CN102690192A - Bismuth citrate synthesizing method - Google Patents
Bismuth citrate synthesizing method Download PDFInfo
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- CN102690192A CN102690192A CN2012102100575A CN201210210057A CN102690192A CN 102690192 A CN102690192 A CN 102690192A CN 2012102100575 A CN2012102100575 A CN 2012102100575A CN 201210210057 A CN201210210057 A CN 201210210057A CN 102690192 A CN102690192 A CN 102690192A
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- bismuth
- bismuth citrate
- citric acid
- water
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Abstract
The invention belongs to the technical field of complexe synthesis, and specifically relates to a bismuth citrate synthesizing method. The bismuth citrate synthesizing method comprises the following steps: dissolving a citric acid in water at a temperature of 45-48 DEG C; then adding bismuth oxide into the obtained mixture, and uniformly mixing the obtained product; carrying out atmospheric reaction on the obtained product for 20-24 hours at a temperature of 80-85 DEG C; and filtering, washing and drying the obtained reaction product so as to obtain white powdered solids, namely, bismuth citrate, wherein the molar ratio of the bismuth oxide to the citric acid to the water is 1:(3.5-4):(18-20). The method is performed under atmospheric pressure and low temperature conditions, the reaction conditions are mild, meanwhile, the product yield is high, and the quality of products is good.
Description
Technical field
The invention belongs to the coordination compound synthesis technical field, be specifically related to a kind of compound method of bismuth citrate.
Background technology
Bismuth citrate, molecular formula BiC
6H
5O
7, molecular weight 398, chemical structural formula is as follows, and it is a kind of wide-spectrum bactericide pharmaceutically commonly used, has characteristics such as toxicity is low.It has certain biological activity, and the medicine of participating in many treatment intestinal tract diseases is synthetic.
The compound method of bismuth citrate has many research reports, and mainly contain: 1) traditional technology method-sxemiquantitative ammonia dissolves method.The method that its adopts mainly is that the subnitrate of bismuth adds the Citric Acid preparation and gets.It is mixed with nitrate ion in product, product toxicity is big; And the production of by product nitric acid is arranged, big for environment pollution.2) Chinese patent CN200510111884.9 discloses the method for the synthetic bismuth citrate of a kind of hydro-thermal, and it is synthetic through hot water with bismuth oxide and Citric Acid.But early stage need bismuth oxide and Citric Acid thorough mixing is even in reaction, strengthened work load like this, be unfavorable for scale operation.In addition, in reaction process, need reaction under high pressure, have serious potential safety hazard, and last generation filtrating is not carried out handled, environment is worked the mischief.
Summary of the invention
The object of the invention is to overcome the prior art deficiency, and a kind of novel bismuth citrate compound method of under normal pressure, low temperature, carrying out is provided.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
A kind of bismuth citrate compound method, it may further comprise the steps:
Citric Acid is dissolved in 45～48 ℃ the water; Add bismuth oxide then, (the concrete available ammoniacal liquor of reaction end detected: get reaction solution, to the ammoniacal liquor that wherein drips mass concentration 25～28% in 20～24 hours in 80～85 ℃, synthesis under normal pressure behind the mixing; If there is not deposition; Explain and react completely), reaction product gets the white powder solid through aftertreatment (filter, wash, dry), is bismuth citrate; Wherein, the mol ratio of bismuth oxide, Citric Acid and water is 1 ︰ (3.5～4) ︰ (18～20).
The building-up reactions equation is following:
Bi
2O
3?+?2C
6H
8O
7?=?2BiC
6H
5O
7?+?3H
2O
The present invention is a raw material with the bismuth oxide, in aqueous solution of citric acid, carries out inorganic coordination chemistry, obtains bismuth citrate.The raw materials used bismuth oxide of the present invention, Citric Acid and water etc. all are the raw materials that obtains easily in the industrial production, and inexpensive, are fit to suitability for industrialized production.In addition, the existing processing condition of reactions step gentle (under normal pressure and coldcondition, carrying out), reaction process safety, reaction is thorough, and impurity is few, and is pollution-free, and most of solvent is recyclable to be utilized again, and product yield is high, and quality is good.
Embodiment
Below technology of the present invention being done further to specify through preferred embodiment, but protection scope of the present invention is not limited thereto.
Embodiment 1
A kind of bismuth citrate compound method, it may further comprise the steps:
It is in 45 ℃ the 324g water that the 672.5g Citric Acid is dissolved in temperature fully; Add the 466g bismuth oxide then, be warming up to 80 ℃ behind the mixing, (ammoniacal liquor with mass concentration 25～28% detected synthesis under normal pressure in 20 hours; There is not deposition); Reaction product through filter, wash, dry 789.6g white powder solid, be bismuth citrate, yield 99.2%.
Embodiment 2
It is in 46 ℃ the 342g water that the 730.1g Citric Acid is dissolved in temperature fully; Add the 466g bismuth oxide then, be warming up to 83 ℃ behind the mixing, (ammoniacal liquor with mass concentration 25～28% detected synthesis under normal pressure in 22 hours; There is not deposition); Reaction product through filter, wash, dry 791.2g white powder solid, be bismuth citrate, yield 99.4%.
Embodiment 3
It is in 48 ℃ the 360g water that the 768.6g Citric Acid is dissolved in temperature fully; Add the 466g bismuth oxide then, be warming up to 85 ℃ behind the mixing, (ammoniacal liquor with mass concentration 25～28% detected synthesis under normal pressure in 24 hours; There is not deposition); Reaction product through filter, wash, dry 790.4g white powder solid, be bismuth citrate, yield 99.3%.
Embodiment 4
It is in 48 ℃ the 360g water that the 672.5g Citric Acid is dissolved in temperature fully; Add the 466g bismuth oxide then, be warming up to 85 ℃ behind the mixing, (ammoniacal liquor with mass concentration 25～28% detected synthesis under normal pressure in 24 hours; There is not deposition); Reaction product through filter, wash, dry 792.0g white powder solid, be bismuth citrate, yield 99.5%.
Embodiment 5
It is in 45 ℃ the 324g water that the 768.6g Citric Acid is dissolved in temperature fully; Add the 466g bismuth oxide then, be warming up to 80 ℃ behind the mixing, (ammoniacal liquor with mass concentration 25～28% detected synthesis under normal pressure in 20 hours; There is not deposition); Reaction product through filter, wash, dry 790.8g white powder solid, be bismuth citrate, yield 99.3%.
White powder solid to the synthetic gained of above-mentioned each embodiment carries out ultimate analysis, and the result is: carbon 18.15%, hydrogen 1.22%, bismuth 52.3%.This result and theoretical value (BiC
6H
5O
7): carbon 18.10%, hydrogen 1.27%, bismuth 52.5% basically identical.
Claims (1)
1. a bismuth citrate compound method is characterized in that, may further comprise the steps:
Citric Acid is dissolved in 45～48 ℃ the water, adds bismuth oxide then, in 80～85 ℃, synthesis under normal pressure 20～24 hours, reaction product got the white powder solid through aftertreatment, is bismuth citrate behind the mixing; Wherein, the mol ratio of bismuth oxide, Citric Acid and water is 1 ︰ (3.5～4) ︰ (18～20).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102100575A CN102690192A (en) | 2012-06-25 | 2012-06-25 | Bismuth citrate synthesizing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102100575A CN102690192A (en) | 2012-06-25 | 2012-06-25 | Bismuth citrate synthesizing method |
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|---|---|
| CN102690192A true CN102690192A (en) | 2012-09-26 |
Family
ID=46855947
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| CN2012102100575A Pending CN102690192A (en) | 2012-06-25 | 2012-06-25 | Bismuth citrate synthesizing method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2012
- 2012-06-25 CN CN2012102100575A patent/CN102690192A/en active Pending
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: "柠檬酸铋的热分解机理、非等温反应动力学及其对双基推进剂燃烧的催化作用", 《高等学校化学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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Application publication date: 20120926 |