Preparation method for bismuth subsalicylate

A technology of bismuth subsalicylate and salicylic acid, which is applied in the field of preparation of bismuth compounds, can solve the problems of being unsuitable for industrial production, harsh conditions for ultra-fine metal bismuth, and easy oxidation of ultra-fine bismuth, so as to achieve less impurities and easy Industrialized production, high yield effect

Active Publication Date: 2013-07-03
昆明先导新材料科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0013] The preparation method of bismuth subsalicylate according to the present invention comprises the steps of: pulverizing bismuth oxide to a specified average particle size; according to the chemical reaction equation Bi 2 o 3 +2C 7 h 6 o 3 = 2C 7 h 5 BiO 4 +H 2 O makes the initial excess coefficient of the salicylic acid of salicylic acid aqueous solution be 0.05~0.3, prepare salicylic acid according to the quality and initial excess coefficient of the bismuth oxide that will adopt pulverization; Add the bismuth oxide of pulverization gradually to be heated to predetermined temperature In the aqueous solution of salicylic acid, the salicylic acid is reacted with bismuth oxide under the conditions of maintaining a predetermined temperature and avoiding light; after the reaction is completed, filter, wash and dry to obtain a bismuth subsalicylate product.

[0014] In the method for preparing bismuth subsalicylate according to the present invention, preferably, the sp...

Embodiment 1

[0023] The bismuth oxide is pulverized to an average particle size of 0.2 μm, and the pulverization adopts an experimental airflow pulverizer produced by Shanghai Saishan Powder Machinery Manufacturing Co., Ltd.;

[0024] Control the initial excess coefficient of salicylic acid to 0.05, weigh 75g of pulverized bismuth oxide particles, add salicylic acid into water, and heat to 80°C.

[0025] Weigh the bismuth oxide particles and gradually add them to the salicylic acid aqueous solution, keep away from light and stir for 1 hour, and increase the stirring speed as the reaction progresses;

[0026] After the reaction finishes, filter and wash the product bismuth subsalicylate with ultrapure water, then use excessive salicylic acid in the absolute ethanol washing product;

[0027] Dry the filter cake in a vacuum oven at 60°C to obtain a white powder product.

[0028] The obtained product was detected and analyzed by EDTA coordination titration, and the content of bismuth in the d...

Embodiment 2

[0030] The bismuth oxide is pulverized to an average particle size of 0.35 μm, and the pulverization adopts an experimental jet pulverizer produced by Shanghai Saishan Powder Machinery Manufacturing Co., Ltd.;

[0031] Control the initial excess coefficient of salicylic acid to 0.1, weigh 75g of pulverized bismuth oxide particles, add salicylic acid into water, and heat to 80°C;

[0032] The bismuth oxide particles weighed will be gradually added to the salicylic acid aqueous solution, and the light-proof airtight stirring reaction will be carried out for 1.5 hours, and the stirring speed will be accelerated as the reaction proceeds;

[0033] After the reaction finishes, filter and wash the product bismuth subsalicylate with ultrapure water, then use excessive salicylic acid in the absolute ethanol washing product;

[0034] Dry the filter cake in a vacuum oven at 50°C to obtain a white powder product.

[0035] The obtained product was detected and analyzed by EDTA coordinatio...

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Abstract

The invention provides a preparation method for bismuth subsalicylate. The preparation method comprises the steps of smashing bismuth oxide into particles with specified average particle size which is 0.1-1.35 mu m; making an initial excess coefficient of salicylic acid of a salicylic acid aqueous solution 0.05-0.3 according to a chemical reaction equation Bi2O3 + 2C7H6O3 = 2C7H5BiO4 + H2O; preparing the salicylic acid aqueous solution according to mass of the smashed bismuth oxide that to be adopted and the initial excess coefficient; gradually adding the smashed bismuth oxide into the salicylic acid aqueous solution heated to a predetermined temperature; reacting the salicylic acid and the bismuth oxide while keeping the predetermined temperature and a sealed condition away from light; and filtering and drying after the reaction is finished, thus obtaining a bismuth subsalicylate product. The preparation method can reduce production conditions for the raw material metal bismuth, can effectively reduce oxidation of the raw material metal bismuth and can easily realize industrialized production.

Description

technical field [0001] The invention relates to a preparation method of a bismuth compound, in particular to a preparation method of bismuth subsalicylate. Background technique [0002] Bismuth subsalicylate is used in the treatment of syphilis and also in the treatment of flat warts. The traditional method for producing bismuth subsalicylate is mainly to add 30% ammonia water to bismuth nitrate solution to hydrolyze it into bismuth hydroxide, filter and wash with water, then condense with salicylic acid to generate bismuth subsalicylate. NO in bismuth subsalicylate produced by traditional methods 3 - Difficult to wash off. [0003] The Chinese Invention Patent Application Publication No. CN101041617A published on September 26, 2007 discloses a method for producing bismuth citrate, bismuth oxalate and bismuth subsalicylate by electrolytically activating metal bismuth. In this method, ultrafine bismuth with a particle size in the range of 20-350nm is first produced by ele...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C65/10C07C51/41
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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