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Preparation method of bismuth citrate

A technology of bismuth citrate and citrate, which is applied in the field of synthesizing bismuth-based raw materials, can solve the problems of black spots in products, difficult to complete reaction and high product yield, and achieves excellent appearance quality, reduced processing cost, and technological process. simple effect

Active Publication Date: 2014-06-18
FIRST RARE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Among them, nano-bismuth powder is synthesized by reaction with citric acid, the cost of producing nano-bismuth powder is high, the excess coefficient of citric acid is large, the reaction is difficult to complete, the product quality is poor, and there is a hidden danger of incomplete reaction
And bismuth oxide is synthesized by direct reaction with citric acid, the excess coefficient of citric acid is large, the reaction time is longer, the temperature is higher, and the reaction is difficult to complete, the product quality is poor, and there are high requirements on the purity and particle size of bismuth oxide, and the purity is not high. Then the reaction is difficult to complete, the reaction is slow if the particle size is large, the overall reaction time is long, and the reaction is difficult to complete. In addition, the fire-process bismuth oxide with a relatively suitable price is generally used in production, because incompletely oxidized bismuth powder does not react with citric acid, so It is easy to cause black spots in the product, and the black spots are unreacted bismuth powder
[0005] Further say, above-mentioned two kinds of synthetic methods all need to add excessive bismuth citrate, the amount that adds is more than 1.2 times of theoretical amount, in the production process of raw material medicine, as reclaiming the residual citric acid in the mother liquor in production control The requirements are extremely strict, and there are risks such as product pollution. Direct disposal will cause waste and increase the treatment cost of waste liquid, and the product yield is high.

Method used

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preparation example Construction

[0023] The embodiment of the present invention provides a preparation method of bismuth citrate, using bismuth nitrate solution and citrate solution as raw materials to synthesize bismuth citrate in one step.

[0024] It should be noted that purified water (H 2 O) has a molecular weight of 18.02, and is generally water for medicinal purposes obtained from drinking water by distillation, ion exchange, reverse osmosis or other appropriate methods, without any additives.

[0025] Bismuth nitrate is a colorless and lustrous crystal with the smell of nitric acid, easy to deliquescence, the solution is acidic, decomposed into basic salt in water, soluble in dilute nitric acid, it is mainly used in the manufacture of medicine and bismuth salt.

[0026] A kind of preparation method of bismuth citrate provided by the invention comprises the following steps:

[0027] Step A, adding bismuth nitrate solution to the citrate solution, the molar ratio of bismuth nitrate in the bismuth nitra...

Embodiment 1

[0046] Add 500 mL of purified water into the reaction kettle, add 500 g of sodium citrate to the reaction kettle at room temperature, and stir until the sodium citrate is completely dissolved in the purified water.

[0047] Continue to stir, control the rotational speed at 50rpm, add 3900g of bismuth nitrate solution to the reaction kettle at the same time, control the reaction temperature at 80°C, and control the feeding time within 60 minutes. After adding the bismuth nitrate solution, continue to keep warm and stir, and react for 1 hour. Wherein, the bismuth nitrate solution is bismuth nitrate content Bi(NO 3 ) 3 %=18.25%, free acidity=9.7%.

[0048] After reacting for 1 hour, remove the supernatant, wash and filter with 600ml of purified water, vacuum-dry at 90°C, and dry for 8h at a vacuum degree of ≤0.8Mpa to obtain 707.3g of bismuth citrate sample.

[0049] After testing, the bismuth content was 52.43%, and the other indicators also met the standards of the United Sta...

Embodiment 2

[0051] Add 1000 mL of purified water to the reactor, add 500 g of sodium citrate to the reactor at room temperature, and stir until the sodium citrate is completely dissolved in the purified water.

[0052] Continue to stir, control the rotational speed at 120rpm, add 2100g of bismuth nitrate solution to the reaction kettle at the same time, control the reaction temperature at 60°C, and control the feeding time within 40 minutes. After adding the bismuth nitrate solution, continue to keep warm and stir, and react for 4 hours. Wherein, the bismuth nitrate solution is bismuth nitrate content Bi(NO 3 ) 3 %=30.48%, free acidity=5.2%.

[0053] After reacting for 4 hours, remove the supernatant, wash and filter with 600ml of purified water, vacuum-dry at 90°C, and dry for 8h at a vacuum degree of ≤0.8Mpa to obtain 639.9g of bismuth citrate sample.

[0054] After testing, the content of bismuth was 52.49%, and other indicators also met the standards of the United States Pharmacopoe...

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PUM

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Abstract

The embodiment of the invention discloses a preparation method of bismuth citrate. The method comprises the following steps: A, adding a bismuth nitrate solution into a citrate solution; B, reacting for 1 to 6 hours in a heat preservation manner at 60 DEG C to 80 DEG C; and C, washing and drying so as to prepare the bismuth citrate. The bismuth citrate is synthesized by one step by taking the bismuth nitrate solution and the citrate solution as raw materials, so that the process is simple and short in time; the reaction speed of the citrate solution is rapid, so that the yield of the bismuth citrate is high and the quality of the bismuth citrate is good; the consumption of the raw materials is decreased, so that the treatment cost of waste liquids is reduced; the reaction is thoroughly carried out, so that the obtained bismuth citrate is good; the difficult problem caused by the existing technology is avoided well.

Description

technical field [0001] The invention relates to the synthesis of bismuth-based raw materials, in particular to a preparation method of bismuth citrate. Background technique [0002] Bismuth citrate, also known as bismuth citrate, is the raw material for the synthesis of bismuth drug bismuth potassium citrate. Bismuth potassium citrate is a stomach drug that can disintegrate rapidly in the stomach. The protein on the ulcer surface or inflammation site forms insoluble bismuth-containing precipitates, which firmly adhere to the erosion surface to form a protective barrier, resist the erosion of gastric acid and pepsin on the mucosal surface, and stimulate the release of endogenous prostaglandins to promote gastric mucus secretion , to accelerate the repair of mucosal epithelium, in addition to the role of eliminating Helicobacter pylori, clinically used for the treatment of gastric ulcer, duodenal ulcer and erythema exudative gastritis erosive gastritis. In addition, bismuth c...

Claims

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Application Information

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IPC IPC(8): C07C59/265C07C51/41
CPCC07C51/412C07C59/265
Inventor 王波朱刘刘留朱世明朱世会
Owner FIRST RARE MATERIALS CO LTD
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