Method of synthesizing 1, 3-dichloroacetone with catalysis of silicon dioxide-carried phosphotungstic heteropoly acid

A technology of phosphotungstic heteropolyacid and silicon dioxide, which is applied in the preparation of carbonyl compounds by oxidation, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of application limitation, small specific surface area, difficulty in recycling, etc. High performance, high yield and good purity

Inactive Publication Date: 2018-04-24
SHAANXI HUANKE BIOLOGICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the specific surface area of ​​heteropoly acid is small (2 /g), easily so...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The method for synthesizing 1,3-dichloroacetone catalyzed by silica-supported phosphotungstic acid includes the following steps:

[0019] (1) Dissolve sodium tungstate dihydrate in water at 40°C, add phosphoric acid dropwise to the system under stirring, and reflux at 80°C for 6 hours after the addition is complete; among them, sodium tungstate dihydrate, water, phosphoric acid The mass ratio is 3:20:2;

[0020] (2) The product of step (1) is naturally cooled and crystallized, the crystals are re-dissolved in 80°C water, and then extracted with ether, and recrystallized in water to obtain phosphotungstic heteropoly acid;

[0021] (3) Mix ethyl orthosilicate, deionized water, absolute ethanol, and phosphotungstic heteropoly acid in a mass ratio of 14:25:20:0.45, stir at 55°C to form a gel, and then Leave it to stand for 24 hours and dry it at 140°C for 4 hours to obtain a silica-supported phosphotungstic heteropoly acid catalyst;

[0022] (4) Mix 1,3-dichloropropanol with a 30%...

Embodiment 2

[0024] The method for synthesizing 1,3-dichloroacetone catalyzed by silica-supported phosphotungstic acid includes the following steps:

[0025] (1) Dissolve sodium tungstate dihydrate in water at 50°C, add phosphoric acid dropwise to the system under stirring, and reflux at 80°C for 8 hours after the addition is complete; among them, sodium tungstate dihydrate, water, phosphoric acid The mass ratio is 3:20:2;

[0026] (2) The product of step (1) is naturally cooled and crystallized, the crystals are re-dissolved in 80°C water, and then extracted with ether, and recrystallized in water to obtain phosphotungstic heteropoly acid;

[0027] (3) Mix ethyl orthosilicate, deionized water, absolute ethanol, and phosphotungstic heteropoly acid at a mass ratio of 14:35:25:3.3, stir at 60℃ to form a gel, and then Leave it to stand for 24 hours and dry it at 150°C for 4 hours to obtain a silica-supported phosphotungstic heteropoly acid catalyst;

[0028] (4) Mix 1,3-dichloropropanol with a 30% m...

Embodiment 3

[0030] The method for synthesizing 1,3-dichloroacetone catalyzed by silica-supported phosphotungstic acid includes the following steps:

[0031] (1) Dissolve sodium tungstate dihydrate in water at 45°C, add phosphoric acid dropwise to the system under stirring, and reflux at 80°C for 7 hours after the addition is complete; among them, sodium tungstate dihydrate, water, phosphoric acid The mass ratio is 3:20:2;

[0032] (2) The product of step (1) is naturally cooled and crystallized, the crystals are re-dissolved in 80°C water, and then extracted with ether, and recrystallized in water to obtain phosphotungstic heteropoly acid;

[0033] (3) Mix ethyl orthosilicate, deionized water, absolute ethanol, and phosphotungstic heteropoly acid at a mass ratio of 14:30:22:2.2, stir at 58°C to form a gel, and then Leave it to stand for 24 hours and dry it at 145°C for 4 hours to obtain a silica-supported phosphotungstic heteropoly acid catalyst;

[0034] (4) Mix 1,3-dichloropropanol with a 30% ...

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Abstract

The invention discloses a method for catalytically synthesizing 1,3-dichloroacetone supported by silica-supported phosphotungstic heteropolyacid, which comprises the following steps: (1) dissolving sodium tungstate dihydrate in water, and injecting into the system under stirring Phosphoric acid was added dropwise in the water, and then refluxed after the dropwise addition; (2) Natural cooling and crystallization, redissolving the crystals in water at 80°C, then adding ether for extraction, recrystallizing in water, and obtaining phosphotungstic heteropoly acid; (3) Tetraethyl orthosilicate, deionized water, absolute ethanol, and phosphotungstic heteropolyacid are mixed and stirred to form a gel, then left to stand for aging and dried to obtain silica-loaded phosphotungstic heteropoly Acid catalyst; (4) Mix 1,3-dichloropropanol with hydrogen peroxide solution, add silica-supported phosphotungstic heteropolyacid catalyst, react at constant temperature for 10 hours, filter, and the filtrate is 1,3-dichloroacetone . The method provided by the invention has the advantages of simple operation, less environmental pollution, high yield and good purity of 1,3-dichloroacetone.

Description

Technical field [0001] The invention belongs to a preparation method of 1,3-dichloroacetone, and specifically relates to a method for catalyzing the synthesis of 1,3-dichloroacetone by silica-supported phosphotungstic heteropoly acid. Background technique [0002] 1,3-Dichloroacetone has two active functional groups, carbonyl group and halogen atom, and is an important reaction intermediate in the chemical and pharmaceutical industries. [0003] At present, the synthesis methods of 1,3-dichloroacetone are as follows: (1) Direct substitution reaction of acetone with chlorine gas is used. This method is not easy to control the reaction rate, and large amounts of 1,1-dichloroacetone and 1,1,3- Trichloroacetone is difficult to separate and severely corrodes the equipment; (2) 1,3-Dichloropropanol is used as raw material to prepare 1,3-chloride by the oxidation method of chromium trioxide-sulfuric acid or sodium dichromate-concentrated sulfuric acid Acetone, the yield of this method is...

Claims

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Application Information

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IPC IPC(8): C07C49/16C07C45/29B01J27/188B01J37/28B01J37/03
CPCC07C45/294B01J27/188B01J37/036B01J37/28C07C49/16
Inventor 郝青
Owner SHAANXI HUANKE BIOLOGICAL TECH CO LTD
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