Method for preparing difluorochloroacetate and difluorochloroacetic acid through continuous non-catalytic reaction

A technology of difluorochloroacetic acid ester and difluorochloroacetic acid, which is applied in the field of preparation of difluorochloroacetic acid ester and difluorochloroacetic acid, can solve problems that are not conducive to continuous large-scale production, achieve easy separation and purification, and reduce three wastes The production amount and the effect of high yield

Active Publication Date: 2018-12-18
ZHEJIANG RES INST OF CHEM IND CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method adopts a batch process, which is not conducive to the realization of continuous large-scale production

Method used

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  • Method for preparing difluorochloroacetate and difluorochloroacetic acid through continuous non-catalytic reaction
  • Method for preparing difluorochloroacetate and difluorochloroacetic acid through continuous non-catalytic reaction
  • Method for preparing difluorochloroacetate and difluorochloroacetic acid through continuous non-catalytic reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Such as figure 1 As shown, the jacketed spray towers A and B of 200L enamel materials connected in series are used in two stages, the spray towers A and B are filled with 125L ceramic packing respectively, and the liquid storage areas (100L) of the spray towers A and B are each introduced with 720mol (33170g, 42L) ethanol, wherein spray tower A is a primary spray tower, and spray tower B is a secondary spray tower. Add raw material CClF in spray tower A with the speed of 1.5mol / min (254g / min) 2 COCl stream 1, 90mol (15246g) CClF was added in 1h 2 COCl, add stream 2 ethanol to the spray tower A in a spray manner at an initial speed of 2 mol / min (92 g / min). In the spray tower A, the temperature inside the tower is controlled at about 20°C, and the pressure inside the tower is controlled at about normal pressure, so that the CCIF 2 Reverse contact reaction of COCl and ethanol in the packing area, CClF 2 The residence time of COCl in the packing area is about 3.7min. I...

Embodiment 2

[0048] On the basis of completion of Example 1, the spray tower B that completed the reaction in Example 1 is switched to a primary spray tower, and the spray tower A is switched to a secondary spray tower, and the reaction is continued, such as figure 2 shown.

[0049] Add the raw material CClF to the spray tower B at a speed of 1.5mol / min (254g / min) 2 COCl flow 7, a total of 90mol (15246g) CClF was added in 1h 2 COCl, add stream 8 ethanol to the spray tower B at an initial speed of 2 mol / min (92 g / min) in a spray manner. In the spray tower B, the temperature inside the tower is controlled at about 20°C, and the pressure inside the tower is controlled at about normal pressure, so that the CCIF 2 Reverse contact reaction of COCl and ethanol in the packing area, CClF 2 The residence time of COCl in the packing area is about 3.7min. In the spray tower B, the tower top obtains and contains unreacted CClF 2 The stream 9 of COCl, the stream 9 enters the spray tower A, and the...

Embodiment 3

[0052] On the basis that embodiment 1 and 2 are finished, the spray tower A that finishes reaction among the embodiment 2 is switched to one-stage spray tower, and spray tower B is switched to two-stage spray tower, continues to react, as figure 1 shown.

[0053] Add raw material CClF in spray tower A with the speed of 1.5mol / min (254g / min) 2 COCl stream 1, 90mol (15246g) CClF was added in 1h 2 COCl, add stream 2 ethanol to the spray tower A in a spray manner at an initial speed of 2 mol / min (92 g / min). In the spray tower A, the temperature inside the tower is controlled at about 20°C, and the pressure inside the tower is controlled at about normal pressure, so that the CCIF 2 Reverse contact reaction of COCl and ethanol in the packing area, CClF 2 The residence time of COCl in the packing area is about 3.7min. In the spray tower A, the tower top obtains and contains unreacted CClF 2 Stream 3 of COCl, stream 3 enters spray tower B, and stream 5 ethanol is added to spray t...

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Abstract

The invention provides a method for preparing difluorochloroacetate and difluorochloroacetic acid through a two-stage tandem continuous non-catalytic reaction, wherein a two-stage spraying tower tandem process is used during single-pass operation, and after the single-pass operation is completed, a first-stage absorption tower and a second-stage absorption tower are switched so as to continuouslycarry out a reaction. According to the present invention, the method has advantages of low alcohol or water content in the reaction product, easy separation and purification of the product, continuousreaction, high reaction efficiency, high yield, no requirement of catalysts and acid binding agents, less three-waste, and the like.

Description

technical field [0001] The invention relates to a method for preparing difluorochloroacetic acid ester and difluorochloroacetic acid. Background technique [0002] Alkyl difluorochloroacetate, such as methyl difluorochloroacetate (CClF 2 COOCH 3 , referred to as CDFAMe) and ethyl difluorochloroacetate (CClF 2 COOC 2 h 5 , referred to as CDFAEt), due to containing CClF 2 The - group can not only be used for hydrodechlorination to prepare difluoroacetate and its derivatives, but also can be used as a building block for the synthesis of difluoromethyl and difluoromethylene for the synthesis of various compounds. Chlorodifluoroacetic acid (CClF 2 COOH, referred to as CDFA), can be used to synthesize difluoroacetic acid, aryl difluoromethyl ether and difluorocyclopropylidene compounds, etc., and can also be used to synthesize intermediates for drugs such as malaria and cancer. [0003] Difluorochloroacetate can pass through difluorochloroacetyl chloride (CClF 2 COCl (abbr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/14C07C69/63C07C51/04C07C53/18
CPCC07C51/04C07C67/14C07C69/63C07C53/18
Inventor 王术成刘武灿袁光伟刘建鹏吴江平王军祥
Owner ZHEJIANG RES INST OF CHEM IND CO LTD
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