CN112299955A - Method for removing benzaldehyde impurities in benzyl alcohol - Google Patents
Method for removing benzaldehyde impurities in benzyl alcohol Download PDFInfo
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- CN112299955A CN112299955A CN202011216095.2A CN202011216095A CN112299955A CN 112299955 A CN112299955 A CN 112299955A CN 202011216095 A CN202011216095 A CN 202011216095A CN 112299955 A CN112299955 A CN 112299955A
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- benzyl alcohol
- rectification system
- benzaldehyde
- impurities
- percent
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- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 title claims abstract description 143
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 235000019445 benzyl alcohol Nutrition 0.000 title claims abstract description 47
- 239000012535 impurity Substances 0.000 title claims abstract description 31
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims abstract description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 5
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 5
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical group [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 5
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 5
- 239000003963 antioxidant agent Substances 0.000 claims description 4
- 230000003078 antioxidant effect Effects 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 238000005273 aeration Methods 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 238000000889 atomisation Methods 0.000 claims 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract description 21
- MHDVGSVTJDSBDK-UHFFFAOYSA-N dibenzyl ether Chemical compound C=1C=CC=CC=1COCC1=CC=CC=C1 MHDVGSVTJDSBDK-UHFFFAOYSA-N 0.000 abstract description 14
- 150000002978 peroxides Chemical class 0.000 abstract description 11
- 239000003814 drug Substances 0.000 abstract description 10
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 abstract description 8
- 229940073608 benzyl chloride Drugs 0.000 abstract description 8
- VSSAZBXXNIABDN-UHFFFAOYSA-N cyclohexylmethanol Chemical compound OCC1CCCCC1 VSSAZBXXNIABDN-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000546 pharmaceutical excipient Substances 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 8
- 229940079593 drug Drugs 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 16
- 230000006872 improvement Effects 0.000 description 9
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229940124531 pharmaceutical excipient Drugs 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
The invention discloses a method for removing benzaldehyde impurities in benzyl alcohol, which comprises the following steps of starting a steam control valve to heat and dry a clean rectification system, introducing nitrogen into the rectification system through an atomizer for 15-30 minutes, and replacing air in the rectification system; adding benzyl alcohol to be refined into a rectification system under the condition of reduced pressure, starting stirring, slowly heating to raise the temperature, controlling the temperature to be 170-220 ℃ and the time to be 30-60min, and discarding collected fractions; under the condition of stirring, a reducing agent is slowly added into the benzyl alcohol in the rectification system, and the amount of distillate is controlled to be 15-30 kg/h. The method has the advantages of simple process, high efficiency, environmental protection and large-scale industrial production; can efficiently remove impurities such as benzaldehyde, cyclohexyl methanol, benzyl chloride, benzyl ether, benzene and the like and peroxide remained in the benzyl alcohol, improve the quality of the benzyl alcohol refined by the content of the benzyl alcohol and meet and exceed the related standard requirements of raw material medicines and pharmaceutic adjuvants, and the content of the benzaldehyde is less than 0.001 percent.
Description
Technical Field
The invention relates to the field of medicine and fine chemical engineering, in particular to a method for removing benzaldehyde impurities in benzyl alcohol.
Background
Benzyl alcohol is used as a raw material drug (or API) and a pharmaceutical adjuvant, and is loaded in pharmacopoeias such as Ch.P 2020 edition (pharmacopoeia of the people's republic of China), USP (United states pharmacopoeia), EP (European pharmacopoeia), BP (British pharmacopoeia) and JP (Japanese pharmacopoeia), wherein the content of benzyl alcohol serving as a key quality characteristic index is not less than 98.0 percent, and the content of impurities such as benzaldehyde, cyclohexyl methanol, benzyl chloride, dibenzyl ether and the like and peroxide are specified in detail; wherein the content of benzaldehyde is less than or equal to 0.05%, cyclohexyl methanol is less than or equal to 0.1%, benzyl chloride is less than or equal to 0.005%, benzyl ether is less than or equal to 0.2%, benzene is less than or equal to 0.0001%, peroxide is less than or equal to 5%, single unknown impurity is less than or equal to 0.01%, total impurity is less than or equal to 0.05%, and water content is less than or equal to 0.5%;
during the production and storage processes, benzyl alcohol is easily oxidized by oxygen or other oxides in the air to generate corresponding aldehydes and acids, so that related substances exceed standards and do not meet the related standard requirements of raw medicines and pharmaceutic adjuvants. At present, benzyl alcohol for raw material medicines (or API) and pharmaceutic adjuvants produced at home and abroad is refined by rectification mostly, key quality characteristic indexes of products meet the standards, and the content of single benzaldehyde is in the range of 0.03-0.05%. The method for removing the benzaldehyde mostly adopts a multi-time rectification method, and is difficult to meet the requirement of higher-purity product quality standard (the content of the benzaldehyde is less than 0.001 percent). Therefore, it is necessary to solve the above-mentioned drawbacks and to develop a benzyl alcohol with a higher quality improvement.
Disclosure of Invention
In order to overcome the problems existing in the prior art, the scheme provides a better method for removing impurities in benzyl alcohol, which is characterized by comprising the following steps:
(1) opening a steam control valve to heat and dry a clean rectification system, introducing nitrogen into the rectification system through a bottom atomizer for 15-30 minutes, and replacing air in the rectification system;
(2) adding benzyl alcohol to be refined into the rectification system under the condition of reduced pressure, starting stirring, slowly heating to raise the temperature, controlling the temperature to be 170-220 ℃ and the time to be 30-60min, and discarding the collected fraction;
(3) slowly adding a reducing agent into the benzyl alcohol in the rectification system under the condition of stirring, controlling the temperature at 170 ℃ and 220 ℃, collecting fractions after 10-60 minutes, and controlling the amount of the fractions to be 15-30 kg/h.
The further improvement is that the nitrogen is subjected to oil removal and water removal treatment, and the purity is more than 99.9%.
The further improvement is that the pressure reducing condition is set between-0.06 MPa and-0.12 MPa.
In a further improvement, the atomizer is a bottom aeration device using a single or multiple air atomizing nozzle array.
The further improvement is that the reducing agent is sodium ethoxide, sodium borohydride, sodium bisulfite or 2, 6-di-tert-butyl-4-cresol antioxidant.
The further improvement is that the dosage of the reducing agent is 0.1-2.0 percent of the mass of the benzyl alcohol to be refined.
The further improvement is that the collection time period of the fraction is that the fraction at the early stage is discarded, and the fraction at the later stage is collected into a finished product.
The further improvement is that the whole rectification process is protected by nitrogen.
Compared with the prior art, the invention has the following advantages:
1. the benzyl alcohol refined and produced by the method has greatly improved product quality, the content of the benzyl alcohol can reach more than 99.5 percent, the content of benzaldehyde is less than or equal to 0.001 percent, the content of cyclohexyl methanol is less than or equal to 0.001 percent, the content of benzyl chloride is less than or equal to 0.0001 percent, the content of dibenzyl ether is less than or equal to 0.005 percent, the content of benzene is less than or equal to 0.00005 percent, the content of peroxide is less than or equal to 0.2 percent, the content of single unknown impurity is less than or equal to 0.005 percent, the content of total impurities is less than; is far higher than the relative standard requirements of pharmacopoeia standards such as Ch.P 2020 edition (pharmacopoeia of the people's republic of China), USP (United states pharmacopoeia), EP (European pharmacopoeia), BP (British pharmacopoeia), JP (Japanese pharmacopoeia) and the like on the raw material medicaments of the p-benzyl alcohol and pharmaceutical excipients;
2. the nitrogen gas protection gas mode of the invention adopts the mode of spraying from the bottom of the rectification equipment to ensure that nitrogen gas is contacted with liquid as much as possible when the nitrogen gas is in the liquid, thereby preventing benzyl alcohol from being further oxidized by contacting with air in the rectification process, and the nitrogen gas is adopted as the circulating gas, thereby reducing the oxidation of the product caused by the contact with oxygen and being beneficial to removing other substances in the product refining process;
3. sodium ethoxide, sodium borohydride, sodium bisulfite reducing agent or BHT antioxidant are selected to reduce residual benzaldehyde and some oxidation components in the benzyl alcohol so as to reduce the content of the benzaldehyde and some oxidation components;
4. at the initial stage of refining, the temperature is kept at 170-220 ℃ for 30 minutes to 2 hours, and nitrogen is introduced for vacuum rectification, so that moisture removal and reduction reaction are facilitated, the content of peroxide is reduced, and the product quality is improved.
5. The production process is simple and easy to control, the purity of the main component of the product is high (more than 99.9 percent), and the organic impurities are as follows: the content of benzaldehyde is reduced to 0.02%, the content of peroxide is lower than 0.02%, and the pharmaceutical raw materials (API) and the standard requirements of auxiliary materials for injection meet the requirements of Ch.P 2020 edition (pharmacopoeia of the people's republic of China), USP (United states pharmacopoeia), EP (European pharmacopoeia), BP (British pharmacopoeia) and JP (Japanese pharmacopoeia).
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely illustrative of some, but not all, of the presently preferred embodiments of the invention, and that the present invention is best described in the specification. This invention may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present disclosure is set forth in order to provide a more thorough understanding thereof. 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.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention.
A method for removing benzaldehyde impurities in benzyl alcohol is characterized by comprising the following steps:
(1) opening a steam control valve to heat and dry a clean rectification system, introducing nitrogen into the rectification system through a bottom atomizer for 15-30 minutes, and replacing air in the rectification system;
(2) adding benzyl alcohol to be refined into the rectification system under the condition of reduced pressure, starting stirring, slowly heating to raise the temperature, controlling the temperature to be 170-220 ℃ and the time to be 30-60min, and discarding the collected fraction;
(3) slowly adding a reducing agent into the benzyl alcohol in the rectification system under the condition of stirring, controlling the temperature at 170 ℃ and 220 ℃, collecting fractions after 10-60 minutes, and controlling the amount of the fractions to be 15-30 kg/h.
The whole rectification process is protected by nitrogen, the nitrogen is subjected to oil removal and water removal treatment, the purity is over 99.9 percent, and the reduced pressure condition is set to be-0.06 to-0.12 MPa. The atomizer is a bottom air-breather which is formed by arranging and combining a single air atomizing nozzle or a plurality of air atomizing nozzles. The reducing agent is sodium ethoxide, sodium borohydride, sodium bisulfite or 2, 6-di-tert-butyl-4-cresol antioxidant, and the dosage of the reducing agent is 0.1-2.0% of the mass of the benzyl alcohol to be refined. The fraction is collected in the early stage and is discarded, and the fraction in the later stage is collected to obtain the final product.
Example 1: nitrogen with the oil and water removal purity of more than 99.9 percent is used for introducing the nitrogen into a clean and dry vacuum rectification system so as to replace the air in the vacuum rectification system; adding benzyl alcohol to be refined into a rectification system under the condition of reduced pressure (-0.06 MPa), protecting with nitrogen gas during rectification, starting stirring and heating, controlling the temperature at 170 deg.C, and maintaining for 30 min; rectifying a certain amount of sodium ethoxide (0.1% of the mass of benzyl alcohol to be refined) at 180 ℃, collecting fractions after 10 minutes, and controlling the amount of the fractions to be 15 kg/h. The product detects that the content of the benzyl alcohol reaches more than 99.8 percent, the content of the benzaldehyde is less than or equal to 0.001 percent, the content of the cyclohexyl methanol is less than or equal to 0.001 percent, the benzyl chloride is less than or equal to 0.0001 percent, the dibenzyl ether is less than or equal to 0.002 percent, the benzene is less than or equal to 0.00005 percent, the peroxide is less than or equal to 0.1 percent, the single unknown impurity is less than or equal to 0.005 percent, the total impurity is less than or equal to.
Example 2: nitrogen is introduced into a clean and dry decompression rectification system by using nitrogen with the oil and water removal purity of more than 99.9 percent to replace the air in the system; adding benzyl alcohol to be refined into the rectification system under reduced pressure (-0.10 MPa), protecting with nitrogen gas during rectification, stirring and heating to control the temperature at 180 deg.C, and maintaining for 50 min; and (3) rectifying a certain amount of sodium bisulfite (0.5 percent of the mass of the benzyl alcohol to be refined) at the temperature of 200 ℃, collecting fractions after 30 minutes, and controlling the amount of the fractions to be 20 kg/h. The product detects that the content of the benzyl alcohol reaches more than 99.7 percent, the content of the benzaldehyde is less than or equal to 0.001 percent, the content of the cyclohexyl methanol is less than or equal to 0.001 percent, the benzyl chloride is less than or equal to 0.0001 percent, the dibenzyl ether is less than or equal to 0.001 percent, the benzene is less than or equal to 0.00005 percent, the peroxide is less than or equal to 0.05 percent, the content of single unknown impurities is less than or equal to 0.005 percent, the total impurities is less than or.
Example 3: nitrogen is introduced into a clean and dry decompression rectification system by using nitrogen with the oil and water removal purity of more than 99.9 percent to replace the air in the system; adding benzyl alcohol to be refined into the rectification system under reduced pressure (-0.06 MPa), protecting with nitrogen gas during rectification, stirring and heating to control its temperature at 200 deg.C, and maintaining for 1 hr; rectifying a certain amount of 2, 6-di-tert-butyl-4-cresol (0.1 percent of the mass of benzyl alcohol to be refined) at 210 ℃, collecting fractions after 1 hour, and controlling the amount of the fractions to be 30 kg/hour. The product detects that the content of the benzyl alcohol reaches more than 99.9 percent, the content of the benzaldehyde is less than or equal to 0.001 percent, the content of the cyclohexyl methanol is less than or equal to 0.001 percent, the benzyl chloride is less than or equal to 0.0001 percent, the dibenzyl ether is less than or equal to 0.001 percent, the benzene is less than or equal to 0.00005 percent, the peroxide is less than or equal to 0.03 percent, the content of single unknown impurities is less than or equal to 0.002 percent, the total impurities are less than or. ,
after the method is adopted for refining, the quality of the benzyl alcohol is greatly improved, and the benzyl alcohol is produced and detected by the people who: the benzyl alcohol content can reach more than 99.5 percent, the benzaldehyde content is less than or equal to 0.001 percent, the cyclohexyl methyl alcohol content is less than or equal to 0.001 percent, the benzyl chloride content is less than or equal to 0.0001 percent, the dibenzyl ether content is less than or equal to 0.005 percent, the benzene content is less than or equal to 0.00005 percent, the peroxide content is less than or equal to 0.2 percent, the single unknown impurity content is less than or equal to 0.005 percent, the total impurity content is less than or equal to 0; is far higher than the relative standard requirements of pharmacopoeia standards such as Ch.P 2020 edition (pharmacopoeia of the people's republic of China), USP (United states pharmacopoeia), EP (European pharmacopoeia), BP (British pharmacopoeia), JP (Japanese pharmacopoeia) and the like on the raw material medicaments of the p-benzyl alcohol and pharmaceutical excipients.
The invention aims to provide a method for removing benzaldehyde impurities in benzyl alcohol, so that the quality of pharmaceutical raw material medicines (or API) and pharmaceutical excipients and perfume-grade products is improved, the medication safety is ensured, and the improvement of the standard of benzyl alcohol products in China is facilitated. The method can overcome the defects of the prior rectification technology, has the advantages of simple process, advanced technology, low price and environmental protection, avoids high energy consumption caused by multiple times of rectification, and also overcomes the defect that the oxide, peroxide and other organic impurities in the product, such as formaldehyde, benzaldehyde and the like, increase along with the extension of the rectification time. Improves the quality and the application of the product, and ensures that the benzyl alcohol product conforms to and meets the application of raw material medicines (API) and pharmaceutic adjuvants, and the use of spices and high-end solvents.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described in the foregoing detailed description, or equivalent changes may be made in some of the features of the embodiments described above. All equivalent structures made by using the content of the specification of the invention can be directly or indirectly applied to other related technical fields, and are also within the protection scope of the patent of the invention.
Claims (8)
1. A method for removing benzaldehyde impurities in benzyl alcohol is characterized by comprising the following steps:
opening a steam control valve to heat and dry a clean rectification system, introducing nitrogen into the rectification system through a bottom atomizer for 15-30 minutes, and replacing air in the rectification system;
adding benzyl alcohol to be refined into the rectification system under the condition of reduced pressure, starting stirring, slowly heating to raise the temperature, controlling the temperature to be 170-220 ℃ and the time to be 30-60min, and discarding the collected fraction;
slowly adding a reducing agent into the benzyl alcohol in the rectification system under the condition of stirring, controlling the temperature at 170 ℃ and 220 ℃, collecting fractions after 10-60 minutes, and controlling the amount of the fractions to be 15-30 kg/h.
2. The method for removing benzaldehyde impurities from benzyl alcohol as claimed in claim 1, wherein the nitrogen gas is subjected to oil removal and water removal treatment to obtain a purity of 99.9% or more.
3. The method for removing benzaldehyde impurities from benzyl alcohol according to claim 2, wherein the reduced pressure condition is set at-0.06 to-0.12 MPa.
4. A method for removing benzaldehyde as an impurity in benzyl alcohol as claimed in claim 3, wherein the atomizer is a bottom aeration device using a single or multiple air atomization nozzle arrangement.
5. The method for removing benzaldehyde impurities from benzyl alcohol as claimed in claim 4, wherein the reducing agent is sodium ethoxide, sodium borohydride, sodium bisulfite or 2, 6-di-tert-butyl-4-cresol antioxidant.
6. The method for removing benzaldehyde impurities in benzyl alcohol according to claim 5, wherein the amount of the reducing agent is 0.1-2.0% of the mass of the benzyl alcohol to be refined.
7. The method for removing benzaldehyde as an impurity in benzyl alcohol, as claimed in claim 6, wherein the fraction is collected during a period of time in which the first fraction is discarded and the second fraction is collected as a final product.
8. The method for removing benzaldehyde impurities in benzyl alcohol according to claim 7, wherein the whole rectification process is protected by nitrogen.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113200823A (en) * | 2021-04-29 | 2021-08-03 | 南京威尔生物科技有限公司 | Preparation method of benzyl alcohol with low peroxide value |
| CN114292159A (en) * | 2021-12-31 | 2022-04-08 | 江苏保易制药有限公司 | Medicinal benzyl alcohol with long storage period and high safety |
| CN115974650A (en) * | 2022-12-15 | 2023-04-18 | 南京化学试剂股份有限公司 | Method for efficiently producing phenethyl alcohol |
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| CN113200823B (en) * | 2021-04-29 | 2024-02-06 | 南京威尔生物科技有限公司 | Preparation method of benzyl alcohol with low peroxide value |
| CN114292159A (en) * | 2021-12-31 | 2022-04-08 | 江苏保易制药有限公司 | Medicinal benzyl alcohol with long storage period and high safety |
| CN115974650A (en) * | 2022-12-15 | 2023-04-18 | 南京化学试剂股份有限公司 | Method for efficiently producing phenethyl alcohol |
| CN115974650B (en) * | 2022-12-15 | 2023-11-24 | 南京化学试剂股份有限公司 | Method for efficiently producing phenethyl alcohol |
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