A method for purifying high-purity trichloroacetone for preparing folic acid

A technology of trichloroacetone and a purification method, applied in the field of purification of high-purity trichloroacetone, can solve the problems of high cost, complicated process, low yield and purity, and achieve the effects of low price, good purity and high extraction rate

Active Publication Date: 2020-07-17
CHANGZHOU XINHONG PHARMA & CHEM IND TECHOLOGIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem to be solved in the present invention is to provide a simple process, convenient operation, low cost, environmental protection and high yield for the problems of complex process, high cost, low yield and purity in the current purification process of trichloroacetone. The purification process of high-purity trichloroacetone, which can improve low-purity trichloroacetone (such as about 50%) to more than 98%, and the high-purity trichloroacetone obtained is applied to the preparation of folic acid and has also achieved good results

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The first step: trichloroacetone crude product is extracted with water:

[0021] Add 400 ml (about 600 grams) of commercially available trichloroacetone (content 51.8%) into a 1000 ml beaker, add 200 ml of water, heat up to about 35°C under stirring, transfer to a 1000 ml separatory funnel for shaking, and then let it stand for stratification , separate the upper trichloroacetone aqueous extract and place it separately, continue to add 200 ml of water to the lower layer and repeat the above operation to extract trichloroacetone, and the trichloroacetone aqueous extract separated for the second time is merged into the trichloroacetone water separated for the first time In the extract, 200 ml of water was added to the lower layer to repeat the above operation to extract trichloroacetone, and the trichloroacetone aqueous extracts extracted three times were combined. The total time of three extractions is about 2.5 hours, and the content of trichloroacetone in the water ext...

Embodiment 2

[0025] The first step: trichloroacetone crude product extraction:

[0026] Add 400 milliliters (about 600 grams) of commercially available trichloroacetone (content 51.8%) in a 1000 milliliter beaker, add filtrate (the filtrate described in the second step in the embodiment 1) 240 milliliters, heat up to about 35 ℃ under stirring, transfer After shaking the separating funnel to 1000 milliliters, let it stand for stratification, separate the trichloroacetone water extract from the upper layer and place it separately, and continue to add 200 milliliters of filtrate to the lower layer to repeat the above operation to extract trichloroacetone, and the trichloroacetone water separated for the second time The extract was merged into the trichloroacetone water extract that was separated for the first time, and about 200 ml of filtrate was added to the lower layer to repeat the above operation to extract trichloroacetone, and the trichloroacetone water extract extracted three times was...

Embodiment 3

[0030] The first step: trichloroacetone crude product extraction:

[0031] Add 400 milliliters (about 600 grams) of commercially available trichloroacetone (content 51.8%) in a 1000 milliliter beaker, add filtrate (the filtrate described in the second step in the embodiment 1) 240 milliliters, heat up to about 10 ℃ under stirring, transfer After shaking the separating funnel to 1000 milliliters, let it stand for stratification, separate the trichloroacetone water extract from the upper layer and place it separately, and continue to add 200 milliliters of filtrate to the lower layer to repeat the above operation to extract trichloroacetone, and the trichloroacetone water separated for the second time The extract was merged into the trichloroacetone water extract that was separated for the first time, and about 200 ml of filtrate was added to the lower layer to repeat the above operation to extract trichloroacetone, and the trichloroacetone water extract extracted three times was...

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PUM

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Abstract

The invention discloses a method for purifying high-purity trichloroacetone for preparation of folic acid. The method is characterized in that a water solvent is used for purifying to prepare the high-purity trichloroacetone, and comprises the following steps of step 1, using the water solvent to extract the trichloroacetone with purity of 50% by three times; step 2, recrystallizing the obtained extracting solution by a gradient cooling type, and increasing the purity of the crude trichloroacetone with purity of about 50% to be above 98% by two steps of purification, wherein the extracting yield rate of trichloroacetone is 90% or above, the solution after separating and crystallizing in step 2 can be repeatedly utilized, and the yield rate of trichloroacetone can reach 80% or above by raw material. The method has the advantages that the preparation of high-purity trichloroacetone is easy, the safety and environment-friendly effects are realized, and the requirement of industrialization on environment protection is met; the prepared high-purity trichloroacetone can be used for preparing the folic acid, and the yield rate and purity of the folic acid are certainly improved.

Description

technical field [0001] The invention relates to the technical field of compound purification, in particular to a method for purifying high-purity trichloroacetone, in particular to a method for purifying high-purity trichloroacetone for folic acid synthesis. Background technique [0002] Trichloroacetone is a very important chemical raw material. Trichloroacetone, especially high-purity trichloroacetone, has an extremely wide range of uses and can be used for the synthesis and Research. [0003] Trichloroacetone is also an important intermediate in the production of folic acid. Folic acid, also known as vitamin M or vitamin B9, is one of the basic varieties of vitamins. It is used to treat megaloblastic anemia, aplastic anemia, neutropenia, dysplasia, colorectal cancer and other diseases, and can prevent neural tube defects. It is used as an anti-anemia drug additive and nutritional supplement in the food and feed industries. [0004] Traditional synthetic method of folic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/78C07C49/16C07D475/04
CPCC07C45/78C07D475/04C07C49/16
Inventor 王胜忠张继振王国华
Owner CHANGZHOU XINHONG PHARMA & CHEM IND TECHOLOGIES
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