CN103172510A - Preparation method of bismuth citrate - Google Patents
Preparation method of bismuth citrate Download PDFInfo
- Publication number
- CN103172510A CN103172510A CN2011104318382A CN201110431838A CN103172510A CN 103172510 A CN103172510 A CN 103172510A CN 2011104318382 A CN2011104318382 A CN 2011104318382A CN 201110431838 A CN201110431838 A CN 201110431838A CN 103172510 A CN103172510 A CN 103172510A
- Authority
- CN
- China
- Prior art keywords
- citric acid
- preparation
- bismuth
- bismuth citrate
- acid solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a preparation method of bismuth citrate, which comprises the following steps: crushing bismuth oxide to a specified average particle size; step two, preparing a citric acid aqueous solution with a preset concentration and heating the citric acid aqueous solution to a preset temperature lower than the boiling point of water; step three, according to the chemical reaction equation Bi2O3+2C6H8O7＝2C6H5BiO7+3H2O maintaining an initial excess coefficient of citric acid in the aqueous citric acid solution below 1, gradually adding the pulverized bismuth oxide to the heated aqueous citric acid solution to react the citric acid with the bismuth oxide; gradually adding citric acid aqueous solution with another concentration along with the reaction to keep the initial liquid-solid ratio; and step five, after the reaction is finished, filtering and drying to obtain the bismuth citrate product. The preparation method of the bismuth citrate has no special requirements on equipment, is easy to realize industrial production, has simple process, is convenient to operate and control, and has high yield and less impurities.
Description
Technical field
The present invention relates to a kind of preparation method of bismuth compound, relate in particular to a kind of preparation method of bismuth citrate.
Background technology
Bismuth citrate (claiming again bismuth citrate) is treatment stomach trouble, the intermediate of anti-ulcerative drug.Be used for the treatment of stomach ulcer, duodenal ulcer, complex ulcer, multiple ulcers and stoma ulcer.And be used for chronic superficial gastritis and with the treatment of Helicobacter pylori infection.The method of traditional mode of production bismuth citrate is mainly to add citric acid reactions to generate product in bismuth nitrate solution or the pH value of regulating Bismuth trinitrate generates after bismuth hydroxide and citric acid reactions generation product it.NO in the bismuth citrate of produced in conventional processes
3 -Higher.
Disclosed Chinese patent application publication number CN1793101A disclosed a kind of method of Hydrothermal Synthesis bismuth citrate on June 28th, 2006, it adopts bismuth oxide and citric acid to be ground and puts into autoclave, then autoclave is placed in baking oven 100～150 ℃ of constant temperature 1～12 hour, washing and drying obtains bismuth citrate.This method need to be carried out in hyperbaric environment, and is higher to equipment requirements, and autoclave need put into baking oven, is unfavorable for scale operation.
Disclosed Chinese invention patent application publication number CN101041617A disclosed a kind of method that electrolyzing active metal bismuth is produced bismuth citrate on September 26th, 2007.Then this method makes it directly and citric acid reactions generation bismuth citrate at first by the ultra-fine bismuth of electrolysis production particle diameter in 20～350nm scope.The condition of this method electrolysis production superfine metal bismuth is harsh, and ultra-fine bismuth is very easily oxidized, is not suitable for industrial production.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of preparation method of bismuth citrate, the requirement that it can reduce equipment is easy to realize suitability for industrialized production.
Another object of the present invention is to a kind of preparation method of bismuth citrate, it can reduce preparation condition, and convenient operation is controlled.
In order to realize above-mentioned purpose of the present invention, the invention provides a kind of preparation method of bismuth citrate, comprise step: step 1 is crushed to the regulation median size with bismuth oxide; Step 2, the aqueous citric acid solution of preparation predetermined concentration also is heated to preset temperature lower than water boiling point; Step 3 is according to chemical equation Bi
2O
3+ 2C
6H
8O
7=2C
6H
5BiO
7+ 3H
2O makes the initial excess coefficient of the citric acid in aqueous citric acid solution remain on below 1, the bismuth oxide of pulverizing is progressively added in the aqueous citric acid solution of described heating, so that citric acid and bismuth oxide react; Step 4 along with the carrying out of reaction, is progressively added the aqueous citric acid solution of another concentration, to keep initial liquid-solid ratio; Step 5, reaction is filtered and is dried after finishing, and namely obtains the bismuth citrate goods.
Beneficial effect of the present invention is as follows.
The preparation method of bismuth citrate of the present invention to equipment without particular requirement and be easy to realize suitability for industrialized production.
Simple and the convenient operation of preparation method's preparation flow of bismuth citrate of the present invention is controlled.
The preparation method of bismuth citrate of the present invention very easily realizes suitability for industrialized production.
The productive rate of the bismuth citrate that the preparation method of bismuth citrate of the present invention obtains is high, impurity is few.
Embodiment
The below describes the preparation method according to bismuth citrate of the present invention in detail.
Preparation method according to bismuth citrate of the present invention comprises step: step 1 is crushed to the regulation median size with bismuth oxide; Step 2, the aqueous citric acid solution of preparation predetermined concentration also is heated to preset temperature lower than water boiling point; Step 3 is according to chemical equation Bi
2O
3+ 2C
6H
8O
7=2C
6H
5BiO
7+ 3H
2O makes the initial excess coefficient of the citric acid in aqueous citric acid solution remain on below 1,, the bismuth oxide of pulverizing is progressively added in the aqueous citric acid solution of described heating, so that citric acid and bismuth oxide react; Step 4 along with the carrying out of reaction, is progressively added the aqueous citric acid solution of another concentration, to keep initial liquid-solid ratio; Step 5, reaction is filtered and is dried after finishing, and namely obtains the bismuth citrate goods.
Wherein, the initial excess coefficient of citric acid refer to add on the basis of the amount of the citric acid required according to the chemical equation theory of computation into the mole number of citric acid; Initial liquid-solid ratio refers to liquid before bismuth oxide and citric acid solution reaction and the mass ratio of solid.
In the preparation method according to bismuth citrate of the present invention, preferably, in step 1, the median size of described bismuth oxide is 0.1～0.5 μ m.
In the preparation method according to bismuth citrate of the present invention, preferably, in step 2, the predetermined concentration of aqueous citric acid solution is 200～500g/L.
In the preparation method according to bismuth citrate of the present invention, preferably, in step 2, preset temperature is 60～90 ℃.
In the preparation method according to bismuth citrate of the present invention, preferably, in step 3, initial excess coefficient is 0.3～1.
In the preparation method according to bismuth citrate of the present invention, preferably, in step 3, when the bismuth oxide that will pulverize progressively adds in the aqueous citric acid solution of described heating, be added with stirring.Preferably, stirring velocity is 250～300rpm.Preferably, churning time is 28～48h.
In the preparation method according to bismuth citrate of the present invention, preferably, in step 4, the concentration of the described aqueous citric acid solution of adding another concentration of adding is 50～200g/L.
In the preparation method according to bismuth citrate of the present invention, preferably, in step 4, the viscosity of the aqueous citric acid solution before the aqueous citric acid solution of progressively adding another concentration is added by real-time measurement is carried out.
In the preparation method according to bismuth citrate of the present invention, preferably, in step 5, bake out temperature is 60 ℃.
Next provides the preparation method's of bismuth citrate of the present invention embodiment.
Embodiment 1
Step 1, it is 0.1 μ m that bismuth oxide is crushed to median size.The broken test-type micronizer mill that adopts Shanghai Sai Shan powder machinery Manufacturing Co., Ltd to produce.
Step 2, configuration 200mL concentration is the aqueous citric acid solution of 200g/L, and is heated to 60 ℃.
Step 3, the initial excess coefficient of controlling citric acid is 0.3, takes the bismuth oxide particle of 43.7g pulverizing and will progressively join in the aqueous citric acid solution of step 2 stirring reaction 28h.
Step 4 in reaction process, according to the toughness of reaction soln, is progressively added the aqueous citric acid solution of 200g/L and is kept the initial liquid-solid ratio of reaction.
Step 5, reaction finish to use ultrapure water filtration washing product bismuth citrate to filter cake pH=5～7, and in vacuum drying oven, 60 ℃ of oven dry filter cakes, obtain white powder bismuth citrate product.
Adopt the EDTA complexometric titration to detect and analyze the product that obtains, bi content is 53.07%.The quality of qualified product is 66.44g, and ratio defective product is 89% (ratio defective product calculates with the amount of the bismuth oxide that adds, is the ratio of product actual output and theoretical yield).
Embodiment 2
Step 1, it is 0.2 μ m that bismuth oxide is crushed to median size.The broken test-type micronizer mill that adopts Shanghai Sai Shan powder machinery Manufacturing Co., Ltd to produce.
Step 2, configuration 200mL concentration is the aqueous citric acid solution of 300g/L, and is heated to 70 ℃.
Step 3, the initial excess coefficient of controlling citric acid is 0.5, takes the bismuth oxide particle of 56.83g pulverizing and will progressively join in the aqueous citric acid solution of step 2 stirring reaction 36h.
Step 4 in reaction process, according to the toughness of reaction soln, is progressively added the aqueous citric acid solution of 150g/L and is kept the initial liquid-solid ratio of reaction.
Step 5, reaction finish to use ultrapure water filtration washing product bismuth citrate to filter cake pH=5～7, and in vacuum drying oven, 60 ℃ of oven dry filter cakes, obtain white powder bismuth citrate product.
Adopt the EDTA complexometric titration to detect and analyze the product that obtains, bi content is 52.8%.The quality of qualified product is 88.34g, calculates with the amount of the bismuth oxide that adds, and ratio defective product is 91%.
Embodiment 3
Step 1, it is 0.3 μ m that bismuth oxide is crushed to median size.The broken test-type micronizer mill that adopts Shanghai Sai Shan powder machinery Manufacturing Co., Ltd to produce.
Step 2, configuration 200mL concentration is the aqueous citric acid solution of 400g/L, and is heated to 80 ℃.
Step 3, the initial excess coefficient of controlling citric acid is 0.8, takes the bismuth oxide particle of 63.15g pulverizing and will progressively join in the aqueous citric acid solution of step 2 stirring reaction 36h.
Step 4 in reaction process, according to the toughness of reaction soln, is progressively added the aqueous citric acid solution of 100g/L and is kept the initial liquid-solid ratio of reaction.
Step 5, reaction finish to use ultrapure water filtration washing product bismuth citrate to filter cake pH=5～7, and in vacuum drying oven, 60 ℃ of oven dry filter cakes, obtain white powder bismuth citrate product.
Adopt the EDTA complexometric titration to detect and analyze the product that obtains, bi content is 52.63%.The quality of qualified product is 93.85g, calculates with the amount of the bismuth oxide that adds, and ratio defective product is 87%.
Embodiment 4
Step 1, it is 0.5 μ m that bismuth oxide is crushed to median size.The broken test-type micronizer mill that adopts Shanghai Sai Shan powder machinery Manufacturing Co., Ltd to produce.
Step 2, configuration 200mL concentration is the aqueous citric acid solution of 500g/L, and is heated to 90 ℃.
Step 3, the initial excess coefficient of controlling citric acid is 1, takes the bismuth oxide particle of 71g pulverizing and will progressively join in the aqueous citric acid solution of step 2 stirring reaction 48h.
Step 4 in reaction process, according to the toughness of reaction soln, is progressively added the aqueous citric acid solution of 50g/L and is kept the initial liquid-solid ratio of reaction.
Step 5, reaction finish to use ultrapure water filtration washing product bismuth citrate to filter cake pH=5～7, and in vacuum drying oven, 60 ℃ of oven dry filter cakes, obtain white powder bismuth citrate product.
Adopt the EDTA complexometric titration to detect and analyze the product that obtains, bi content is 52.36%.The quality of qualified product is 112.79g, calculates with the amount of the bismuth oxide that adds, and ratio defective product is 93%.
Claims (10)
1. the preparation method of a bismuth citrate, is characterized in that, comprises step:
Step 1 is crushed to the regulation median size with bismuth oxide;
Step 2, the aqueous citric acid solution of preparation predetermined concentration also is heated to preset temperature lower than water boiling point;
Step 3 is according to chemical equation Bi
2O
3+ 2C
6H
8O
7=2C
6H
5BiO
7+ 3H
2O makes the initial excess coefficient of the citric acid in aqueous citric acid solution remain on below 1, the bismuth oxide of pulverizing is progressively added in the aqueous citric acid solution of described heating, so that citric acid and bismuth oxide react;
Step 4 along with the carrying out of reaction, is progressively added the aqueous citric acid solution of another concentration, to keep initial liquid-solid ratio;
Step 5, reaction is filtered and is dried after finishing, and namely obtains the bismuth citrate goods.
2. the preparation method of bismuth citrate according to claim 1, is characterized in that, in step 1, the median size of described bismuth oxide is 0.1～0.5 μ m.
3. the preparation method of bismuth citrate according to claim 1, is characterized in that, in step 2, the predetermined concentration of aqueous citric acid solution is 200～500g/L.
4. the preparation method of bismuth citrate according to claim 1, is characterized in that, in step 2, preset temperature is 60～90 ℃.
5. the preparation method of bismuth citrate according to claim 1, is characterized in that, in step 3, initial excess coefficient is 0.3～1.
6. the preparation method of bismuth citrate according to claim 1, is characterized in that, in step 3, when the bismuth oxide that will pulverize progressively adds in the aqueous citric acid solution of described heating, is added with stirring.
7. the preparation method of bismuth citrate according to claim 6, is characterized in that, in step 3, stirring velocity is 250～300rpm, and churning time is 28～48h.
8. the preparation method of bismuth citrate according to claim 1, is characterized in that, in step 4, the concentration of the described aqueous citric acid solution of adding another concentration of adding is 50～200g/L.
9. the preparation method of bismuth citrate according to claim 1, is characterized in that, in step 4, the viscosity of the aqueous citric acid solution before the aqueous citric acid solution of progressively adding another concentration is added by real-time measurement is carried out.
10. the preparation method of bismuth citrate according to claim 1, is characterized in that, in step 5, bake out temperature is 60 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110431838.2A CN103172510B (en) | 2011-12-20 | 2011-12-20 | Preparation method of bismuth citrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110431838.2A CN103172510B (en) | 2011-12-20 | 2011-12-20 | Preparation method of bismuth citrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103172510A true CN103172510A (en) | 2013-06-26 |
| CN103172510B CN103172510B (en) | 2015-09-30 |
Family
ID=48632778
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110431838.2A Active CN103172510B (en) | 2011-12-20 | 2011-12-20 | Preparation method of bismuth citrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103172510B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864605A (en) * | 2014-03-24 | 2014-06-18 | 清远先导材料有限公司 | Preparation method of bismuth citrate |
| CN110357778A (en) * | 2019-08-02 | 2019-10-22 | 湖南柿竹园有色金属有限责任公司 | A kind of preparation method of bismuth citrate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1793101A (en) * | 2005-12-23 | 2006-06-28 | 华东师范大学 | Process for hydrothermal synthesizing bismuth citrate |
| CN101628735A (en) * | 2009-08-24 | 2010-01-20 | 中南大学 | Method for preparing bismuth-series chemical product |
-
2011
- 2011-12-20 CN CN201110431838.2A patent/CN103172510B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1793101A (en) * | 2005-12-23 | 2006-06-28 | 华东师范大学 | Process for hydrothermal synthesizing bismuth citrate |
| CN101628735A (en) * | 2009-08-24 | 2010-01-20 | 中南大学 | Method for preparing bismuth-series chemical product |
Non-Patent Citations (1)
| Title |
|---|
| 宋秀铎等: "柠檬酸铋的制备、结构表征及其在固体推进剂中的催化作用", 《兵工学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864605A (en) * | 2014-03-24 | 2014-06-18 | 清远先导材料有限公司 | Preparation method of bismuth citrate |
| CN103864605B (en) * | 2014-03-24 | 2015-11-25 | 清远先导材料有限公司 | A kind of preparation method of bismuth citrate |
| CN110357778A (en) * | 2019-08-02 | 2019-10-22 | 湖南柿竹园有色金属有限责任公司 | A kind of preparation method of bismuth citrate |
| CN110357778B (en) * | 2019-08-02 | 2022-02-11 | 湖南柿竹园有色金属有限责任公司 | Preparation method of bismuth citrate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103172510B (en) | 2015-09-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2018024083A1 (en) | Method using highly concentrated vanadium solution for manufacturing ammonium polyvanadate | |
| CN102583575B (en) | Method for producing pigment-level iron oxide red by using titanium dioxide waste residue ferrous sulfate | |
| CN102603000B (en) | Process for preparing high-purity vanadium pentoxide by adopting ammonium metavanadate as raw material | |
| CN102756131B (en) | Preparation method for micro-order platy silver powder | |
| CN101633516A (en) | Preparation method of high-purity cerium hydroxide | |
| CN102079537A (en) | Preparation method of nano zinc oxide and roasting furnace | |
| CN102009967B (en) | Method for preparing iron phosphate with micro/nano structure | |
| CN107055609B (en) | A kind of preparation method of ultra-pure 3Y yttrium stable zirconium oxides | |
| CN100528758C (en) | Method for producing powder in micron order of bismuth oxide | |
| CN103318959A (en) | Production method for sodium pyroantimonate by using high-temperature high-pressure pure-oxygen oxidation | |
| CN102910683A (en) | Production method for synthesizing nanoscale oxide iron red through full-wet method | |
| CN106830051A (en) | A kind of method for preparing nanometer Zinc oxide powder as raw material with industrial zinc oxide | |
| CN103172510B (en) | Preparation method of bismuth citrate | |
| CN101602716B (en) | Synthesis method of 2-chromium picolinate | |
| CN107572588B (en) | A kind of environment-friendly type sodium tungstate preparation process and its application | |
| CN104276594A (en) | Process for preparing nano-zinc oxide by using zinc sulfide concentrate calcined zinc sand | |
| CN101723420B (en) | Method for preparing thermocompressed polycrystalline magnesium fluoride powder | |
| CN103979600A (en) | Preparation method of ultrathin copper oxide powder | |
| CN105753047B (en) | A kind of new method for preparing dental nano zirconium oxide powder | |
| CN103183608B (en) | Preparation method of bismuth subsalicylate | |
| CN104355333B (en) | A kind of preparation method of antimony peroxide composite dry powder | |
| CN105366731A (en) | Preparation method of high quality iron oxide red | |
| CN106219580A (en) | A kind of method preparing basic magnesium carbonate | |
| CN104445349A (en) | Preparation method of Y2O3 superfine powder by virtue of PEG4000 and SDBS compound precipitation | |
| CN113582259B (en) | Liquid ruthenium nitrate synthesis process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20220519 Address after: No. 1116-1, building 1, Dianzhong Business Plaza, Dianzhong new area, Kunming, Yunnan 650212 Patentee after: Kunming forerunner New Material Technology Co.,Ltd. Address before: 511500 Industrial Zone, wo Yun town, Qingxin County, Qingyuan, Guangdong (beside the fish dam road) Patentee before: FIRST RARE MATERIALS Co.,Ltd. |