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Synthesis production process of difluorochloroacetic acid

A difluorochloroacetic acid and production process technology, applied in the direction of sulfur compounds, chlorine/hydrogen chloride, acid halide preparation, etc., can solve the problems of many by-products and high prices, achieve high absorption rate and total yield, low energy consumption, Reasonable effect of preparation process design

Active Publication Date: 2016-08-17
NANTONG BAOKAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The price of raw materials in this process is relatively high, and there are many by-products

Method used

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  • Synthesis production process of difluorochloroacetic acid

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Effect test

Embodiment 1

[0023] Such as figure 1 A kind of synthetic production technique of difluorochloroacetic acid shown, comprises the steps:

[0024] (1) Using a batch process, press sulfur trioxide into the oxidation reaction kettle with nitrogen, and start stirring;

[0025] (2) After reaching a certain temperature, add difluorotetrachloroethane and catalyst to the oxidation reactor according to the specified ratio;

[0026] (3) Start the heating reaction and observe the reflux condition. When the temperature of the kettle rises to a certain temperature but the reflux is small, the oxidation reaction of the raw material difluorotetrachloroethane is basically completed;

[0027] (4) Start the operation of steaming by-product sulfuryl chloride, and then carry out the hydrolysis process: adopt a batch process, first add a certain amount of water into the hydrolysis reaction kettle, slowly add sulfuryl chloride dropwise, and stir at a temperature of 20-100°C for hydrolysis reaction, the generate...

Embodiment 2

[0038] A kind of synthetic production technique of difluorochloroacetic acid, comprises the steps:

[0039] (1) Using a batch process, press sulfur trioxide into the oxidation reaction kettle with nitrogen, and start stirring;

[0040] (2) After reaching a certain temperature, add difluorotetrachloroethane and catalyst to the oxidation reactor according to the specified ratio;

[0041] (3) Start the heating reaction and observe the reflux condition. When the temperature of the kettle rises to a certain temperature but the reflux is small, the oxidation reaction of the raw material difluorotetrachloroethane is basically completed;

[0042] (4) Start the operation of steaming by-product sulfuryl chloride, and then carry out the hydrolysis process: adopt a batch process, first add a certain amount of water into the hydrolysis reaction kettle, slowly add sulfuryl chloride dropwise, and stir at a temperature of 20-100°C for hydrolysis reaction, the generated hydrogen chloride gas ...

Embodiment 3

[0053] A kind of synthetic production technique of difluorochloroacetic acid, comprises the steps:

[0054] (1) Using a batch process, press sulfur trioxide into the oxidation reaction kettle with nitrogen, and start stirring;

[0055] (2) After reaching a certain temperature, add difluorotetrachloroethane and catalyst to the oxidation reactor according to the specified ratio;

[0056] (3) Start the heating reaction and observe the reflux condition. When the temperature of the kettle rises to a certain temperature but the reflux is small, the oxidation reaction of the raw material difluorotetrachloroethane is basically completed;

[0057] (4) Start the operation of steaming by-product sulfuryl chloride, and then carry out the hydrolysis process: adopt a batch process, first add a certain amount of water into the hydrolysis reaction kettle, slowly add sulfuryl chloride dropwise, and stir at a temperature of 20-100°C for hydrolysis reaction, the generated hydrogen chloride gas ...

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Abstract

The invention discloses a synthesis production process of difluorochloroacetic acid, comprising the following steps: charging sulfur trioxide with nitrogen gas into an oxidation reaction kettle by an intermittent process, starting stirring; after reaching a certain temperature, adding difluorotetrachloroethane and catalyst according to a predetermined ratio into the oxidation reaction kettle; heating for reaction, observing the backflow condition, starting steaming the byproduct sulfuric chloride when the kettle temperature rises to a certain temperature while the backflow is small; after steaming the byproduct sulfuric chloride, carrying out charging for the second time; carrying out three-stage spray hydrolysis and absorption on the product difluorochloracetyl chloride to generate crude product difluorochloroacetic acid, and carrying out defluorination and rectification on the crude product to obtain finished product difluorochloroacetic acid. The synthesis production process of difluorochloroacetic acid disclosed by the invention adopts the difluorotetrachloroethane as a raw material, the finished product difluorochloroacetic acid is prepared by oxidation reaction, the preparation process has reasonable design, high absorption rate, high overall yield and low energy consumption; and the byproduct can be hydrolyzed and reused, so that the production process is clean, environment-friendly, safe and reliable.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a synthesis production process of difluorochloroacetic acid. Background technique [0002] Difluorochloroacetic acid is an important intermediate in organic synthesis, often used in the synthesis of drugs and pesticides with biological enzyme inhibitory functions. In difluorochloroacetic acid, a difluoromethyl group with strong biological activity is introduced into the compound by replacing the chlorine atom, thereby increasing the activity of biological enzymes. [0003] At present, the synthesis techniques of difluorochloroacetic acid mainly include the following types; 1) Using tetrafluoroethylene as raw material to synthesize chlorodifluoroacetyl, and then hydrolyzing it to form difluorochloroacetic acid. Tetrafluoroethylene is reacted with sodium methoxide to form trifluorovinyl methyl ether, then added with chlorine gas, then oxidized with chlorosulf...

Claims

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Application Information

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IPC IPC(8): C07C51/04C07C53/18C01B7/01C01B17/74
CPCC01B7/01C01B17/74C07C51/04C07C51/58C07C53/48C07C53/18
Inventor 葛繁龙闫宗刚褚军王松建
Owner NANTONG BAOKAI CHEM
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