CN107963967A - The method for synthesizing Bismuth Potassium Citrate - Google Patents
The method for synthesizing Bismuth Potassium Citrate Download PDFInfo
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- CN107963967A CN107963967A CN201711459599.5A CN201711459599A CN107963967A CN 107963967 A CN107963967 A CN 107963967A CN 201711459599 A CN201711459599 A CN 201711459599A CN 107963967 A CN107963967 A CN 107963967A
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- bismuth
- citrate
- potassium citrate
- potassium
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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Abstract
The application provides a kind of method for synthesizing Bismuth Potassium Citrate, it includes step：Prepare potassium citrate solution；Deionized water is added into reaction kettle under stirring, ammonium hydroxide is added afterwards or ammonia is passed through into deionized water, bismuth citrate to bismuth citrate is then added and is completely dissolved, obtain bismuth citrate ammonium salt solution；Lasting stirring simultaneously will be such that potassium citrate is reacted with bismuth and ammonium citrate in potassium citrate solution addition reaction kettle, spray-dried after reaction to obtain Bismuth Potassium Citrate.The synthetic method craft flow of the application is simple, low raw-material cost, reaction condition are gentle, is appropriate for producing in enormous quantities.
Description
Technical field
This application involves pharmaceutical synthesis field, more particularly to a kind of method for synthesizing Bismuth Potassium Citrate.
Background technology
Bismuth Potassium Citrate is a kind of compound of bismuth-containing, and its preparation method, which is typically necessary, to be prepared among bismuth subnitrate
Body, technique is more complicated and cost is higher, and Synthesis liquid generally requires to be concentrated by evaporation in preparation process, then with ethyl alcohol recrystallization, washing,
It is dry, obtain product.The applying date discloses the above method in August, 2016 Chinese patent application of 3 days 201610632889.4.
But there are such Railway Project for ethyl alcohol recrystallization method：Rate of deposition of the cocnentration factor to bismuth, the bi content shadow to product in concentration process
Sound is larger, is difficult to control product specification；Ethyl alcohol recrystallization and washing process can reduce yield, and the consuming time is more, and efficiency is low, and
And product cut size not easy to control；A large amount of productions also need to consider ethanol Explosion-Proof；Ethanol demand is more, and cost is higher.Therefore should
Method is not suitable for producing in enormous quantities.
In consideration of it, special propose the application.
The content of the invention
In view of problem present in background technology, the purpose of the application is to provide a kind of side for synthesizing Bismuth Potassium Citrate
Method, the synthetic method craft flow is simple, low raw-material cost, reaction condition are gentle, is appropriate for producing in enormous quantities.
In order to achieve the above object, in the one side of the application, this application provides a kind of side for synthesizing Bismuth Potassium Citrate
Method, it includes step；Prepare potassium citrate solution；Deionized water is added into reaction kettle under stirring, adds ammonia afterwards
Water is passed through ammonia into deionized water, then adds bismuth citrate to bismuth citrate and is completely dissolved, it is molten to obtain bismuth and ammonium citrate
Liquid；Lasting stirring simultaneously will be such that potassium citrate is reacted with bismuth and ammonium citrate in potassium citrate solution addition reaction kettle, after reaction
It is spray-dried to obtain Bismuth Potassium Citrate.
Relative to the prior art, the application includes at least beneficial effect as described below：
The method technological process of the synthesis Bismuth Potassium Citrate of the application is simple, low raw-material cost, reaction condition are gentle, suitable
Conjunction is produced in enormous quantities.
The Bismuth Potassium Citrate quality that is obtained by the synthetic method of the application is loose, uniform particle diameter, yield are higher.
The Bismuth Potassium Citrate obtained by the synthetic method of the application also has preferable water solubility, facilitates absorption of human body,
Drug effect is set faster to play.
Embodiment
The following detailed description of the method for the synthesis Bismuth Potassium Citrate according to the application.
Step is included according to the method for the synthesis Bismuth Potassium Citrate of the application：S1, prepares potassium citrate solution；S2, is being stirred
Mix and add deionized water under state into reaction kettle, add ammonium hydroxide afterwards or ammonia is passed through into deionized water, then add lemon
Lemon acid bismuth to bismuth citrate is completely dissolved, and obtains bismuth citrate ammonium salt solution；S3, lasting stirring simultaneously add potassium citrate solution anti-
Answering makes potassium citrate be reacted with bismuth and ammonium citrate in kettle, spray-dried after reaction to obtain Bismuth Potassium Citrate.
In the synthetic method of the application, by potassium citrate solution and bismuth citrate ammonium salt solution processed respectively, then by two
Solution hybrid reaction is planted, then spray-dried method obtains Bismuth Potassium Citrate, and the synthetic method is without pass through preparation time
Bismuth nitrate intermediate and it the processes such as heating concentration, ethyl alcohol recrystallization washing be dry need not be carried out can obtain Bismuth Potassium Citrate, because
This technological process is simple, low raw-material cost, at the same the synthesising method reacting condition is gentle, heat production easy to control, be adapted into
Row is produced in enormous quantities.
In the synthetic method of the application, citron that is dry and making can be completed with moment by way of spray drying
Sour bismuth potassium quality is loose, uniform particle diameter, yield are higher.
The Bismuth Potassium Citrate obtained by the synthetic method of the application also has preferable water solubility, facilitates absorption of human body,
Drug effect is set faster to play.
In the synthetic method of the application, in step S1, potassium citrate solution can be by being dissolved in deionization by potassium citrate
Obtained in water；Also can react to obtain by citric acid and potassium carbonate, saleratus or potassium hydroxide.Preferably, potassium carbonate, carbonic acid
The molar ratio of potassium ion and citric acid is 3 in hydrogen potassium or potassium hydroxide:1~3.2:1, slightly excessive potassium carbonate, saleratus or
Potassium hydroxide can be used for potassium citrate and the pH value of bismuth and ammonium citrate reaction in regulating step S3.Preferably, citric acid and carbon
The reaction time of sour potassium, saleratus or potassium hydroxide is 10min~30min.
In the synthetic method of the application, in step S2, it is preferable that bismuth citrate can be added portionwise.
In the synthetic method of the application, in step S2, it is preferable that the molar ratio of ammonium hydroxide or ammonia and bismuth citrate is
1.3:1~3.3:1.
In the synthetic method of the application, in step S2, it is preferable that stop when the bismuth citrate of addition is completely dissolved to
Ammonia is passed through in deionized water, it is cost-effective to avoid ammonia is wasted.
In the synthetic method of the application, in step S3, it is preferable that the molar ratio of bismuth and ammonium citrate and potassium citrate is
1.5:1~2.7:1.
In the synthetic method of the application, in step S3, it is preferable that reaction temperature is 50 DEG C~90 DEG C, further preferably
Ground, reaction temperature are 65 DEG C~90 DEG C.
In the synthetic method of the application, in step S3, it is preferable that the reaction time is 20min~60min.
In the synthetic method of the application, in step S3, the temperature of spray drying is 150 DEG C~200 DEG C.
In the synthetic method of the application, in step S3, it is preferable that pH value when potassium citrate is reacted with bismuth and ammonium citrate
Control as 6~8.
With reference to embodiment, the application is expanded on further.It is to be understood that these embodiments be merely to illustrate the application without
For limiting scope of the present application.
Embodiment 1
Weigh 40mL deionized waters to be placed in beaker, room temperature opens stirring, adds 16.8g Citric Acid Monos, adds
16.2g potassium hydroxide, stirs 10min, obtains potassium citrate solution.Weigh 80mL deionized waters to be placed in flask, while stirring
Into flask, addition 30mL, concentration are 25% ammonium hydroxide, then 72.7g bismuth citrates are added portionwise, and stirring is until bismuth citrate is complete
Fully dissolved, obtains bismuth citrate ammonium salt solution.Heating-up temperature is set as 55 DEG C, adds lemon into bismuth citrate ammonium salt solution while stirring
Lemon acid potassium solution, stirring stop heating and stirring after reacting 30min, are then spray-dried at 150 DEG C, obtain bismuth citrate
Potassium, is computed learning, the yield of Bismuth Potassium Citrate is 96.7%.
Embodiment 2
Weigh 40mL deionized waters to be placed in beaker, room temperature opens stirring, adds 16.8g Citric Acid Monos, adds
16.2g potassium hydroxide, stirs 20min, obtains potassium citrate solution.Weigh 120mL deionized waters to be placed in flask, while stirring
Into flask, addition 26mL, concentration are 25% ammonium hydroxide, then 65g bismuth citrates are added portionwise, and stirring is until bismuth citrate is complete
Dissolving, obtains bismuth citrate ammonium salt solution.90 DEG C of heating-up temperature is set, adds citric acid into bismuth citrate ammonium salt solution while stirring
Potassium solution, stirring stop heating and stirring after reacting 30min, are then spray-dried at 180 DEG C, obtain Bismuth Potassium Citrate,
It is computed learning, the yield of Bismuth Potassium Citrate is 97.4%.
Embodiment 3
Weigh 50mL deionized waters to be placed in beaker, room temperature opens stirring, adds 26.1g Citric Acid Mono potassium, stirring
15min, obtains potassium citrate solution.100mL deionized waters are weighed to be placed in beaker, while stirring into flask add 26mL,
Concentration is 25% ammonium hydroxide, then 65g bismuth citrates are added portionwise, and stirring is completely dissolved up to bismuth citrate, obtains bismuth citrate
Ammonium salt solution.75 DEG C of heating-up temperature is set, adds potassium citrate solution, stirring reaction into bismuth citrate ammonium salt solution while stirring
Stop heating and stirring after 30min, be then spray-dried at 160 DEG C, obtain Bismuth Potassium Citrate, be computed learning, citron
The yield of sour bismuth potassium is 96.9%.
Comparative example 1
Weigh 40mL deionized waters to be placed in beaker, room temperature opens stirring, adds 16.8g Citric Acid Monos, adds
16.2g potassium hydroxide, stirs 20min, obtains potassium citrate solution.Weigh 120mL deionized waters to be placed in flask, while stirring
Into flask, addition 26mL, concentration are 25% ammonium hydroxide, then 65g bismuth citrates are added portionwise, and stirring is until bismuth citrate is complete
Dissolving, obtains bismuth citrate ammonium salt solution.90 DEG C of heating-up temperature is set, adds citric acid into bismuth citrate ammonium salt solution while stirring
Potassium solution, stirring stop heating and stirring after reacting 30min, bismuth citrate potassium solution are obtained, then by bismuth citrate potassium solution
It is concentrated by evaporation at 180 DEG C, the time is about 1h, 100mL absolute ethyl alcohols is added after concentration, stirring is to there are a large amount of white solids
Separate out, then solid is filtered and is washed repeatedly with absolute ethyl alcohol, is then dried in vacuo under 70 degrees Celsius, obtains bismuth citrate
Potassium, is computed learning, the yield of Bismuth Potassium Citrate is 83.4%.
The performance test results of 1 embodiment 1 of table
The performance test results of 2 embodiment 2 of table
The performance test results of 3 embodiment 3 of table
The performance test results of 4 embodiment 2 of table and comparative example 1
It was found from the analysis of the performance test results of embodiment 1-3 and comparative example 1, pass through the citron of the present processes synthesis
Sour bismuth potassium meets higher, the simultaneously synthesizing Bismuth Potassium Citrate of Chinese Pharmacopoeia 2015 editions performance requirements and yield to Bismuth Potassium Citrate
Also have the advantages that quality is loose, good water solubility.
Claims (10)
- A kind of 1. method for synthesizing Bismuth Potassium Citrate, it is characterised in that including step：S1, prepares potassium citrate solution；S2, adds deionized water under stirring into reaction kettle, adds ammonium hydroxide afterwards or ammonia is passed through into deionized water, Then add bismuth citrate to bismuth citrate to be completely dissolved, obtain bismuth citrate ammonium salt solution；S3, lasting stirring simultaneously will be such that potassium citrate is reacted with bismuth and ammonium citrate in potassium citrate solution addition reaction kettle, reaction knot Shu Houjing is spray-dried to obtain Bismuth Potassium Citrate.
- 2. the method for synthesis Bismuth Potassium Citrate according to claim 1, it is characterised in that in step S2, ammonium hydroxide or ammonia Molar ratio with bismuth citrate is 1.3:1~3.3:1.
- 3. the method for synthesis Bismuth Potassium Citrate according to claim 1, it is characterised in that in step S3, bismuth and ammonium citrate Molar ratio with potassium citrate is 1.5:1~2.7:1.
- 4. the method for synthesis Bismuth Potassium Citrate according to claim 1, it is characterised in that in step S3, reaction temperature is 50 DEG C~90 DEG C.
- 5. the method for synthesis Bismuth Potassium Citrate according to claim 4, it is characterised in that in step S3, reaction temperature is 65 DEG C~90 DEG C.
- 6. the method for synthesis Bismuth Potassium Citrate according to claim 1, it is characterised in that in step S1, potassium citrate is molten Liquid is obtained by the way that potassium citrate is dissolved in deionized water.
- 7. the method for synthesis Bismuth Potassium Citrate according to claim 1, it is characterised in that in step S1, potassium citrate is molten Liquid reacts to obtain by citric acid and potassium carbonate, saleratus or potassium hydroxide.
- 8. the method for synthesis Bismuth Potassium Citrate according to claim 7, it is characterised in that potassium carbonate, saleratus or hydrogen The molar ratio of potassium ion and citric acid is 3 in potassium oxide:1~3.2:1.
- 9. it is according to claim 1 synthesis Bismuth Potassium Citrate method, it is characterised in that in step S3, potassium citrate with PH value control when bismuth and ammonium citrate reacts is 6~8.
- 10. the method for synthesis Bismuth Potassium Citrate according to claim 1, it is characterised in that in step S3, spray drying Temperature is 150 DEG C~200 DEG C.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4626424A (en) * | 1985-05-28 | 1986-12-02 | Gte Products Corporation | Method of producing crystalline ammonium metatungstate |
| CN105646188A (en) * | 2016-03-15 | 2016-06-08 | 西陇科学股份有限公司 | Production method of medicinal grade bismuth potassium citrate |
| CN106278870A (en) * | 2016-08-03 | 2017-01-04 | 广东先导稀材股份有限公司 | A kind of preparation method of bismuth potassium citrate |
-
2017
- 2017-12-28 CN CN201711459599.5A patent/CN107963967A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4626424A (en) * | 1985-05-28 | 1986-12-02 | Gte Products Corporation | Method of producing crystalline ammonium metatungstate |
| CN105646188A (en) * | 2016-03-15 | 2016-06-08 | 西陇科学股份有限公司 | Production method of medicinal grade bismuth potassium citrate |
| CN106278870A (en) * | 2016-08-03 | 2017-01-04 | 广东先导稀材股份有限公司 | A kind of preparation method of bismuth potassium citrate |
Non-Patent Citations (1)
| Title |
|---|
| 邵冠儒: "温度对枸橼酸铋钾合成中的影响", 《数理医药学杂志》 * |
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Application publication date: 20180427 |