CN113526528A - Preparation method of medicinal potassium iodide - Google Patents
Preparation method of medicinal potassium iodide Download PDFInfo
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- CN113526528A CN113526528A CN202110805473.9A CN202110805473A CN113526528A CN 113526528 A CN113526528 A CN 113526528A CN 202110805473 A CN202110805473 A CN 202110805473A CN 113526528 A CN113526528 A CN 113526528A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/12—Iodides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention relates to a preparation method of medicinal potassium iodide, which comprises the following steps: s1, dissolving potassium hydroxide in purified water to prepare a potassium hydroxide solution; s2, adding formic acid into the potassium hydroxide solution in the step S1, heating, stirring, and keeping constant temperature for sufficient neutralization reaction; s3, adding refined iodine, maintaining the liquid temperature at 70-90 ℃ by adopting a cooling device in the process of adding the refined iodine, heating the liquid material to 90-105 ℃ after adding the refined iodine, and keeping constant temperature reaction; s4, adding potassium hydroxide to adjust the PH value after the iodine ion yellow of the feed liquid gradually fades; s5, adding activated carbon to decolor and adsorb impurities, layering the liquid, and filtering; s6, concentrating and separating; and S7, finally drying to obtain the finished product. The invention achieves the following beneficial effects: the method has the advantages of adding acid and alkali at one time, fast reaction, easy control, small iodine volatilization, full participation of iodine in the reaction, avoidance of generation of a large amount of unreacted waste materials and cost saving.
Description
Technical Field
The invention relates to the technical field of production methods of potassium iodide, in particular to a preparation method of medicinal potassium iodide.
Background
The production method of potassium iodide mainly comprises an iron powder reduction method and a formic acid reduction method.
The method for producing potassium iodide by the iron powder reduction method has the advantages of stable process, short reaction time and easy operation, but the amount of generated solid waste gas is very large.
The formic acid reduction method is to react potassium hydroxide with iodine to produce potassium iodide and potassium iodate, to produce partial potassium iodate, and to add formic acid to reduce potassium iodide. But during the reaction with addition of formic acid, I-And IO3-Under acidic conditions, I is easily generated2Causing iodine vapor to escape, resulting in material loss; in addition, potassium hydroxide used for PH adjustment tends to react with excess formic acid to form potassium formate, resulting in a decrease in potassium iodide content.
Therefore, the company improves the process on the basis of the formic acid reduction method, reduces material loss, and simultaneously improves the reaction efficiency and the production efficiency. Thereby saving production cost.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of medicinal potassium iodide, which has the advantages of one-time addition of acid and alkali, quick and easily controlled reaction, small iodine volatilization amount, full participation of iodine in the reaction, avoidance of generation of a large amount of unreacted waste materials and cost saving.
The purpose of the invention is realized by the following technical scheme: a preparation method of medicinal potassium iodide comprises the following steps:
s1, preparing a potassium hydroxide solution;
dissolving potassium hydroxide in purified water to prepare a potassium hydroxide solution containing 11-15% of potassium hydroxide;
s2, neutralization reaction;
adding formic acid into the potassium hydroxide solution in the step S1, and simultaneously heating and stirring the feed liquid;
when the temperature is raised to 65-85 ℃, keeping the temperature constant, and carrying out full neutralization reaction;
s3, synthesis reaction;
adding refined iodine into the liquid after the neutralization reaction, and maintaining the temperature of the liquid at 70-90 ℃ by adopting a cooling device in the process of adding the refined iodine;
after adding refined iodine, heating the feed liquid to 90-105 ℃, and keeping constant temperature reaction;
s4, adjusting the pH value;
after the constant temperature reaction in the step S3, adding potassium hydroxide to adjust the PH value to 8-9 after the iodine ion yellow of the feed liquid gradually fades;
s5, layering and filtering;
adding activated carbon for decoloring and adsorbing impurities, and boiling the feed liquid for 10-30 min after adding the activated carbon;
then stopping heating and stirring, standing to precipitate small particles in the feed liquid, suspending suspended matters in the feed liquid and promoting the feed liquid to be layered;
then filtering is carried out;
s6, concentrating and separating;
heating and concentrating the filtered feed liquid, and cooling to 30-40 ℃ when the solid-to-liquid ratio reaches 30-40 ℃;
then carrying out centrifugal separation to obtain a solid material;
and S7, carrying out vacuum drying on the wet solid material obtained after centrifugation to obtain a finished product.
Further, in the step S2, after the potassium hydroxide is added to the formic acid, the temperature is raised to 65 to 85 ℃ while the feed liquid is heated and stirred, and the temperature is kept constant for 5 to 30 min.
Further, in the step S3, in the process of adding the refined iodine, a cooling device is used to maintain the liquid temperature at 75-85 ℃; in step S3, after the refined iodine is added, the temperature of the feed liquid is raised to 95-102 ℃, and the reaction time for keeping the constant temperature is 2-5 h.
Preferably, the constant temperature in the step S2 is kept for 10 min; the isothermal reaction time in step S3 was 3.5 h.
Preferably, in step S5, activated carbon is added to boil the liquid for about 20min, and the solution is left to stand for about 10 min.
Preferably, in step S6, when the solid-to-liquid ratio reaches 30 to 40 ℃, the temperature is cooled to about 35 ℃.
After the preparation is finished, all indexes of potassium iodide in a finished product meet the requirements of Chinese pharmacopoeia, and the content is 99.1-99.5%.
Preferably, in step S5, after the activated carbon is added, the feed liquid is boiled by high-temperature steam, and the stirring is performed while the high-temperature steam is introduced.
The reaction principle of the scheme is as follows: the potassium hydroxide and the formic acid react to generate potassium formate, and the potassium formate reacts with the iodine to generate potassium iodide. Two main reactions are involved: first, KOH + HCOOH ═ KCOOH + H20; second step, OH-+COOH-+I2＝2I-+H20+CO2↑。
The invention has the following advantages:
(1) in the scheme, the potassium hydroxide and the formic acid are added in proportion, the iodine is gradually added after the temperature is raised to a certain temperature, the whole reaction system is alkaline, the iodine is not easy to volatilize, the whole reaction process is stable and easy to operate, and compared with an iron powder reduction method, the generation of a large amount of solid waste is reduced;
(2) compared with a two-step reduction method of formic acid, the method has the advantages that acid and alkali are added at one time, the reaction is fast, the control is easy, the addition of granular iodine into water (liquid) is fast, the loss of iodine vapor is not easy to cause, and the process is convenient and easy to operate; in addition, simple substance iodine is reduced by utilizing the reducibility of formate in the reaction process, the reduction reaction is easy to carry out, and the reaction process is relatively quick.
Detailed Description
The present invention is further described below, but the scope of the present invention is not limited to the following.
Example 1
A preparation method of medicinal potassium iodide comprises the following steps:
s1, preparing a potassium hydroxide solution, namely dissolving 33.85kg of potassium hydroxide in purified water to prepare a potassium hydroxide solution containing about 12% of potassium hydroxide;
s2, neutralization reaction, namely adding 15.87kg of formic acid into the potassium hydroxide solution in the step S1, and heating and stirring the solution at the same time; when the temperature is raised to about 65 ℃, keeping the constant temperature for 10min, and carrying out full neutralization reaction;
s3, carrying out synthetic reaction, namely adding 75kg of refined iodine into the liquid after the neutralization reaction, starting a condensation reflux device and jacket cooling water simultaneously in the process of adding the refined iodine, and ensuring that the reaction temperature is about 75 ℃; after adding refined iodine, heating the feed liquid to 95 ℃, and keeping constant temperature for reaction for 3.5 hours;
s4, adjusting the pH value, and after the constant-temperature reaction in the step S3, adding potassium hydroxide to adjust the pH value to 8-9 after the iodine ion yellow of the feed liquid gradually fades away;
s5, layering, filtering, adding 0.75kg of active carbon for decoloring and adsorbing impurities, adding the active carbon, and boiling the feed liquid for 20 min; then stopping heating and stirring, standing for 10min to precipitate small particles in the feed liquid, suspend suspended matters in the feed liquid, and promote layering of the feed liquid; finally, filtering is carried out;
s6, concentrating, separating, heating and concentrating the filtered feed liquid, and cooling to 30 ℃ when the solid-to-liquid ratio reaches about 30%; then carrying out centrifugal separation to obtain a solid material;
and S7, carrying out vacuum drying on the wet solid material obtained after centrifugation to obtain a finished product.
Example 2
A preparation method of medicinal potassium iodide comprises the following steps:
s1, preparing a potassium hydroxide solution, namely dissolving 90.28kg of potassium hydroxide in purified water to prepare a potassium hydroxide solution containing about 13% of potassium hydroxide;
s2, neutralization reaction, namely adding 42.34kg of formic acid into the potassium hydroxide solution in the step S1, and heating and stirring the solution at the same time; when the temperature is raised to about 75 ℃, keeping the constant temperature for 10min, and carrying out full neutralization reaction;
s3, carrying out synthetic reaction, namely adding 75kg of refined iodine into the liquid after the neutralization reaction, starting a condensation reflux device and jacket cooling water simultaneously in the process of adding the refined iodine, and ensuring that the reaction temperature is about 80 ℃; after adding refined iodine, heating the feed liquid to 98 ℃, and keeping constant temperature for reaction for 3.5 hours;
s4, adjusting the pH value, and after the constant-temperature reaction in the step S3, adding potassium hydroxide to adjust the pH value to 8-9 after the iodine ion yellow of the feed liquid gradually fades away;
s5, layering, filtering, adding 1.56kg of active carbon for decoloring and adsorbing impurities, adding the active carbon, and boiling the feed liquid for 20 min; then stopping heating and stirring, standing for 10min to precipitate small particles in the feed liquid, suspend suspended matters in the feed liquid, and promote layering of the feed liquid; finally, filtering is carried out;
s6, concentrating, separating, heating and concentrating the filtered feed liquid, and cooling to about 30 ℃ when the solid-to-liquid ratio reaches 35%; then carrying out centrifugal separation to obtain a solid material;
and S7, carrying out vacuum drying on the wet solid material obtained after centrifugation to obtain a finished product.
Example 3
A preparation method of medicinal potassium iodide comprises the following steps:
s1, preparing a potassium hydroxide solution, namely dissolving 183.2kg of potassium hydroxide in purified water to prepare a potassium hydroxide solution containing about 14% of potassium hydroxide;
s2, neutralization reaction, namely, adding 83.8kg of formic acid into the potassium hydroxide solution in the step S1, and simultaneously heating and stirring the solution; when the temperature is raised to about 80 ℃, keeping the constant temperature for 10min, and carrying out full neutralization reaction;
s3, carrying out synthetic reaction, namely adding 75kg of refined iodine into the liquid after the neutralization reaction, starting a condensation reflux device and jacket cooling water simultaneously in the process of adding the refined iodine, and ensuring that the reaction temperature is about 85 ℃; after adding refined iodine, heating the feed liquid to 102 ℃, and keeping constant temperature for reaction for 3.5 hours;
s4, adjusting the pH value, and after the constant-temperature reaction in the step S3, adding potassium hydroxide to adjust the pH value to 8-9 after the iodine ion yellow of the feed liquid gradually fades away;
s5, layering, filtering, adding 3kg of active carbon for decoloring and adsorbing impurities, adding the active carbon, and boiling the feed liquid for 20 min; then stopping heating and stirring, standing for 10min to precipitate small particles in the feed liquid, suspend suspended matters in the feed liquid, and promote layering of the feed liquid; finally, filtering is carried out;
s6, concentrating, separating, heating and concentrating the filtered feed liquid, and cooling to about 40 ℃ when the solid-to-liquid ratio reaches about 40%; then carrying out centrifugal separation to obtain a solid material;
and S7, carrying out vacuum drying on the wet solid material obtained after centrifugation to obtain a finished product.
In the above three embodiments, in step S5, after the activated carbon is added, the feed liquid is boiled by high-temperature steam, and stirring is achieved while introducing the high-temperature steam.
In the three examples, the mother liquor was also separated when the centrifugation was performed.
Experimental example, using the three examples described above, the content of potassium iodide in the finished product was measured, and the experimental data and results are shown in table one.
Table-table of raw material input and product content
From the experimental results of the three examples, it can be seen that potassium iodide in the final product meets the requirements of Chinese pharmacopoeia, and the content is 99.1-99.5%. Therefore, the preparation method of the scheme has the advantages that the iodine is not easy to volatilize, the reaction is fully participated, and compared with an iron powder reduction method, the generation of a large amount of solid wastes is reduced.
The method belongs to a finished product of potassium iodide with high content, and is also explained from the side surface, the process of adding acid and alkali at one time has quick reaction and easy control; the granular iodine is added into water (liquid) quickly, the loss of iodine vapor is not easy to cause, and the process is convenient and easy to operate.
The above examples only represent preferred embodiments, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (8)
1. A preparation method of medicinal potassium iodide is characterized in that: the method comprises the following steps:
s1, preparing a potassium hydroxide solution;
dissolving potassium hydroxide in purified water to prepare a potassium hydroxide solution containing 11-15% of potassium hydroxide;
s2, neutralization reaction;
adding formic acid into the potassium hydroxide solution in the step S1, and simultaneously heating and stirring the feed liquid;
when the temperature is raised to 65-85 ℃, keeping the temperature constant, and carrying out full neutralization reaction;
s3, synthesis reaction;
adding refined iodine into the liquid after the neutralization reaction, and maintaining the temperature of the liquid at 70-90 ℃ by using a cooling device in the process of adding the refined iodine;
after adding refined iodine, heating the feed liquid to 90-105 ℃, and keeping constant temperature reaction;
s4, adjusting the pH value;
after the constant temperature reaction in the step S3, adding potassium hydroxide to adjust the PH value to 8-9 after the iodine ion yellow of the feed liquid gradually fades;
s5, layering and filtering;
adding activated carbon for decoloring and adsorbing impurities, and boiling the feed liquid for 10-30 min after adding the activated carbon;
then stopping heating and stirring, standing to precipitate small particles in the feed liquid, suspending suspended matters in the feed liquid and promoting the feed liquid to be layered;
then filtering is carried out;
s6, concentrating and separating;
heating and concentrating the filtered feed liquid, and cooling to 30-40 ℃ when the solid-liquid ratio reaches 30-40 ℃;
then carrying out centrifugal separation to obtain a solid material;
and S7, carrying out vacuum drying on the wet solid material obtained after centrifugation to obtain a finished product.
2. The process of claim 1 for the preparation of a pharmaceutical potassium iodide, wherein: in the step S2, after the potassium hydroxide is added into the formic acid, the temperature is raised to 65-80 ℃ while the feed liquid is heated and stirred, and the temperature is kept constant for 5-30 min.
3. The process of claim 2, wherein the potassium iodide comprises: in the step S3, in the process of adding the refined iodine, a cooling device is adopted to maintain the liquid temperature at 75-85 ℃;
in the step S3, after the refined iodine is added, the temperature of the feed liquid is raised to 95-102 ℃, and the reaction time for keeping the constant temperature is 2-5 h.
4. The process of claim 3, wherein the potassium iodide comprises: keeping the constant temperature in the step S2 for 10 min; the isothermal reaction time in step S3 was 3.5 h.
5. The process for preparing potassium iodide for pharmaceutical use according to claim 3 or 4, wherein: in the step S5, activated carbon is added to boil the liquid for about 20min, and the liquid is kept still for about 10 min.
6. The process of claim 5, wherein the potassium iodide comprises: in the step S6, when the solid-to-liquid ratio reaches 30-40%, cooling to about 35 ℃.
7. The process of claim 6, wherein the potassium iodide comprises: in the finished product, the content of potassium iodide is 99.1-99.5%.
8. The process of claim 6, wherein the potassium iodide comprises: in the step S5, after the activated carbon is added, the feed liquid is boiled by high-temperature steam, and the stirring is realized while the high-temperature steam is introduced.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB358728A (en) * | 1929-10-14 | 1931-10-15 | Johannes Hendrik Van Der Meule | Process of preparing iodides of alkali metals or alkaline earth metals |
| JPH07242414A (en) * | 1994-03-04 | 1995-09-19 | Mitsui Toatsu Chem Inc | Production of alkali metal iodic salt |
| JP2015137214A (en) * | 2014-01-23 | 2015-07-30 | 日宝化学株式会社 | Manufacturing method of alkali metal iodide or alkali earth metal iodide |
| CN106517252A (en) * | 2016-10-10 | 2017-03-22 | 无锡易水元资源循环科技有限公司 | Analytical pure potassium iodide preparation method using waste liquid containing iodine |
| CN106800303A (en) * | 2016-12-27 | 2017-06-06 | 国药集团化学试剂有限公司 | A kind of method that utilization micro passage reaction prepares KI |
| CN112079364A (en) * | 2020-09-08 | 2020-12-15 | 山东博苑医药化学股份有限公司 | Method for recycling fluorine-and iodine-containing waste material resources |
-
2021
- 2021-07-16 CN CN202110805473.9A patent/CN113526528A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB358728A (en) * | 1929-10-14 | 1931-10-15 | Johannes Hendrik Van Der Meule | Process of preparing iodides of alkali metals or alkaline earth metals |
| JPH07242414A (en) * | 1994-03-04 | 1995-09-19 | Mitsui Toatsu Chem Inc | Production of alkali metal iodic salt |
| JP2015137214A (en) * | 2014-01-23 | 2015-07-30 | 日宝化学株式会社 | Manufacturing method of alkali metal iodide or alkali earth metal iodide |
| CN106517252A (en) * | 2016-10-10 | 2017-03-22 | 无锡易水元资源循环科技有限公司 | Analytical pure potassium iodide preparation method using waste liquid containing iodine |
| CN106800303A (en) * | 2016-12-27 | 2017-06-06 | 国药集团化学试剂有限公司 | A kind of method that utilization micro passage reaction prepares KI |
| CN112079364A (en) * | 2020-09-08 | 2020-12-15 | 山东博苑医药化学股份有限公司 | Method for recycling fluorine-and iodine-containing waste material resources |
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