CN113200823B - Preparation method of benzyl alcohol with low peroxide value - Google Patents
Preparation method of benzyl alcohol with low peroxide value Download PDFInfo
- Publication number
- CN113200823B CN113200823B CN202110473598.6A CN202110473598A CN113200823B CN 113200823 B CN113200823 B CN 113200823B CN 202110473598 A CN202110473598 A CN 202110473598A CN 113200823 B CN113200823 B CN 113200823B
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- China
- Prior art keywords
- benzyl alcohol
- molecular distillation
- distillation device
- peroxide value
- vacuum degree
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- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 title claims abstract description 141
- 235000019445 benzyl alcohol Nutrition 0.000 title claims abstract description 47
- 150000002978 peroxides Chemical class 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000000199 molecular distillation Methods 0.000 claims abstract description 43
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims abstract description 32
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 5
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims description 6
- 239000000047 product Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 230000000202 analgesic effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003889 eye drop Substances 0.000 description 1
- 230000001976 improved effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000008177 pharmaceutical agent Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C33/00—Unsaturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
- C07C33/18—Monohydroxylic alcohols containing only six-membered aromatic rings as cyclic part
- C07C33/20—Monohydroxylic alcohols containing only six-membered aromatic rings as cyclic part monocyclic
- C07C33/22—Benzylalcohol; phenethyl alcohol
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of benzyl alcohol with a low peroxide value, which is characterized by comprising the following steps: (1) Setting heating temperature and condensing temperature of the molecular distillation device, starting a vacuum system, and adjusting vacuum degree of the molecular distillation device and parameters of a balance system; (2) After each parameter of the molecular distillation device is stable, industrial grade benzyl alcohol is conveyed to the molecular distillation device through a material conveying pump at a certain speed, molecular distillation is carried out at a set temperature and vacuum degree, and intermediate components obtained by molecular distillation are collected, so that a benzyl alcohol product is obtained. The peroxide value and the benzaldehyde content of the benzyl alcohol product prepared by the method are obviously reduced, the peroxide value is not detected, and the benzaldehyde content can reach below 0.01%.
Description
Technical Field
The invention belongs to the technical field of chemical medicine preparation, and particularly relates to a preparation method of benzyl alcohol with a low peroxide value.
Background
Benzyl alcohol is a colorless transparent viscous liquid with weak aromatic smell, slightly soluble in water (4 g/100 mL), and miscible with organic solvents such as ethanol, diethyl ether, benzene, chloroform, etc. Benzyl alcohol is used as a preservative and as a local analgesic in pharmaceutical agents. In the aqueous solution or the oily preparation, the dosage can reach 20 percent, 0.5 to 1.0 percent of the eye drop can be used, and 5 to 20 percent of the cosolvent can be used. The quality requirement of the medicament on benzyl alcohol is higher, and the structure and properties of impurity benzaldehyde in the benzyl alcohol are similar to those of benzyl alcohol, so that the general purification method for removing benzaldehyde is difficult to reach the pharmaceutical grade requirement.
At present, benzyl alcohol produced by the traditional process mainly has the following defects: 1. the peroxide value of benzyl alcohol produced by the traditional process is generally higher; 2. the molecular structure of benzaldehyde is similar to that of benzyl alcohol, the boiling point difference is not large, and the high-efficiency and complete separation is difficult to realize by common rectification; 3. the traditional method for removing benzaldehyde in benzyl alcohol generally adds a catalyst and needs high-temperature reaction to reduce the benzaldehyde into benzyl alcohol, so that other impurities are easy to introduce, and the benzyl alcohol is easy to oxidize and discolor when heated for a long time, so that more impurities are generated.
The prior art also discloses a device and a method for purifying benzyl alcohol. For example, patent CN202526927U reports an apparatus for producing benzyl alcohol of high purity; patent CN207904157U discloses a benzyl alcohol continuous rectification system; patent CN108821948U discloses a method for recycling benzyl alcohol rectification byproducts. However, the removal effect of the impurity benzaldehyde is not given in the prior art. At present, no report of reducing peroxide value of benzyl alcohol is known.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of benzyl alcohol with a low peroxide value. The method mainly adopts a molecular distillation purification method, and mainly solves the problems that the peroxide value in benzyl alcohol is higher and the benzaldehyde is difficult to remove.
The aim and the technical problems of the invention are realized by adopting the following technical proposal.
The invention provides a preparation method of benzyl alcohol with a low peroxide value, which is characterized by comprising the following steps:
(1) Setting heating temperature and condensing temperature of the molecular distillation device, starting a vacuum system, and adjusting vacuum degree of the molecular distillation device and parameters of a balance system;
(2) After each parameter of the molecular distillation device is stable, industrial grade benzyl alcohol is conveyed to the molecular distillation device through a material conveying pump at a certain speed, molecular distillation is carried out at a set temperature and vacuum degree, and intermediate components obtained by molecular distillation are collected, so that a benzyl alcohol product is obtained.
Preferably, the heating temperature of the molecular distillation device is 60-66 ℃, and the condensing temperature is 0-5 ℃.
Preferably, the vacuum degree of the molecular distillation device is 1-50 Pa.
More preferably, the vacuum degree of the molecular distillation device is 1-10 Pa.
More preferably, the vacuum degree of the molecular distillation device is 1-5 Pa.
The aim and the technical problems of the invention are also realized by adopting the following technical proposal.
The invention also provides benzyl alcohol with a low peroxide value, which is characterized by being prepared by the method.
Preferably, no peroxide value is detected in the benzyl alcohol, and the content of benzaldehyde is less than or equal to 0.01%.
By means of the technical scheme, the invention has at least the following advantages: the invention adopts molecular distillation technology to reduce the peroxide value of benzyl alcohol and simultaneously reduce the content of benzaldehyde in benzyl alcohol, thus obtaining a benzyl alcohol product with low peroxide value and low benzaldehyde. The molecular distillation has the advantages of high vacuum degree, low distillation temperature, short heating time and the like, can keep the naturalness of materials, avoid the heating and oxidization of the materials, and meanwhile, does not need to use chemical solvents, catalysts and the like, thereby being a low-carbon and green process. The peroxide value and the benzaldehyde content of the benzyl alcohol product prepared by the method are obviously reduced, the peroxide value is not detected, and the benzaldehyde content can reach below 0.01%.
In summary, the preparation method of the present invention has many advantages and practical values, and does not see similar design disclosure or use in similar products, which is an innovation, has great improvements in product components or functions, has great improvements in technology, and produces good use and practical effects, and has improved effects compared with the existing preparation methods, so that the preparation method is more suitable for practical use, has wide industrial use value, and is a novel, advanced and practical new design.
The foregoing description is only an overview of the present invention, and is intended to provide a more thorough understanding of the present invention, and is to be accorded the full scope of the present invention.
Specific embodiments of the present invention are given in detail by the following examples.
Detailed Description
In order to further describe the technical means and effects adopted by the invention to achieve the preset aim, the following is a detailed description of the specific implementation, the method and the effects of the auxiliary agent and the prepared double grass aqua according to the invention in combination with the preferred embodiment.
Example 1
Setting the heating temperature of the molecular distillation device at 60 ℃ and the condensing temperature at 5 ℃, starting a vacuum system, adjusting the vacuum degree of the molecular distillation device to be 1Pa, and balancing system parameters. Benzyl alcohol is added into a molecular distillation device at a certain speed, the feeding speed is used for ensuring that molecular distillation is stable to form a film, and a light-component benzyl alcohol sample is collected. The results of the detection of the benzyl alcohol obtained are shown in Table 1.
Example 2
Setting the heating temperature of the molecular distillation device at 62 ℃ and the condensing temperature at 0 ℃, starting a vacuum system, adjusting the vacuum degree of the molecular distillation device to 5Pa, and balancing system parameters. Benzyl alcohol is added into a molecular distillation device at a certain speed, the feeding speed is used for ensuring that molecular distillation is stable to form a film, and a light-component benzyl alcohol sample is collected. The results of the detection of the benzyl alcohol obtained are shown in Table 1.
Example 3
Setting the heating temperature of the molecular distillation device to 65 ℃ and the condensing temperature to 3 ℃, starting a vacuum system, adjusting the vacuum degree of the molecular distillation device to 10Pa, and balancing system parameters. Benzyl alcohol is added into a molecular distillation device at a certain speed, the feeding speed is used for ensuring that molecular distillation is stable to form a film, and a light-component benzyl alcohol sample is collected. The results of the detection of the benzyl alcohol obtained are shown in Table 1.
Example 4
Setting the heating temperature of the molecular distillation device at 68 ℃ and the condensing temperature at 5 ℃, starting a vacuum system, adjusting the vacuum degree of the molecular distillation device to 50Pa, and balancing system parameters. Benzyl alcohol is added into a molecular distillation device at a certain speed, the feeding speed is used for ensuring that molecular distillation is stable to form a film, and a light-component benzyl alcohol sample is collected. The results of the detection of the benzyl alcohol obtained are shown in Table 1.
The benzyl alcohol test results prepared in examples 1-4 above are shown in Table 1:
TABLE 1 detection results of benzyl alcohol finished products
As can be seen from the results of Table 1, benzyl alcohol obtained by the preparation method according to the present invention has a detected peroxide value, and the content of benzaldehyde is far below the standard. The yield is also higher.
While the invention has been described with respect to preferred embodiments, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention, and that any such changes and modifications as described in the above embodiments are intended to be within the scope of the invention.
Claims (1)
1. A preparation method of benzyl alcohol with a low peroxide value is characterized in that no peroxide value is detected in the benzyl alcohol, and the content of benzaldehyde is less than or equal to 0.01 percent, and the method comprises the following steps:
(1) Setting heating temperature and condensing temperature of the molecular distillation device, starting a vacuum system, and adjusting vacuum degree of the molecular distillation device and parameters of a balance system;
(2) After each parameter of the molecular distillation device is stable, industrial grade benzyl alcohol is conveyed to the molecular distillation device through a material conveying pump at a certain speed, molecular distillation is carried out at a set temperature and vacuum degree, and intermediate components obtained by molecular distillation are collected, namely benzyl alcohol products;
the heating temperature of the molecular distillation device is 60-66 ℃, and the condensing temperature is 0-5 ℃;
the vacuum degree of the molecular distillation device is 1-5 Pa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110473598.6A CN113200823B (en) | 2021-04-29 | 2021-04-29 | Preparation method of benzyl alcohol with low peroxide value |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110473598.6A CN113200823B (en) | 2021-04-29 | 2021-04-29 | Preparation method of benzyl alcohol with low peroxide value |
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| Publication Number | Publication Date |
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| CN113200823A CN113200823A (en) | 2021-08-03 |
| CN113200823B true CN113200823B (en) | 2024-02-06 |
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Families Citing this family (1)
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| 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 |
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2021
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