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1,1,1-trichloroacetone preparation method

A technology of trichloroacetone and chloroacetone, which is applied in the field 1, can solve problems such as difficult operability, and achieve the effects of convenient operation, convenient raw materials, and convenient industrial production

Pending Publication Date: 2020-03-03
ZHANGJIAGANG JIULI NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This route is to electrolyze salt water to generate chlorine gas, and at the same time make the newly generated chlorine gas participate in the reaction quickly, so the industrial operability is relatively difficult

Method used

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  • 1,1,1-trichloroacetone preparation method

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preparation example Construction

[0026] The preparation method of 1,1,1-trichloroacetone of the present invention comprises the following steps:

[0027] Step 1, use a large amount of aqueous solution, drop into monochloroacetone and water, do not use other organic solvents; Aqueous solution and raw material monochloroacetone form a kind of water-oil two-phase system or water-monochloroacetone-undissolved basic compound three-phase system;

[0028] Step 2, the basic compound forms an aqueous solution or suspension in water;

[0029] Step 3, feed chlorine gas under stirring until the solution is clear;

[0030] Step 4, during the whole reaction process, the temperature is controlled at 0 to 25 degrees Celsius;

[0031] Step 5, after the reaction is over, let it stand still, separate the lower oil phase, wash with water, then dry with anhydrous calcium chloride or anhydrous sodium sulfate or anhydrous magnesium sulfate, filter off the desiccant, and obtain products 1, 1, 1 - Trichloroacetone.

[0032] The b...

Embodiment 1

[0038] In a 5-liter reaction kettle with mechanical stirring (externally connected to an exhaust gas absorption device), 231 grams of monochloroacetone, 564 grams of sodium bicarbonate, and 1080 grams of water were successively put in, the temperature was controlled at 20 to 24 degrees Celsius, and chlorine gas was passed for 6 hours under stirring. (About 400 grams according to the flowmeter calculation), the solution system becomes clear, put it aside for 1 hour, and separate the liquids, and the yellow-green organic phase liquid in the lower layer of the gained is dried with 200 grams of anhydrous calcium chloride to obtain the product 1,1,1-trichloro 298 grams of acetone, yield 74%; gas phase purity 85%, moisture<0.1%.

Embodiment 2

[0040] In a 5-liter reaction kettle with mechanical stirring (externally connected to an exhaust gas absorption device), 231 grams of monochloroacetone, 564 grams of sodium bicarbonate, and 1080 grams of water are successively dropped into, and the temperature is controlled at 10 to 20 degrees Celsius, and the chlorine gas is passed for about 7 hours under stirring. Hour (calculate about 400 grams according to flow meter), solution system becomes clarified, leaves standstill 1 hour, liquid separation, the yellow-green organic phase liquid of gained lower floor is dried with 200 grams of calcium chloride anhydrous, obtains product 1,1,1-three Chloroacetone 297 grams; gas phase purity 85%, water <0.1%.

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Abstract

The invention provides a 1,1,1-trichloroacetone preparation method, which comprises the following steps: 1, adding monochloroacetone and an alkaline compound into a large amount of an aqueous solutionwithout other organic solvents; 2, forming an aqueous solution or a turbid liquid from the alkaline compound in water while stirring; 3, introducing chlorine gas while stirring until the solution isclear; and 4, in the whole reaction process, controlling the temperature at 0-25 DEG C. According to the invention, the method is simple in process, convenient to operate, high in yield and convenientfor industrial production, and can effectively control the acetone chlorination position, so that the generation of byproducts such as 1,1,3-trichloroacetone, tetrachloroacetone, pentachloroacetone and the like is reduced, and the purity of the prepared product is high and can reach more than 85% without further purification.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a preparation method of 1,1,1-trichloroacetone. Background technique [0002] Chlorinated acetone series compounds are important organic chemical raw materials. There are two Class A compounds on acetone, with a total of 6 hydrogens, which can be replaced by chlorine separately or simultaneously to form monochloroacetone to hexachloroacetone series compounds. Starting from different raw materials, relatively simple substituted chloroacetones can be prepared, such as oxidizing chlorohydrins to prepare corresponding chloroacetones, etc., or through the chlorination process of acetone, forming acetals with alcohols, and then obtaining the target in catalytic protection Product, although some of these methods can obtain relatively high-purity chloroacetone, because the raw material price is relatively expensive, the operation is relatively complicated, and it is not suitable...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/63C07C49/16
CPCC07C45/63C07C49/16
Inventor 苏旭
Owner ZHANGJIAGANG JIULI NEW MATERIAL TECH CO LTD
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