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Preparation method of bismuth citrate

A technology of bismuth citrate and citric acid aqueous solution is applied in the fields of carboxylate preparation, organic chemistry, etc., and can solve the problems of unsuitability for industrial production, harsh conditions of ultra-fine metal bismuth, easy oxidation of ultra-fine bismuth, etc., and achieves the yield High and low impurity effect

Active Publication Date: 2013-06-26
昆明先导新材料科技有限责任公司
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Problems solved by technology

The conditions for the electrolytic production of ultrafine metal bismuth by this method are harsh, and the ultrafine bismuth is easily oxidized, so it is not suitable for industrial production

Method used

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preparation example Construction

[0014] The preparation method of bismuth citrate according to the present invention comprises steps: Step 1, pulverizing bismuth oxide to a prescribed average particle size; Step 2, preparing an aqueous citric acid solution with a predetermined concentration and heating it to a predetermined temperature lower than the boiling point of water; Step 3 , according to the chemical reaction equation Bi 2 o 3 +2C 6 h 8 o 7 = 2C 6 h 5 BiO 7 +3H 2 O makes the initial excess coefficient of citric acid in the citric acid aqueous solution remain below 1, and the bismuth oxide that pulverizes is gradually added in the citric acid aqueous solution of described heating, so that citric acid and bismuth oxide react; Step 4, with As the reaction progresses, another concentration of citric acid aqueous solution is gradually added to maintain the initial liquid-solid ratio; Step 5, after the reaction is completed, filter and dry to obtain bismuth citrate products.

[0015] Wherein, the in...

Embodiment 1

[0026] Step 1, pulverizing bismuth oxide to an average particle size of 0.1 μm. The crushing adopts the experimental jet mill produced by Shanghai Saishan Powder Machinery Manufacturing Co., Ltd.

[0027] Step 2, prepare 200 mL of citric acid aqueous solution with a concentration of 200 g / L, and heat to 60° C.

[0028] Step 3: Control the initial excess coefficient of citric acid to 0.3, weigh 43.7g of pulverized bismuth oxide particles and gradually add them to the citric acid aqueous solution in Step 2, and stir for 28 hours.

[0029] Step 4, during the reaction process, according to the viscosity of the reaction solution, gradually add 200 g / L citric acid aqueous solution to maintain the initial liquid-solid ratio of the reaction.

[0030] Step 5: After the reaction is completed, filter and wash the bismuth citrate product with ultrapure water until the pH of the filter cake is 5-7, and dry the filter cake in a vacuum drying oven at 60° C. to obtain a white powdery bismuth...

Embodiment 2

[0033] Step 1, pulverizing bismuth oxide to an average particle size of 0.2 μm. The crushing adopts the experimental jet mill produced by Shanghai Saishan Powder Machinery Manufacturing Co., Ltd.

[0034] Step 2, prepare 200 mL of citric acid aqueous solution with a concentration of 300 g / L, and heat to 70° C.

[0035] Step 3: Control the initial excess coefficient of citric acid to 0.5, weigh 56.83g of pulverized bismuth oxide particles, and gradually add them to the citric acid aqueous solution in Step 2, and stir for 36 hours.

[0036] Step 4, during the reaction process, according to the viscosity of the reaction solution, gradually add 150 g / L citric acid aqueous solution to maintain the initial liquid-solid ratio of the reaction.

[0037] Step 5: After the reaction is completed, filter and wash the bismuth citrate product with ultrapure water until the pH of the filter cake is 5-7, and dry the filter cake in a vacuum oven at 60°C to obtain a white powdery bismuth citrat...

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Abstract

The invention provides a preparation method of bismuth citrate. The preparation method comprises the steps of 1, smashing bismuth oxide into specified average grain diameter; 2, preparing a citric acid aqueous solution with the predetermined concentration and heating to a predetermined temperature lower than the boiling point of water; 3, remaining the initial excess coefficient of citric acid in the citric acid aqueous solution below 1 according to the chemical reaction equation Bi2O3+2C6H8O7=2C6H5BiO7+3H2O and gradually adding the smashed bismuth oxide into the heated citric acid aqueous solution to ensure that the citric acid reacts with the bismuth oxide; 4, as the reaction progresses, gradually adding the citric acid aqueous solution with another concentration to keep the initial liquid-solid ratio; and 5, after the reaction is finished, filtering and drying to obtain the bismuth citrate product. The preparation method of the bismuth citrate, provided by the invention, has the advantages of no special requirements on equipment, easiness in the industrial production, simple process, convenience in operation and control, high yield and little impurity.

Description

technical field [0001] The invention relates to a preparation method of a bismuth compound, in particular to a preparation method of bismuth citrate. Background technique [0002] Bismuth citrate (also known as bismuth citrate) is an intermediate for treating stomach diseases and anti-ulcer drugs. For the treatment of gastric ulcer, duodenal ulcer, compound ulcer, multiple ulcer and anastomotic ulcer. And for the treatment of chronic superficial gastritis and Helicobacter pylori infection. The traditional method for producing bismuth citrate is mainly to add citric acid to the bismuth nitrate solution to react to generate products or to adjust the pH value of bismuth nitrate so that it generates bismuth hydroxide and then reacts with citric acid to generate products. NO in bismuth citrate produced by traditional methods 3 - higher. [0003] The Chinese Invention Application Publication No. CN1793101A published on June 28, 2006 discloses a method for hydrothermally synth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/265C07C51/41
Inventor 朱刘李琼芳徐金凤
Owner 昆明先导新材料科技有限责任公司
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