature was controlled to ±5°C. If the bed temperature changed greatly, The nitrogen ratio can be increased until it is all nitrogen. When the bed is stable, gradually reduce the nitrogen ratio until all the gas is HF, and keep it for 100h. Heating was stopped, HF was turned off, nitrogen was started, and the nitrogen flow was about 10 L / h, and the catalyst was naturally cooled to room temperature to complete the catalyst preparation.

[0039] (2) Preparation of crude 2-chloro-1,1-difluoroethane: 65g (6...

Embodiment 2

[0042] On the basis of Example 1, the reaction temperature of step (2) was changed to 250°C, N 2 : R142b=10:1 (mol), the space velocity is 330 / h, after half an hour of reaction, samples were taken at the outlet of the reactor to detect the content of each component. The reaction results are shown in Table 1.

Embodiment 3

[0044] On the basis of Example 1, the reaction temperature was changed to 200°C, N 2 : R142b=5:1 (mol), the space velocity is 330 / h, and the content of each component is detected by sampling at the reactor outlet after half an hour of reaction. The reaction results are shown in Table 1.

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Abstract

The invention discloses a preparation method of 2-chloro-1, 1-difluoroethane, and belongs to the technical field of organic fluorine chemical industry. The preparation method of the 2-chloro-1, 1-difluoroethane comprises the following steps: firstly preparing an isomerization catalyst, isomerizing 1, 1-difluoro-1-chloroethane by using the catalyst to prepare the 2-chloro-1, 1-difluoroethane, then separating to obtain a finished product of the 2-chloro-1, 1-difluoroethane, recovering the unreacted 1, 1-difluoro-1-chloroethane to serve as a raw material, and continuing to react. The preparation method of 2-chloro-1, 1-difluoroethane has the advantages of abundant raw material sources, high reaction yield, simple process, realization of industrial continuous production, easy product separation and the like, reduces the production cost, and is safe and environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of organic fluorine chemicals, in particular to a preparation method of 2-chloro-1,1-difluoroethane. Background technique [0002] 2-Chloro-1,1-difluoroethane (2-chloro-1,1-difluoroethane, referred to as HCFC-142) is a colorless transparent liquid, the molecular formula is C 2 H 3 ClF 2 , molecular weight: 100.5, CAS number: 338-65-8, boiling point: 36°C, melting point: -82.13°C, density: 1.312 g / mL (15°C), refractive index: 1.3528 (15°C). Critical temperature: 204.76 ℃, critical pressure: 4.277 MPa. It is an important aliphatic fluorine-containing intermediate, an intermediate product for the preparation of 2,2-difluoroethanol, etc., and can also be used in the field of aerosols and foaming agents for cleaning, drying and degreasing solid surfaces. , medicine, refrigerant and other aspects also have a wide range of uses. [0003] At present, the synthesis methods of 2-chloro-1,1-difluoroethane in the p...

Claims

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Application Information

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IPC IPC(8): C07C17/358C07C19/12B01J27/125
CPCC07C17/358B01J27/125C07C19/12Y02P20/584
Inventor 王瑞英李丕永邹冉王永千张丽平
Owner SHANDONG HUAAN NEW MATERIAL
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