CN111269088A - Preparation method of anhydrous ethanol for medicine - Google Patents
Preparation method of anhydrous ethanol for medicine Download PDFInfo
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- CN111269088A CN111269088A CN202010161321.5A CN202010161321A CN111269088A CN 111269088 A CN111269088 A CN 111269088A CN 202010161321 A CN202010161321 A CN 202010161321A CN 111269088 A CN111269088 A CN 111269088A
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- ethanol
- molecular sieve
- anhydrous ethanol
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C31/00—Saturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
- C07C31/02—Monohydroxylic acyclic alcohols
- C07C31/08—Ethanol
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of ethanol purification, and provides a preparation method of absolute ethanol for medicines, which at least comprises the following steps: (1) taking 95% ethanol raw material in a distillation still, heating and evaporating, and passing through a molecular sieve column to obtain first ethanol; (2) adding a water removing agent into the ethanol at the first stage, heating, refluxing and collecting to obtain second ethanol; (3) adding the second ethanol into a reaction kettle, adding a dewatering oxidant, heating to 60-70 ℃, and distilling the reflux liquid to obtain third ethanol; (4) adding a dehydrating agent into absolute ethyl alcohol, stirring and dispersing for 24-48 hours, distilling and collecting reflux liquid, and enabling the reflux liquid to pass through a molecular sieve column to obtain the absolute ethyl alcohol for medicines.
Description
Technical Field
The invention relates to the technical field of ethanol purification, in particular to a preparation method of absolute ethanol for medicines.
Background
The main component of medical alcohol is ethanol, and it is a mixture. The medical alcohol is made up by using starch plant through the processes of saccharification, secondary fermentation and distillation, and is equivalent to the process of making wine, but its distillation temp. is lower than that of wine, its distillation number is more than that of wine, alcohol content is high, and the yield of finished product is high, and the ether and aldehyde components other than alcohol are more than that of wine, so that it can not be drunk, but can be contacted with human body for medical purpose. The medical absolute ethyl alcohol is different from industrial absolute ethyl alcohol and chemical reagent absolute ethyl alcohol (chemical purity or analytical purity and the like), the medical absolute ethyl alcohol must meet the quality control requirement of the medical absolute ethyl alcohol, and the limit of impurity content is strictly limited except that the content of the ethyl alcohol is more than or equal to 99.5 percent, such as less than or equal to 0.5 percent of water, less than or equal to 0.2 percent of methanol and less than or equal to 10ppm of esters. The main preparation method of the absolute ethyl alcohol comprises the following steps: chemical dehydration of calcium lime, catalytic cracking synthesis, solvent-water method, adsorption dehydration by resin or molecular sieve, etc. However, the existing method for purifying medical alcohol is simple, can not remove some organic small molecules in the medical alcohol, and has certain influence on the use of the medical alcohol.
Disclosure of Invention
In order to solve the above technical problems, a first aspect of the present invention provides a method for preparing anhydrous ethanol for use in medicine, comprising at least the steps of:
(1) taking 95% ethanol raw material in a distillation still, heating and evaporating, and passing through a molecular sieve column to obtain first ethanol;
(2) adding a water removing agent into the ethanol at the first stage, heating, refluxing and collecting to obtain second ethanol;
(3) adding the second ethanol into a reaction kettle, adding a dewatering oxidant, heating to 60-70 ℃, and distilling the reflux liquid to obtain third ethanol;
(4) adding a dehydrating agent into absolute ethyl alcohol, stirring and dispersing for 24-48 hours, distilling and collecting reflux liquid, and enabling the reflux liquid to pass through a molecular sieve column to obtain the absolute ethyl alcohol for medicines.
As a preferable technical scheme, the addition amount of the water removing agent is 10-25% of the mass of the ethanol raw material.
As a preferable technical scheme, the water removal agent in the invention is at least one selected from silica gel, quicklime and attapulgite.
As a preferable technical scheme, the addition amount of the water removal oxidizing agent is 0.005-0.05% of the mass of the ethanol raw material.
As a preferred technical scheme, the water removal oxidant is concentrated sulfuric acid and/or potassium permanganate.
As a preferred technical scheme, the weight ratio of the concentrated sulfuric acid to the potassium permanganate in the invention is (1-5): 1.
in a preferred embodiment of the present invention, the dehydrating agent is at least one selected from mesoporous silica and mesoporous alumina.
As a preferred technical scheme, the filler in the molecular sieve column is a 3A type molecular sieve and/or a 4A type molecular sieve.
As a preferable technical solution, the distillation temperature in the step (4) in the present invention is 70 to 90 ℃.
The second aspect of the invention provides medical alcohol prepared by the preparation method of the absolute ethyl alcohol for medicine.
Compared with the prior art, the invention has the following excellent beneficial effects:
the invention provides a preparation method of medical absolute ethyl alcohol, which is mainly used for further purifying, separating and refining the ethyl alcohol.
Detailed Description
The technical features of the technical solutions provided by the present invention will be further clearly and completely described below with reference to the specific embodiments, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The words "preferred", "preferably", "more preferred", and the like, in the present invention, refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
The invention provides a preparation method of absolute ethyl alcohol for medicine, which at least comprises the following steps:
(1) taking 95% ethanol raw material in a distillation still, heating and evaporating, and passing through a molecular sieve column to obtain first ethanol;
(2) adding a water removing agent into the ethanol at the first stage, heating, refluxing and collecting to obtain second ethanol;
(3) adding the second ethanol into a reaction kettle, adding a dewatering oxidant, heating to 60-70 ℃, and distilling the reflux liquid to obtain third ethanol;
(4) adding a dehydrating agent into absolute ethyl alcohol, stirring and dispersing for 24-48 hours, distilling and collecting reflux liquid, and enabling the reflux liquid to pass through a molecular sieve column to obtain the absolute ethyl alcohol for medicines.
In some preferred embodiments, the method for preparing anhydrous ethanol for medicine at least comprises the following steps:
(1) taking 95% ethanol raw material in a distillation still, heating and evaporating, and passing through a molecular sieve column to obtain first ethanol;
(2) adding a water removing agent into the ethanol at the first stage, heating, refluxing and collecting to obtain second ethanol;
(3) adding the second ethanol into a reaction kettle, adding a water-removing oxidant, heating to 65 ℃, and distilling the reflux liquid to obtain third ethanol;
(4) adding a dehydrating agent into absolute ethyl alcohol, stirring and dispersing for 35 hours, distilling and collecting reflux liquid, and enabling the reflux liquid to pass through a molecular sieve column to obtain the absolute ethyl alcohol for medicines.
In some embodiments, the water scavenger is added in an amount of 10-25% by mass of the ethanol feedstock.
In some preferred embodiments, the water scavenger is added in an amount of 20% by mass of the ethanol feedstock.
In some embodiments, the water scavenger is selected from at least one of silica gel, quicklime, attapulgite.
In some preferred embodiments, the water scavenger is selected from silica gel.
In some embodiments, the water-removing oxidizing agent is added in an amount of 0.005 to 0.05% by mass of the ethanol feedstock.
In some preferred embodiments, the water-removing oxidizing agent is added in an amount of 0.01% by mass of the ethanol feedstock.
In some embodiments, the water-removing oxidizing agent is concentrated sulfuric acid and/or potassium permanganate.
In some preferred embodiments, the water-removing oxidizing agent is concentrated sulfuric acid and potassium permanganate.
In some embodiments, the weight ratio of the concentrated sulfuric acid to the potassium permanganate is (1-5): 1.
in some preferred embodiments, the weight ratio of the concentrated sulfuric acid to the potassium permanganate is 3.5: 1.
the concentration of the concentrated sulfuric acid in the invention is 98%.
In some embodiments, the dehydrating agent is selected from at least one of mesoporous silica, mesoporous alumina.
In some preferred embodiments, the dehydrating agent is mesoporous silica.
In some embodiments, the packing in the molecular sieve column is a type 3A molecular sieve and/or a type 4A molecular sieve.
In some preferred embodiments, the packing in the molecular sieve column is a type 3A molecular sieve and a type 4A molecular sieve.
In some embodiments, the weight ratio of the type 3A molecular sieve to the type 4A molecular sieve is 1: (0.1-1).
In some preferred embodiments, the weight ratio of the type 3A molecular sieve to the type 4A molecular sieve is 1: 0.5.
in some embodiments, the distillation temperature in step (4) is 70-90 ℃.
In some preferred embodiments, the distillation temperature in step (4) is 85 ℃.
The second aspect of the invention provides medical alcohol prepared by the preparation method of the absolute ethyl alcohol for medicine.
The present invention is described in detail below by way of examples, and it should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention.
Example 1
A method for preparing anhydrous ethanol for medicine at least comprises the following steps:
(1) taking 95% ethanol raw material in a distillation still, heating and evaporating, and passing through a molecular sieve column to obtain first ethanol;
(2) adding a water removing agent into the ethanol at the first stage, heating, refluxing and collecting to obtain second ethanol;
(3) adding the second ethanol into a reaction kettle, adding a water-removing oxidant, heating to 65 ℃, and distilling the reflux liquid to obtain third ethanol;
(4) adding a dehydrating agent into absolute ethyl alcohol, stirring and dispersing for 35 hours, distilling and collecting reflux liquid, and enabling the reflux liquid to pass through a molecular sieve column to obtain the absolute ethyl alcohol for medicines.
The addition amount of the water removing agent is 20% of the mass of the ethanol raw material. The water removing agent is selected from silica gel. The addition amount of the water removal oxidant is 0.01 percent of the mass of the ethanol raw material. The dewatering oxidant is concentrated sulfuric acid and potassium permanganate. The weight ratio of the concentrated sulfuric acid to the potassium permanganate is 3.5: 1. the dehydrating agent is mesoporous silica. The filler in the molecular sieve column is 3A type molecular sieve and 4A type molecular sieve. The weight ratio of the 3A type molecular sieve to the 4A type molecular sieve is 1: 0.5. the distillation temperature in the step (4) is 85 ℃.
Example 2
A method for preparing anhydrous ethanol for medicine at least comprises the following steps:
(1) taking 95% ethanol raw material in a distillation still, heating and evaporating, and passing through a molecular sieve column to obtain first ethanol;
(2) adding a water removing agent into the ethanol at the first stage, heating, refluxing and collecting to obtain second ethanol;
(3) adding the second ethanol into a reaction kettle, adding a dewatering oxidant, heating to 70 ℃, and distilling the reflux liquid to obtain third ethanol;
(4) adding a dehydrating agent into absolute ethyl alcohol, stirring and dispersing for 48 hours, distilling and collecting reflux liquid, and enabling the reflux liquid to pass through a molecular sieve column to obtain the absolute ethyl alcohol for medicines.
The addition amount of the water removing agent is 10% of the mass of the ethanol raw material. The water removing agent is selected from silica gel. The addition amount of the water removal oxidant is 0.005 percent of the mass of the ethanol raw material. The dewatering oxidant is concentrated sulfuric acid and potassium permanganate. The weight ratio of the concentrated sulfuric acid to the potassium permanganate is 1: 1. the dehydrating agent is mesoporous silica. The filler in the molecular sieve column is 3A type molecular sieve and 4A type molecular sieve. The weight ratio of the 3A type molecular sieve to the 4A type molecular sieve is 1: 0.1. the distillation temperature in the step (4) is 70 ℃.
Example 3
A method for preparing anhydrous ethanol for medicine at least comprises the following steps:
(1) taking 95% ethanol raw material in a distillation still, heating and evaporating, and passing through a molecular sieve column to obtain first ethanol;
(2) adding a water removing agent into the ethanol at the first stage, heating, refluxing and collecting to obtain second ethanol;
(3) adding the second ethanol into a reaction kettle, adding a dewatering oxidant, heating to 60 ℃, and distilling the reflux liquid to obtain third ethanol;
(4) adding a dehydrating agent into absolute ethyl alcohol, stirring and dispersing for 24 hours, distilling and collecting reflux liquid, and enabling the reflux liquid to pass through a molecular sieve column to obtain the absolute ethyl alcohol for medicines.
The addition amount of the water removing agent is 25% of the mass of the ethanol raw material. The water removing agent is selected from silica gel. The addition amount of the water removal oxidant is 0.05 percent of the mass of the ethanol raw material. The dewatering oxidant is concentrated sulfuric acid and potassium permanganate. The weight ratio of the concentrated sulfuric acid to the potassium permanganate is 5: 1. the dehydrating agent is mesoporous silica. The filler in the molecular sieve column is 3A type molecular sieve and 4A type molecular sieve. The weight ratio of the 3A type molecular sieve to the 4A type molecular sieve is 1: 1. the distillation temperature in the step (4) is 90 ℃.
Performance testing
The test results are shown in table 1, examined according to pharmaceutical standards:
TABLE 1 test results
| Examples | Ethanol content (%) | Methanol content (%) | Ester content (%) |
| Example 1 | 99.90 | 99.84 | 99.78 |
| Example 2 | 99.89 | 99.81 | 99.70 |
| Example 3 | 99.86 | 99.76 | 99.67 |
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art may modify or change the technical content disclosed above into an equivalent embodiment with equivalent changes, but all those simple modifications, equivalent changes and modifications made on the above embodiment according to the technical spirit of the present invention still belong to the protection scope of the present invention.
Claims (10)
1. A method for preparing anhydrous ethanol for medicine is characterized by at least comprising the following steps:
(1) taking 95% ethanol raw material in a distillation still, heating and evaporating, and passing through a molecular sieve column to obtain first ethanol;
(2) adding a water removing agent into the ethanol at the first stage, heating, refluxing and collecting to obtain second ethanol;
(3) adding the second ethanol into a reaction kettle, adding a dewatering oxidant, heating to 60-70 ℃, and distilling the reflux liquid to obtain third ethanol;
(4) adding a dehydrating agent into absolute ethyl alcohol, stirring and dispersing for 24-48 hours, distilling and collecting reflux liquid, and enabling the reflux liquid to pass through a molecular sieve column to obtain the absolute ethyl alcohol for medicines.
2. The method for producing anhydrous ethanol for medicine according to claim 1, wherein the amount of the water scavenger added is 10 to 25% by mass of the ethanol raw material.
3. The method for producing anhydrous ethanol for medicine according to claim 1 or 2, wherein the water scavenger is at least one selected from silica gel, quicklime, and attapulgite.
4. The method for producing anhydrous ethanol for pharmaceutical use according to claim 1, wherein the amount of the water-removing oxidizing agent added is 0.005 to 0.05% by mass of the ethanol raw material.
5. The method for producing anhydrous ethanol for use in medicine according to claim 1 or 4, wherein the water-removing oxidizing agent is concentrated sulfuric acid and/or potassium permanganate.
6. The method for producing anhydrous ethanol for use in medicine according to claim 1, 4 or 5, wherein the weight ratio of the concentrated sulfuric acid to the potassium permanganate is (1-5): 1.
7. the method for producing anhydrous ethanol for pharmaceutical use according to claim 1, wherein the dehydrating agent is at least one selected from mesoporous silica and mesoporous alumina.
8. The method for producing anhydrous ethanol for pharmaceutical use according to claim 1, wherein the filler in the molecular sieve column is a 3A type molecular sieve and/or a 4A type molecular sieve.
9. The method for producing anhydrous ethanol for medicine according to claim 1, wherein the distillation temperature in the step (4) is 70 to 90 ℃.
10. A medical alcohol produced by the method for producing anhydrous ethanol for use in medicine according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202010161321.5A CN111269088A (en) | 2020-03-10 | 2020-03-10 | Preparation method of anhydrous ethanol for medicine |
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| CN202010161321.5A CN111269088A (en) | 2020-03-10 | 2020-03-10 | Preparation method of anhydrous ethanol for medicine |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112441879A (en) * | 2020-12-10 | 2021-03-05 | 山东泰和水处理科技股份有限公司 | Method for synthesizing dichloropropanol |
| CN115340444A (en) * | 2022-07-15 | 2022-11-15 | 国药集团国瑞药业有限公司 | Impurity removal method for organic impurities in absolute ethyl alcohol |
| CN115340444B (en) * | 2022-07-15 | 2024-06-07 | 国药集团国瑞药业有限公司 | Impurity removing method for organic impurities in absolute ethyl alcohol |
-
2020
- 2020-03-10 CN CN202010161321.5A patent/CN111269088A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112441879A (en) * | 2020-12-10 | 2021-03-05 | 山东泰和水处理科技股份有限公司 | Method for synthesizing dichloropropanol |
| CN112441879B (en) * | 2020-12-10 | 2022-07-22 | 山东泰和水处理科技股份有限公司 | Method for synthesizing dichloropropanol |
| CN115340444A (en) * | 2022-07-15 | 2022-11-15 | 国药集团国瑞药业有限公司 | Impurity removal method for organic impurities in absolute ethyl alcohol |
| CN115340444B (en) * | 2022-07-15 | 2024-06-07 | 国药集团国瑞药业有限公司 | Impurity removing method for organic impurities in absolute ethyl alcohol |
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Application publication date: 20200612 |
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