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Method for synthesizing bismuth potassium citrate

A technology of bismuth potassium citrate and potassium citrate, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., can solve problems such as time-consuming, high cost, and low efficiency, and achieve raw material cost Low cost, mild reaction conditions, and simple process

Inactive Publication Date: 2018-04-27
清远先导材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But there are several problems in the ethanol recrystallization method: in the concentration process, the concentration ratio has a greater impact on the precipitation rate of bismuth and the bismuth content of the product, and it is difficult to control the product specification; the ethanol recrystallization and washing process will reduce the yield, and it takes more time to consume Many, low efficiency, and difficult to control product particle size; mass production also needs to consider the problem of ethanol explosion; more demand for ethanol, higher cost
Therefore, this method is not suitable for mass production

Method used

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  • Method for synthesizing bismuth potassium citrate
  • Method for synthesizing bismuth potassium citrate
  • Method for synthesizing bismuth potassium citrate

Examples

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Effect test

Embodiment 1

[0026] Weigh 40 mL of deionized water into a beaker, start stirring at room temperature, add 16.8 g of citric acid monohydrate, then add 16.2 g of potassium hydroxide, and stir for 10 min to obtain a potassium citrate solution. Weigh 80mL of deionized water and place it in a flask, add 30mL of ammonia water with a concentration of 25% to the flask while stirring, then add 72.7g of bismuth citrate in batches, and stir until the bismuth citrate is completely dissolved to obtain ammonium bismuth citrate solution. Set the heating temperature to 55°C, add potassium citrate solution to the ammonium bismuth citrate solution while stirring, stop heating and stirring after stirring for 30 minutes, and then spray dry at 150°C to obtain potassium bismuth citrate. It was found that the yield of potassium bismuth citrate was 96.7%.

Embodiment 2

[0028] Weigh 40 mL of deionized water into a beaker, start stirring at room temperature, add 16.8 g of citric acid monohydrate, then add 16.2 g of potassium hydroxide, and stir for 20 min to obtain a potassium citrate solution. Weigh 120mL of deionized water and place it in a flask, add 26mL of ammonia water with a concentration of 25% to the flask while stirring, then add 65g of bismuth citrate in batches, and stir until the bismuth citrate is completely dissolved to obtain ammonium bismuth citrate solution . Set the heating temperature at 90°C, add potassium citrate solution to the ammonium bismuth citrate solution while stirring, stop heating and stirring after stirring for 30 minutes, and then spray dry at 180°C to obtain potassium bismuth citrate, calculated as It is known that the yield of potassium bismuth citrate is 97.4%.

Embodiment 3

[0030] Weigh 50 mL of deionized water into a beaker, start stirring at room temperature, add 26.1 g of potassium citrate monohydrate, and stir for 15 min to obtain a potassium citrate solution. Weigh 100mL of deionized water and place it in a beaker, add 26mL of ammonia water with a concentration of 25% to the flask while stirring, then add 65g of bismuth citrate in batches, stir until the bismuth citrate is completely dissolved, and obtain a bismuth ammonium citrate solution . Set the heating temperature to 75°C, add potassium citrate solution to bismuth ammonium citrate solution while stirring, stop heating and stirring after stirring for 30 minutes, and then spray dry at 160°C to obtain bismuth potassium citrate, calculated as Known, the productive rate of potassium bismuth citrate is 96.9%.

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Abstract

The application provides a method for synthesizing bismuth potassium citrate, comprising the steps of preparing potassium citrate solution; adding deionized water into a reactor under stirring, addingammonia water or introducing ammonia gas into deionized water, and adding bismuth citrate until full dissolution to obtain ammonium bismuth citrate solution; stirring continuously, adding the ammonium bismuth citrate solution into the reactor so that potassium citrate reacts with ammonium bismuth citrate, and spray-drying after reaction to obtain bismuth potassium citrate. The synthetic method ofthe application has simple process, low material cost and mild reaction conditions and is suitable for large-scale production.

Description

technical field [0001] The present application relates to the field of drug synthesis, in particular to a method for synthesizing bismuth potassium citrate. Background technique [0002] Potassium bismuth citrate is a compound containing bismuth. Its preparation method generally requires the preparation of bismuth subnitrate intermediate. The process is more complicated and the cost is higher. Crystallization, washing and drying to obtain the product. The Chinese patent application 201610632889.4 with an application date of August 3, 2016 discloses the above method. But there are several problems in the ethanol recrystallization method: in the concentration process, the concentration ratio has a greater impact on the precipitation rate of bismuth and the bismuth content of the product, and it is difficult to control the product specification; the ethanol recrystallization and washing process will reduce the yield, and it takes more time to consume Many, low efficiency, and...

Claims

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Application Information

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IPC IPC(8): C07C59/265C07C51/41
CPCC07C51/412C07C59/265
Inventor 孙彤光朱刘郭高伟薄福丽
Owner 清远先导材料有限公司
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