CN113461579A - Preparation method of pharmaceutical grade dimethyl sulfoxide - Google Patents
Preparation method of pharmaceutical grade dimethyl sulfoxide Download PDFInfo
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- CN113461579A CN113461579A CN202110878994.7A CN202110878994A CN113461579A CN 113461579 A CN113461579 A CN 113461579A CN 202110878994 A CN202110878994 A CN 202110878994A CN 113461579 A CN113461579 A CN 113461579A
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- C—CHEMISTRY; METALLURGY
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- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/06—Separation; Purification; Stabilisation; Use of additives
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Abstract
The application discloses a preparation method of medicinal dimethyl sulfoxide, which comprises the following steps: adding industrial-grade dimethyl sulfoxide with the content of more than 99.8% into a stainless steel rectifying still, adding distilled water according to the proportion of 1:2, then carrying out rectification operation under the condition of reduced pressure, dehydrating at the top of the tower at the initial stage, taking out a part of impurities in the dimethyl sulfoxide through dehydration, and further removing all impurities in the dimethyl sulfoxide after membrane filtration and resin exchange of the generated medicinal-grade sulfoxide. The preparation method has the characteristics of advanced production technology, controllable process conditions, simple and easily obtained auxiliary raw materials, low unit consumption and the like.
Description
Technical Field
The invention belongs to the technical field of intermediate medicament preparation in the field of medicines, and particularly relates to a preparation method of medicinal dimethyl sulfoxide.
Background
The medical grade dimethyl sulfoxide is an important solvent in the medical industry, can be directly used as a raw material or a carrier of a medicament, has the efficacies of diminishing inflammation, relieving pain, promoting urination, calming and the like, is known as 'universal medicine', and has wide application in the medical field, such as:
dimethyl sulfoxide can rapidly penetrate skin and permeate medicine into organism, and is clinically used as penetrant;
the dimethyl sulfoxide has the effects of diminishing inflammation, relieving pain, promoting urination and quickly reducing swelling, and plays a role in absorbing and enhancing organic solvents such as antibiotics, hormones and the like;
the dimethyl sulfoxide has the function of absorbing water and has the effect of eliminating various edemas, hydrops and herpes;
because the effective components of (IV) dimethyl sulfoxide can be extracted from Chinese herbs, dimethyl sulfoxide is well regarded by the traditional Chinese medicine.
Due to the particularity of the field of medicine, the requirements on the purity, cleanliness and ultraviolet absorbance of the medical-grade dimethyl sulfoxide are very high. In the prior art, the application of the medical-grade dimethyl sulfoxide is limited by the requirements and the limits of content impurities and ultraviolet light absorption values, and the medical-grade dimethyl sulfoxide cannot be utilized from industrial-grade dimethyl sulfoxide, so that the medical-grade dimethyl sulfoxide in China depends on import for a long time, has high price and cannot be popularized and used in a large area. The traditional preparation method of dimethyl sulfoxide (non-medicinal grade), such as CN102093268A and CN106674066A, needs to add an intermediate medium, cannot meet the requirements of medicinal grade due to the introduction of new impurities, and CN104119256A has the problems of complex preparation device and high generation cost.
Disclosure of Invention
The application aims to provide a preparation method of medicinal dimethyl sulfoxide, which can realize the preparation of the medicinal dimethyl sulfoxide at low cost by means of a simple device, is convenient and quick to generate, and greatly improves the processing speed.
The technical purpose of the invention is realized by the following technical scheme:
a preparation method of medicinal dimethyl sulfoxide comprises the following steps:
1) pumping industrial grade dimethyl sulfoxide with the content of more than 99.8 percent into a stainless steel rectifying kettle under the condition of reduced pressure, and metering;
2) adding distilled water according to the mass ratio of 1:2 according to the weight of the dimethyl sulfoxide pumped into the kettle;
3) under the condition of reduced pressure, the pressure at the top of the tower is controlled to be 6-8 Kpa at the temperature of 42-46 ℃, the pressure at the bottom of the tower is controlled to be 8.5-11.5 Kpa at the temperature of 80-90 ℃, and part of impurities in dimethyl sulfoxide are carried out by water extracted from the top of the tower;
4) after all the water in the rectifying still is extracted, when the dimethyl sulfoxide is extracted, the temperature at the top of the tower is 102-105 ℃, the pressure at the top of the tower is 8-10 Kpa, the temperature at the bottom of the tower is 120-125 ℃, and the pressure at the bottom of the tower is 11.5-12.5 Kpa, and the dimethyl sulfoxide is extracted from the top of the tower into an intermediate tank;
5) the extracted dimethyl sulfoxide passes through a micro-membrane by a pressure pump in an intermediate tank under the protection of nitrogen;
6) and (3) carrying out ion exchange on the dimethyl sulfoxide passing through the micro-membrane and the pretreated resin by using a peristaltic pump under the protection of nitrogen to prepare medicinal dimethyl sulfoxide, putting the medicinal dimethyl sulfoxide into a finished product tank, and packaging.
Further, in step 5), the pore size of the micro-membrane is 0.2 μm, and dimethyl sulfoxide is passed through the micro-membrane using a pressure pump.
Further, in step 6), the resin comprises a positive and a negative resin, and ion exchange is performed by chromatography using a peristaltic pump.
Furthermore, the preparation process of the pharmaceutical grade dimethyl sulfoxide can not contact with air, and the whole process is carried out under the protection of nitrogen.
Further, the content of dimethyl sulfoxide prepared by the method is 99.95%.
Further, when nitrogen gas was introduced for 15 minutes, the absorbance values at 275nm, 285nm and 295nm were measured as 0.281, 0.602 and 0.418, respectively.
Compared with the prior art, the invention has the following advantages:
the medicinal dimethyl sulfoxide prepared by the method has the characteristics of high purity, less impurities, ultraviolet light absorption value reaching pharmacopeia standards, easily obtained raw materials, low unit consumption, easy operation of the process and the like. The detection completely reaches the standard of 'Chinese pharmacopoeia' 2020 edition.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
FIG. 1 is a process flow diagram of the process for preparing pharmaceutical grade dimethyl sulfoxide according to the present application.
Detailed Description
In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention comprehensible, the present invention is further explained with reference to examples, and it should be noted that all examples listed herein are only illustrative and are not meant to limit the scope of the present invention.
As shown in figure 1, the preparation method of the pharmaceutical grade dimethyl sulfoxide comprises the steps of putting industrial grade dimethyl sulfoxide with the content of more than 99.8% into a stainless steel rectifying kettle, metering, putting distilled water into the rectifying kettle according to the ratio of 1:2, rectifying under the condition of reduced pressure, controlling the pressure at the top of the tower to be 6-8 Kpa, the temperature to be 42-46 ℃, the pressure at the bottom of the tower to be 8.5-11.5 Kpa and the temperature to be 80-90 ℃ during initial dehydration, mainly taking out part of impurities in the dimethyl sulfoxide during dehydration, controlling the pressure at the top of the tower to be 8-10 Kpa, the temperature at the top of the tower to be 102-105 ℃, the pressure at the bottom of the tower to be 11.5-12.5 Kpa and the temperature at the bottom of the tower to be 120-125 ℃, filtering the dimethyl sulfoxide in the rectifying kettle by a pressure pump through a 3M micro-membrane under the protection of nitrogen after all dimethyl sulfoxide is taken out, and carrying out ion exchange with pretreated anion and cation resin by the peristaltic pump, and putting the obtained medicinal dimethyl sulfoxide into a finished product tank, and packaging.
Comparative example 1:
putting more than 99.8 percent of industrial-grade dimethyl sulfoxide into a stainless steel rectifying kettle, metering, putting common water into the rectifying kettle according to a ratio of 1:2, rectifying under a reduced pressure condition, wherein the pressure at the top of the tower is 6-8 Kpa, the temperature is 42-46 ℃, the pressure at the bottom of the tower is 8.5-11.5 Kpa and the temperature is 80-90 ℃ during initial dehydration, the impurities in the dimethyl sulfoxide are taken out during dehydration, and after dehydration is finished, when the dimethyl sulfoxide at the top of the tower is extracted, the pressure at the top of the tower is 8-10 Kpa, the temperature at the top of the tower is 102-105 ℃, the pressure at the bottom of the tower is 11.5-12.5 Kpa and the temperature at the bottom of the tower is 120-125 ℃. And (3) taking out all dimethyl sulfoxide in the rectifying kettle, then feeding the dimethyl sulfoxide into an intermediate tank, filtering the dimethyl sulfoxide through a 3M micro-membrane by using a pressure pump under the protection of nitrogen, then carrying out ion exchange on the dimethyl sulfoxide and pretreated anion-cation resin by using a peristaltic pump, and feeding the prepared medicinal dimethyl sulfoxide into a finished product tank. The prepared medicinal dimethyl sulfoxide is sampled, the content of the medicinal dimethyl sulfoxide is 99.88 percent through gas chromatography detection, and after the medicinal dimethyl sulfoxide is subjected to nitrogen for 15 minutes, the light absorption values at 275nm, 285nm and 295nm are respectively measured to be 0.556, 0.771 and 0.505. According to the standard of '2020 version of Chinese pharmacopoeia', the light absorption values of 275nm, 285nm and 295nm wavelength are not more than 0.3, 0.65 and 0.45, and do not accord with the standard of medical grade dimethyl sulfoxide.
Comparative example 2:
putting more than 99.8 percent of industrial-grade dimethyl sulfoxide into a stainless steel rectifying kettle, metering, putting distilled water into the rectifying kettle according to a ratio of 1:2, rectifying under a reduced pressure condition, wherein the pressure at the top of the tower is 6-8 Kpa, the temperature is 42-46 ℃, the pressure at the bottom of the tower is 8.5-11.5 Kpa and the temperature is 80-90 ℃ during initial dehydration, the impurities in the dimethyl sulfoxide are taken out during dehydration, after dehydration is finished, when the dimethyl sulfoxide is extracted from the top of the tower, the pressure at the top of the tower is 8-10 Kpa, the temperature at the top of the tower is 102-105 ℃, the pressure at the bottom of the tower is 11.5-12.5 Kpa and the temperature at the bottom of the tower is 120-125 ℃. And (3) extracting all dimethyl sulfoxide in the rectifying kettle, introducing the dimethyl sulfoxide into an intermediate tank, under the protection of nitrogen, introducing the dimethyl sulfoxide into pretreated cation-anion resin by using a peristaltic pump for exchange to obtain medicinal dimethyl sulfoxide, and introducing the medicinal dimethyl sulfoxide into a finished product tank. Sampling the prepared medicinal dimethyl sulfoxide, detecting the content of 99.90% by gas chromatography, and passing nitrogen through the medicinal dimethyl sulfoxide for 15 minutes to respectively measure the light absorption values of 275nm, 285nm and 295nm wavelength as 0.352, 0.404 and 0.273. According to the standard of '2020 version of Chinese pharmacopoeia', the light absorption values of 275nm, 285nm and 295nm wavelength are not more than 0.3, 0.65 and 0.45, and do not accord with the standard of medical grade dimethyl sulfoxide.
Comparative example 3:
putting more than 99.8 percent of industrial-grade dimethyl sulfoxide into a stainless steel rectifying kettle, metering, putting distilled water into the rectifying kettle according to a ratio of 1:2, rectifying under a reduced pressure condition, wherein the pressure at the top of the tower is 6-8 Kpa, the temperature is 42-46 ℃, the pressure at the bottom of the tower is 8.5-11.5 Kpa and the temperature is 80-90 ℃ during initial dehydration, the impurities in the dimethyl sulfoxide are taken out during dehydration, after dehydration is finished, when the dimethyl sulfoxide is extracted from the top of the tower, the pressure at the top of the tower is 8-10 Kpa, the temperature at the top of the tower is 102-105 ℃, the pressure at the bottom of the tower is 11.5-12.5 Kpa and the temperature at the bottom of the tower is 120-125 ℃. And (3) extracting all dimethyl sulfoxide in the rectifying kettle, introducing the dimethyl sulfoxide into an intermediate tank, filtering the dimethyl sulfoxide through a 3M micro-membrane by using a pressure pump under the protection of nitrogen, and introducing the prepared medicinal dimethyl sulfoxide into a finished product tank. Sampling the prepared medicinal dimethyl sulfoxide, detecting the content of 99.92% by gas chromatography, introducing nitrogen for 15 min for replacement, and respectively measuring the light absorption values of 275nm, 285nm and 295nm as 0.328, 0.685 and 0.482. According to the standard of '2020 version of Chinese pharmacopoeia', the light absorption values of 275nm, 285nm and 295nm wavelength are not more than 0.3, 0.65 and 0.45, and do not accord with the standard of medical grade dimethyl sulfoxide.
Example 1:
putting more than 99.8 percent of industrial-grade dimethyl sulfoxide into a stainless steel rectifying kettle, metering, putting distilled water into the rectifying kettle according to a ratio of 1:2, rectifying under a reduced pressure condition, wherein the pressure at the top of the tower is 6-8 Kpa, the temperature is 42-46 ℃, the pressure at the bottom of the tower is 8.5-11.5 Kpa and the temperature is 80-90 ℃ during initial dehydration, the impurities in the dimethyl sulfoxide are taken out during dehydration, after dehydration is finished, when the dimethyl sulfoxide is extracted from the top of the tower, the pressure at the top of the tower is 8-10 Kpa, the temperature at the top of the tower is 102-105 ℃, the pressure at the bottom of the tower is 11.5-12.5 Kpa and the temperature at the bottom of the tower is 120-125 ℃. And (4) extracting all dimethyl sulfoxide in the rectifying kettle to enter an intermediate tank. Filtering dimethyl sulfoxide by a pressure pump through a 3M micro-membrane under the protection of nitrogen, performing ion exchange on the dimethyl sulfoxide through pretreated anions and cations by a peristaltic pump to obtain medicinal dimethyl sulfoxide, and putting the medicinal dimethyl sulfoxide into a finished product tank. Sampling the prepared medicinal dimethyl sulfoxide, detecting the content of 99.95% by gas chromatography, introducing nitrogen for 15 minutes, and respectively measuring the light absorption values of 275nm, 285nm and 295nm as 0.281, 0.602 and 0.418. According to the standard of '2020 version of Chinese pharmacopoeia', the light absorption values of 275nm, 285nm and 295nm wavelength are not more than 0.3, 0.65 and 0.45, and the standard accords with the pharmaceutical grade dimethyl sulfoxide, and the product is packaged after the detection is qualified.
Summarizing the above embodiments, the following conclusions can be drawn:
the quality requirements of raw materials and auxiliary materials in the preparation process of the medicinal dimethyl sulfoxide are quite high, distilled water is adopted and then is filtered through a 3M micro-membrane and exchanged with anion and cation resin, and the prepared medicinal dimethyl sulfoxide meets the standard of '2020 edition of Chinese pharmacopoeia' and can completely meet the requirements of customers.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (6)
1. A preparation method of medicinal dimethyl sulfoxide is characterized by comprising the following steps:
1) pumping industrial grade dimethyl sulfoxide with the content of more than 99.8 percent into a stainless steel rectifying kettle under the condition of reduced pressure, and metering;
2) adding distilled water according to the mass ratio of 1:2 according to the weight of the dimethyl sulfoxide pumped into the kettle;
3) under the condition of reduced pressure, the pressure at the top of the tower is controlled to be 6-8 Kpa at the temperature of 42-46 ℃, the pressure at the bottom of the tower is controlled to be 8.5-11.5 Kpa at the temperature of 80-90 ℃, and part of impurities in dimethyl sulfoxide are carried out by water extracted from the top of the tower;
4) after all the water in the rectifying still is extracted, when the dimethyl sulfoxide is extracted, the temperature at the top of the tower is 102-105 ℃, the pressure at the top of the tower is 8-10 Kpa, the temperature at the bottom of the tower is 120-125 ℃, and the pressure at the bottom of the tower is 11.5-12.5 Kpa, and the dimethyl sulfoxide is extracted from the top of the tower into an intermediate tank;
5) the extracted dimethyl sulfoxide passes through a micro-membrane by a pressure pump in an intermediate tank under the protection of nitrogen;
6) and (3) carrying out ion exchange on the dimethyl sulfoxide passing through the micro-membrane and the pretreated resin by using a peristaltic pump under the protection of nitrogen to prepare medicinal dimethyl sulfoxide, putting the medicinal dimethyl sulfoxide into a finished product tank, and packaging.
2. The method of claim 1, wherein in step 5), the pore size of the micro-membrane is 0.2 μm, and the dimethyl sulfoxide is passed through the micro-membrane by using a pressure pump.
3. The method of claim 1, wherein in step 6), the resin comprises a cation resin and a cation resin, and the ion exchange is performed by chromatography using a peristaltic pump.
4. The method of claim 1, wherein the pharmaceutical grade dimethylsulfoxide is prepared without contact with air and the whole process is carried out under nitrogen protection.
5. The method of claim 1, wherein the dimethyl sulfoxide has a dimethyl sulfoxide content of 99.95%.
6. The process of claim 1, wherein the absorbance values at 275nm, 285nm and 295nm are 0.281, 0.602 and 0.418, respectively, when nitrogen is introduced for 15 minutes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115784952A (en) * | 2022-10-09 | 2023-03-14 | 新疆兴发化工有限公司 | Purification process of electronic grade dimethyl sulfoxide |
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| CN102093268A (en) * | 2010-12-29 | 2011-06-15 | 天津市康科德科技有限公司 | Preparation method of chromatographic grade dimethyl sulfoxide |
| CN106674066A (en) * | 2016-12-09 | 2017-05-17 | 国药集团化学试剂有限公司 | Method for purifying dimethyl sulfoxide |
| CN107459472A (en) * | 2016-06-03 | 2017-12-12 | 中国石油天然气股份有限公司 | Method for refining dimethyl sulfoxide solvent in carbon fiber precursor production process |
| CN112225680A (en) * | 2019-07-15 | 2021-01-15 | 中国石油化工股份有限公司 | Organic solvent purification method and device |
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- 2021-08-02 CN CN202110878994.7A patent/CN113461579B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093268A (en) * | 2010-12-29 | 2011-06-15 | 天津市康科德科技有限公司 | Preparation method of chromatographic grade dimethyl sulfoxide |
| CN107459472A (en) * | 2016-06-03 | 2017-12-12 | 中国石油天然气股份有限公司 | Method for refining dimethyl sulfoxide solvent in carbon fiber precursor production process |
| CN106674066A (en) * | 2016-12-09 | 2017-05-17 | 国药集团化学试剂有限公司 | Method for purifying dimethyl sulfoxide |
| CN112225680A (en) * | 2019-07-15 | 2021-01-15 | 中国石油化工股份有限公司 | Organic solvent purification method and device |
Non-Patent Citations (1)
| Title |
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| 顾金凤等: "减压蒸馏辅助熔融结晶分离技术制备高纯二甲基亚砜", 《化学试剂》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115784952A (en) * | 2022-10-09 | 2023-03-14 | 新疆兴发化工有限公司 | Purification process of electronic grade dimethyl sulfoxide |
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