CN106278870A - A kind of preparation method of bismuth potassium citrate - Google Patents
A kind of preparation method of bismuth potassium citrate Download PDFInfo
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- CN106278870A CN106278870A CN201610632889.4A CN201610632889A CN106278870A CN 106278870 A CN106278870 A CN 106278870A CN 201610632889 A CN201610632889 A CN 201610632889A CN 106278870 A CN106278870 A CN 106278870A
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- bismuth
- citrate
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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 present invention provides the preparation method of a kind of bismuth potassium citrate, comprises the following steps: A) potassium hydroxide and citric acid are mixed in water, react, obtain potassium citrate；B) bismuth citrate, ammonia are mixed with described potassium citrate, react, obtain bismuth potassium citrate.Preparation method in the present invention uses bismuth citrate and citric acid, potassium hydroxide one-step synthesis bismuth potassium citrate, it is not necessary to prepare intermediate bismuth subnitrate, and technique is simple, does not use spray drying, and low cost.Further, the bismuth potassium citrate prepared in the present invention is consistent with the product standard of " Chinese Pharmacopoeia ", applied range, and productivity is 80～90%, and purity is 99.95～99.99%.Further, the present invention is using ethanol as the solvent of crystallization, and crystallization time is short, has saved the time of post processing greatly, has further saved cost.
Description
Technical field
The invention belongs to technical field of medicine synthesis, particularly relate to the preparation method of a kind of bismuth potassium citrate.
Background technology
Bismuth metal is one of the safest green metal that the world today generally acknowledges, is widely used in pharmaceutical industry.China is bismuth
The country that resource is the abundantest, commercial reserves and prospective reserves all rank first in the world, and the production for China's bismuth creates advantage.
Along with deepening continuously and the continuous reinforcement of people's environmental consciousness of the research of bismuth deep processed product and application, bismuth chemical products
Application prospect will be more wide.
It is a kind of to form indefinite bismuth-containing complex that bismuth potassium citrate has another name called bismuth potassium citrate potassium, for white powder,
Salty in the mouth, has and draws moist, easily dissolve, in ethanol slightly soluble in water.Bismuth potassium citrate be treatment gastric ulcer and duodenum burst
The good medicine of infections is it can also be used to complex ulcer, multiple ulcers, oral ulcer and erosive gastritis etc., and can kill H. pylori
Bacterium, be a kind of good gastric mucosa protective agent and its be highly soluble in water, be the novel stomach medicine praised highly of international the world of medicine.
The domestic synthesis about bismuth potassium citrate is reported seldom, in the synthesis report of external existing bismuth potassium citrate, all
Need to prepare intermediate bismuth subnitrate and participate in reaction, and product is required for being spray-dried, complex process, relatively costly.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of bismuth potassium citrate, the preparation method operation letter in the present invention
Single, and cost is relatively low.
The present invention provides the preparation method of a kind of bismuth potassium citrate, comprises the following steps:
A) potassium hydroxide and citric acid are mixed in water, react, obtain potassium citrate；
B) bismuth citrate, ammonia are mixed with described potassium citrate, react, obtain bismuth potassium citrate.
Preferably, described step A) in mixed solution, the molar concentration of potassium hydroxide is 11～13mol/L.
Preferably, the mol ratio of described citric acid and potassium hydroxide is 1:(2～4).
Preferably, described step A) in reaction temperature be 20～30 DEG C；
Described step A) in reaction time be 0.5～1 hour.
Preferably, described step B) in the mass concentration of ammonia be 25～28%.
Preferably, described step B) in bismuth citrate, the mol ratio of ammonia and potassium citrate be (2.0～2.5): (1.0～
1.5): 1.
Preferably, described step B) in reaction temperature be 40～60 DEG C；
Described step B) in reaction time be 20～40min.
Preferably, described step B) the most further comprising the steps of:
By step B) mixed solution that obtains is evaporated concentrating and recrystallization successively after reaction, obtains bismuth potassium citrate.
Preferably, the solvent of described recrystallization is ethanol.
Preferably, the time of described recrystallization is 0.5～2 hour.
The present invention provides the preparation method of a kind of bismuth potassium citrate, comprises the following steps: A) by potassium hydroxide and citric acid
Water mixes, reacts, obtain potassium citrate；B) bismuth citrate, ammonia are mixed with described potassium citrate, carry out anti-
Should, obtain bismuth potassium citrate.Preparation method in the present invention uses bismuth citrate and citric acid, potassium hydroxide one-step synthesis Chinese holly
Rafter acid bismuth potassium, it is not necessary to prepare intermediate bismuth subnitrate, technique is simple, does not use spray drying, and low cost.Further, this
The bismuth potassium citrate prepared in bright is consistent with the product standard of " Chinese Pharmacopoeia ", applied range, and productivity is 80～90%, pure
Degree is 99.95～99.99%.
Further, the present invention using ethanol as crystallization solvent, crystallization time is short, saved greatly post processing time
Between, further save cost.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
In having technology to describe, the required accompanying drawing used is briefly described, it should be apparent that, the accompanying drawing in describing below is only this
Inventive embodiment, for those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to according to
The accompanying drawing provided obtains other accompanying drawing.
Fig. 1 is preparation flow schematic diagram of the present invention.
Detailed description of the invention
The invention provides the preparation method of a kind of bismuth potassium citrate, including:
A) potassium hydroxide and citric acid are mixed in water, react, obtain potassium citrate；
B) bismuth citrate, ammonia are mixed with described potassium citrate, react, obtain bismuth potassium citrate.
Preparation method technique in the present invention is simple, and low cost.
It is preparation flow schematic diagram of the present invention that the flow process of preparation sees Fig. 1, Fig. 1.
Potassium hydroxide and citric acid are mixed in water by the present invention, react, and obtain potassium citrate, and the present invention is the most first
Potassium hydroxide is dissolved in water, is subsequently adding citric acid, react, obtain potassium citrate.In the present invention, described Fructus Citri Limoniae
The mol ratio of acid and potassium hydroxide is preferably 1:(2～4), more preferably 1:(2.5～3.5), most preferably 1:(3～3.2)；This
Invention preferably employs monohydrate potassium and reacts with potassium hydroxide, in the present invention, and the mixing obtained after adding citric acid
In solution, the molar concentration of potassium hydroxide is preferably 1～3mol/L, more preferably 1.5～2.5mol/L, most preferably 2mol/
L.In the present invention, the reaction of potassium hydroxide and citric acid is acid-base neutralization reaction, and the temperature of described reaction is preferably 20～35
DEG C, more preferably 25～30 DEG C, the time of described reaction is preferably 30～50min, more preferably 35～45min.
After completing the reaction of above-mentioned acid-base neutralization, obtain is potassium citrate aqueous solution, and the present invention is preferably added to bismuth citrate,
Then add ammonia all to dissolve to bismuth citrate, react, obtain bismuth potassium citrate.In the present invention, described ammonia
Concentration be preferably 25～28%；The mol ratio of described bismuth citrate, ammonia and potassium citrate is preferably (2.0～2.5): (1.0
～1.5): 1, more preferably (2.1～2.4): (1.1～1.4): 1, most preferably 2.27:1.13:1；The temperature of described reaction is excellent
Elect 40～60 DEG C as, more preferably 45～55 DEG C；The time of described reaction be preferably 20～40min, more preferably 25～
35min.The present invention preferably carries out above-mentioned reaction under conditions of stirring.
After completing above-mentioned reaction, obtain is bismuth citrate aqueous solutions of potassium, and the present invention is preferably by described Bismuth Potassium Citrate water
Solution is evaporated concentrating and recrystallization successively, obtains bismuth potassium citrate.In the present invention, the temperature of described evaporation and concentration is preferred
It is 100～150 DEG C, more preferably 110～140 DEG C, most preferably 120～130 DEG C；The time of described evaporation and concentration is preferably 1
～3 hours, more preferably 1.5～2.5 hours, most preferably 2 hours；Evaporation and concentration separates out to just there being solid.
The product that evaporation and concentration is obtained, the present invention is preferably added to ethanol and carries out recrystallization, add every time ethanol 100～
150mL, after stirring, white solid separates out again, filters, and the solid obtained adds ethanol again, repeats the process of above-mentioned crystallization,
To the bismuth potassium citrate of recrystallization, the number of times of described recrystallization is preferably 1～3 time.
The product of recrystallization is preferably vacuum dried by the present invention, obtains bismuth potassium citrate, and described vacuum drying is this
The drying means that skilled person commonly uses, the present invention does not has special restriction to this.
The present invention provides the preparation method of a kind of bismuth potassium citrate, comprises the following steps: A) by potassium hydroxide and citric acid
Water mixes, reacts, obtain potassium citrate；B) bismuth citrate, ammonia are mixed with described potassium citrate, carry out anti-
Should, obtain bismuth potassium citrate.Preparation method in the present invention uses bismuth citrate and citric acid, potassium hydroxide one-step synthesis Chinese holly
Rafter acid bismuth potassium, it is not necessary to prepare intermediate bismuth subnitrate, technique is simple, does not use spray drying, and low cost.Further, this
The bismuth potassium citrate prepared in bright is consistent with the product standard of " Chinese Pharmacopoeia ", applied range, and productivity is 80～90%, pure
Degree is 99.95～99.99%.
Further, the present invention using ethanol as crystallization solvent, crystallization time is short, saved greatly post processing time
Between, further save cost.
In order to further illustrate the present invention, below in conjunction with the preparation of a kind of bismuth potassium citrate that the present invention is provided by embodiment
Method is described in detail, but can not be understood as limiting the scope of the present invention.
In the examples below, bismuth citrate is purchased from Guangdong Vital Rare Material Co., Ltd., monohydrate potassium, hydrogen-oxygen
Change sodium, ethanol and ammonia and be purchased from Guangzhou Chemical Reagent Factory.
Embodiment 1
Being dissolved in 25mL water by potassium hydroxide 16.2g, complete addition 17.15g citric acid to be dissolved, acid-base neutralization is anti-
Should, prepare potassium citrate aqueous solution, under conditions of T=60 DEG C, add 60g bismuth citrate while stirring, be subsequently adding 65mL
Mass concentration be 25% ammonia be completely dissolved to bismuth citrate, stir 20min, obtain bismuth citrate aqueous solutions of potassium.
By bismuth citrate aqueous solutions of potassium evaporation and concentration at 150 DEG C, time about 1h, concentrate complete, add the anhydrous second of 100mL
Alcohol, stirring has a large amount of white solid to separate out.Solid is filtered, and by washing with alcohol repeatedly, then at T=70 DEG C, vacuum is done
Dry, obtain white solid product about 70g.
In the present embodiment, the purity of bismuth potassium citrate is 99.99%, and yield is 85%.
The performance of the present invention bismuth potassium citrate to obtaining in the present embodiment is detected, and result is as shown in table 1.
The performance data of bismuth potassium citrate in table 1 embodiment of the present invention 1
In table 1, differentiate that one is to the mensuration of bismuth ion in bismuth potassium citrate.Method is to take this product about 1mg, and the 5mL that adds water is molten
Xie Hou, adds dilute sulfuric acid 2～3 acidifyings, adds thiourea solution 1～10, i.e. shows buff.
Differentiate that two is to the mensuration of citric acid radical in bismuth potassium citrate.Method is to take sample about 0.1g, and the 5mL that adds water dissolves
After, add perchloric acid solution 1～10, white opacity or precipitation i.e. occur, insoluble in sodium hydroxide test solution or liquor ammoniae fortis.
Differentiate that three is to the mensuration of potassium ion in bismuth potassium citrate.Method is to take this product about 10mg, and the 0.2mL that adds water dissolves
After, add pyridine-acetic anhydride (3:1) about 5mL, i.e. displaing yellow to red or aubergine.
Differentiating one～differentiate the result explanation of three, the white solid product obtained in the embodiment of the present invention 1 is bismuth citrate
Potassium.
About the content of sulfate and nitrate, according in " Chinese Pharmacopoeia " for sulfate detection explanation it is: take this product
After 1.0g, the 20mL that adds water dissolve, dripping dilute hydrochloric acid 4mL, put in water-bath and heat 10 minutes, let cool, filter, filtrate is divided into 2 equal portions:
1 part adds 25% barium chloride solution 5mL, places 10 minutes, repeatedly filter, clarify to filtrate, after dilute becomes 40mL, mark-on
Quasi-potassium sulfate solution 2.0mL, adds water and makes into 50mL in right amount, shake up, and places 10 minutes, as comparison liquid；Another 1 part adds water dilute
After being interpreted into 40mL, add 25% barium chloride solution 5mL, add water and make into 50mL in right amount, shake up, place 10 minutes, and compare liquor ratio
Relatively, must not richer (0.04%).
" Chinese Pharmacopoeia " for nitrate detection explanation is: take this product 0.50g, put in test tube, after the 5mL that adds water dissolves,
Adding sulphuric acid 5mL, note mixing, let cool, slowly add sulphuric acid Asia test solution 5mL along tube wall, make into two liquid layers, junction face must not show immediately
Brown.
As shown in Table 1, in the bismuth potassium citrate in the embodiment of the present invention 1, sulfate and nitrate all meets " Chinese Pharmacopoeia "
Regulation.
As can be seen from Table 1, the specification of the bismuth potassium citrate in the present embodiment meets the requirement of Chinese Pharmacopoeia, it is possible to application
In field of medicaments.
Embodiment 2
Being dissolved in 25mL water by potassium hydroxide 17.1g, complete addition 18.43g citric acid to be dissolved, acid-base neutralization is anti-
Should, prepare potassium citrate aqueous solution, under conditions of T=60 DEG C, add 73.29g bismuth citrate while stirring, be subsequently adding
78mL mass concentration be 25% ammonia be completely dissolved to bismuth citrate, stir 20min, obtain bismuth citrate aqueous solutions of potassium.
By bismuth citrate aqueous solutions of potassium evaporation and concentration at 120 DEG C, time 1h, concentrate complete, add 90mL dehydrated alcohol,
Stirring has a large amount of white solid to separate out.Solid is filtered, and by washing with alcohol repeatedly, then at T=65 DEG C, vacuum drying,
Obtain white solid product about 68g.
In the present embodiment, the purity of bismuth potassium citrate is 99.95%, and yield is 82%.
Embodiment 3
Being dissolved in 30mL water by potassium hydroxide 21.6g, complete addition 20.26g citric acid to be dissolved, acid-base neutralization is anti-
Should, prepare potassium citrate aqueous solution, under conditions of T=65 DEG C, add 76.74g bismuth citrate while stirring, be subsequently adding
90mL mass concentration be 28% ammonia be completely dissolved to bismuth citrate, stir 20min, obtain bismuth citrate aqueous solutions of potassium.
By bismuth citrate aqueous solutions of potassium evaporation and concentration at 130 DEG C, time 1h, concentrate complete, add the anhydrous second of 110mL
Alcohol, stirring has a large amount of white solid to separate out.Solid is filtered, and by washing with alcohol repeatedly, then at T=75 DEG C, vacuum is done
Dry, obtain white solid product about 75g.
In the present embodiment, the purity of bismuth potassium citrate is 99.98%, and yield is 90%.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For Yuan, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a preparation method for bismuth potassium citrate, comprises the following steps:
A) potassium hydroxide and citric acid are mixed in water, react, obtain potassium citrate；
B) bismuth citrate, ammonia are mixed with described potassium citrate, react, obtain bismuth potassium citrate.
Preparation method the most according to claim 1, it is characterised in that described step A) in mixed solution, hydrogen-oxygen
The molar concentration changing potassium is 11～13mol/L.
Preparation method the most according to claim 1, it is characterised in that the mol ratio of described citric acid and potassium hydroxide is 1:
(2～4).
Preparation method the most according to claim 1, it is characterised in that described step A) in reaction temperature be 20～30
℃；
Described step A) in reaction time be 0.5～1 hour.
Preparation method the most according to claim 1, it is characterised in that described step B) in the mass concentration of ammonia be 25～
28%.
Preparation method the most according to claim 5, it is characterised in that described step B) in bismuth citrate, ammonia and Fructus Citri Limoniae
The mol ratio of acid potassium is (2.0～2.5): (1.0～1.5): 1.
Preparation method the most according to claim 1, it is characterised in that described step B) in reaction temperature be 40～60
℃；
Described step B) in reaction time be 20～40min.
8. according to the preparation method described in claim 1～7 any one, it is characterised in that described step B) after also include with
Lower step:
By step B) mixed solution that obtains is evaporated concentrating and recrystallization successively after reaction, obtains bismuth potassium citrate.
Preparation method the most according to claim 8, it is characterised in that the solvent of described recrystallization is ethanol.
Preparation method the most according to claim 8, it is characterised in that the time of described recrystallization is 0.5～2 hour.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107011156A (en) * | 2017-05-04 | 2017-08-04 | 江苏润普食品科技股份有限公司 | A kind of method of utilization citric acid and liquid potassium hydroxide synthesizing citric acid potassium |
| CN107963967A (en) * | 2017-12-28 | 2018-04-27 | 清远先导材料有限公司 | The method for synthesizing Bismuth Potassium Citrate |
| RU2675869C1 (en) * | 2018-02-05 | 2018-12-25 | Общество с ограниченной ответственностью "Брайт Вэй" | Method of obtaining bismuth-potassium ammonium citrate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402706A (en) * | 2014-11-19 | 2015-03-11 | 江苏悦兴药业有限公司 | Preparation method of high-purity calcium citrate |
-
2016
- 2016-08-03 CN CN201610632889.4A patent/CN106278870A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402706A (en) * | 2014-11-19 | 2015-03-11 | 江苏悦兴药业有限公司 | Preparation method of high-purity calcium citrate |
Non-Patent Citations (2)
| Title |
|---|
| 周雍茂等: "枸橼酸铋钾制备新工艺的研究", 《当代化工》 * |
| 邵冠儒: "温度对枸橼酸铋钾合成中的影响", 《数理医药学杂志》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107011156A (en) * | 2017-05-04 | 2017-08-04 | 江苏润普食品科技股份有限公司 | A kind of method of utilization citric acid and liquid potassium hydroxide synthesizing citric acid potassium |
| CN107963967A (en) * | 2017-12-28 | 2018-04-27 | 清远先导材料有限公司 | The method for synthesizing Bismuth Potassium Citrate |
| RU2675869C1 (en) * | 2018-02-05 | 2018-12-25 | Общество с ограниченной ответственностью "Брайт Вэй" | Method of obtaining bismuth-potassium ammonium citrate |
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