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Process for synthesizing pharmaceutical-grade sodium diacetate

A technology of sodium diacetate and synthesis process, applied in the field of preparation of vitamin B1 intermediates, can solve the problems of difficult to meet high-end pharmaceutical-grade customers, easy to mix unevenly, uneven particle size distribution, etc., to achieve considerable product profit and good fluidity. , the effect of uniform particle size

Active Publication Date: 2015-07-22
江苏兄弟维生素有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The crystal particles of this method are uniform, but the production process is slightly complicated and the yield is low
[0006] The sodium diacetate obtained by the above three methods tends to have fine particles, the average particle size is 100 mesh to 300 mesh, and the particle size distribution is uneven. When used as an additive, it is easy to mix unevenly, and it is difficult to meet the needs of high-end pharmaceutical grade customers.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] At room temperature, the methanol solution of sodium methoxide and anhydrous acetic acid are mixed and reacted according to the molar ratio of 1:2 to form sodium diacetate and methanol, and then stirred and concentrated at 70°C at a speed of 120rap / min to obtain methanol, and the obtained Methanol sodium diacetate crystals, and finally, under the condition of -0.6Mpa, dry to obtain sodium diacetate.

[0022] The average particle size range of the obtained sodium diacetate prepared in this embodiment can reach 70 mesh to 90 mesh, and the yield is 90.29%.

Embodiment 2

[0024] At room temperature, the methanol solution of sodium methoxide and anhydrous acetic acid were mixed and reacted according to the molar ratio of 1:2 to form sodium diacetate and methanol, and then stirred and concentrated at 75°C at a speed of 140rap / min to obtain methanol, and the obtained Sodium diacetate crystals in methanol, and finally, dry under the condition of -0.4Mpa to obtain sodium diacetate.

[0025] The average particle size range of the obtained sodium diacetate prepared in this example can reach 80 mesh to 100 mesh, and the yield is 91.40%.

Embodiment 4

[0027] At room temperature, the methanol solution of sodium methoxide and anhydrous acetic acid were mixed and reacted according to the molar ratio of 1:2 to form sodium diacetate and methanol, and then stirred and concentrated at 72°C at a speed of 150rap / min to obtain methanol, and the obtained Sodium diacetate crystals in methanol, and finally, dry under the condition of -0.3Mpa to obtain sodium diacetate.

[0028] The average particle size range of the obtained sodium diacetate prepared in this embodiment can reach 50 mesh to 80 mesh, and the yield is 90.26%.

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PUM

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Abstract

The invention discloses a process for synthesizing pharmaceutical-grade sodium diacetate. The process comprises the following steps: reacting a methanol solution of sodium methylate and acetic anhydride according to a molar ratio being 1:2 to generate sodium diacetate and methanol; concentrating out methanol, and separating sodium diacetate crystal containing methanol; under the condition of negative pressure, drying, and obtaining sodium diacetate. The sodium diacetate product obtained by the process is very uniform in particle size and good in liquidity, the average particle size range can achieve 50-100 meshes, the content is high and can achieve 99.9 percent, and the demand of high-end medical customers can be met. The product is profitable and has a market prospect.

Description

technical field [0001] The invention relates to the technical field of vitamin production and processing, in particular to a method for preparing vitamin B1 intermediates. Background technique [0002] At present, the synthesis technique of sodium diacetate, three technological routes adopted in the world are: [0003] First, the one-step reaction method of sodium acetate and acetic acid in ethanol. In recent years, manufacturers who have realized industrialized production in our country mostly adopt this method. Although the production process of this method is simple, the production cost is relatively high and the equipment investment is large; [0004] Second, sodium carbonate and acetic acid are synthesized under the action of acetic anhydride. The reaction conditions of this method are harsh, the operation is difficult to control, the product output is unstable, and because the raw material price of acetic anhydride is high and rare, it is rarely used; [0005] Thir...

Claims

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Application Information

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IPC IPC(8): C07C53/10C07C51/41
CPCC07C51/412C07C53/10
Inventor 李来成沈银元陈英明崔胜凯
Owner 江苏兄弟维生素有限公司
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