Micro-chemical process for synthesizing o-phenylphenoxyethanol

By using super-rigid carbon dioxide countercurrent extraction, molecular distillation and nanofiltration membrane separation technologies in the microchemical process, the environmental pollution problems caused by the use of a large number of organic solvents in the prior art are solved, and the production of high-purity o-phenylphenoxyethanol is achieved.

CN119954618APending Publication Date: 2025-05-09SICHUAN HONGPENG NEW MATERIALS CO LTD
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Patent Information

Application Number
CN202510349069.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-24
Publication Date
2025-05-09

AI Technical Summary

Technical Problem

The existing production process of o-phenylphenoxyethanol has serious environmental pollution problems, mainly due to the use of a large number of organic solvents, etc.

Method used

Microchemical technology is adopted, including adding alkaline catalyst to orthophenylphenol and Lewis acid to ethylene oxide, preheating and heating reaction in a microchannel reactor, and then processing through supercritical carbon dioxide countercurrent extraction, molecular distillation and nanofiltration membrane separation to obtain high-purity o-phenylphenoxyethanol.

Benefits of technology

It significantly improves the purity and quality of the product, reduces the use and emission of organic solvents, reduces environmental pollution, and realizes integrated post-treatment of catalyst removal, unreacted raw material recovery and product refining.

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Abstract

The invention relates to the technical field of o-phenylphenoxyethanol, and particularly discloses a micro-chemical process for synthesizing o-phenylphenoxyethanol, aiming at the problem of serious environmental pollution caused by the use of a large amount of organic solvent and the like in the existing o-phenylphenoxyethanol production process, which comprises the following steps: adding a basic catalyst into o-phenylphenol, uniformly mixing, and reacting for 2-4 hours at room temperature to obtain o-phenylphenoxyethanol. A premix I is obtained; additionally taking ethylene oxide, adding Lewis acid, and uniformly mixing to obtain a premix II; preheating the premix I and the premix II, introducing the preheated premix I and premix II into a micro-channel reactor for mixing, and carrying out heating reaction to obtain a mixed product containing an o-phenyl phenoxyethanol crude product; cooling the mixed product, adding a stabilizer, filtering, and collecting filtrate; and sequentially carrying out supercritical carbon dioxide countercurrent extraction, molecular distillation and nanofiltration membrane separation treatment on the filtrate to obtain the o-phenylphenoxyethanol. And by combining a plurality of post-treatment technologies, unreacted raw materials, catalysts, byproducts and the like in the product are sequentially removed, so that the use and emission of organic solvents are reduced, and the environmental pollution is reduced.
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Description

Technical Field

[0001] The invention relates to the technical field of o-phenylphenoxyethanol, and in particular to a micro-chemical process for synthesizing o-phenylphenoxyethanol. Background Art

[0002] o-phenylphenoxyethanol refers to an organic compound with a benzene ring connected to a carbon atom with a hydroxyl group, which in turn is connected to a methylene group, which is connected to a phenoxy group. In chemical production, o-phenylphenol is usually used as a reaction base, ethylene oxide or ethylene carbonate is added, and o-phenylphenoxyethanol is generated by reaction under the action of a catalyst. The hydroxyl group of o-phenylphenoxyethanol can undergo esterification, etherification, oxidation and other reactions to introduce different functional groups, so it is usually used in synthesis, pharmaceutical intermediates, pesticide intermediates and other fine chemicals, or as a modifier for certain polymers.

[0003] The purity and other qualities of o-phenylphenoxyethanol directly affect and determine its appearance, color, morphology, and performance, so how to prepare high-quality o-phenylphenoxyethanol is an important issue in chemical technology. For example, the patent with publication number CN119552060A discloses a method for preparing high-purity o-phenylphenoxyethanol, wherein o-phenylphenol and ethylene carbonate are reacted in the presence of a catalyst to obtain a crude o-phenylphenoxyethanol product, and then the crude o-phenylphenoxyethanol product is dissolved in an organic solvent, an anti-solvent is added, and the temperature is reduced for crystallization to obtain high-purity o-phenylphenoxyethanol.

[0004] However, the existing production process of o-phenylphenoxyethanol, such as the above-mentioned one, only solves the purity and yield problems of o-phenylphenoxyethanol to a certain extent, but it involves the use of a large amount of organic reagents, etc., which has great environmental hazards. Summary of the invention

[0005] The purpose of the present invention is to solve the problem of serious environmental pollution caused by the use of a large amount of organic solvents in the current production process of o-phenylphenoxyethanol.

[0006] The present invention is achieved through the following technical solutions:

[0007] The present invention provides a micro-chemical process for synthesizing o-phenylphenoxyethanol, comprising the following steps:

[0008] S1: adding a basic catalyst to o-phenylphenol and mixing well to obtain a premix Ⅰ; taking ethylene oxide, adding Lewis acid and mixing well to obtain a premix Ⅱ;

[0009] S2 preheats the premix I and the premix II, introduces them into a microchannel reactor for mixing, and heats them for reaction to obtain a mixed product containing crude o-phenylphenoxyethanol;

[0010] S3 cools the mixed product, adds a stabilizer, filters, and collects the filtrate; and then sequentially performs supercritical carbon dioxide countercurrent extraction, molecular distillation, and nanofiltration membrane separation on the filtrate to obtain the o-phenylphenoxyethanol.

[0011] Preferably, in step S3, the specific operating steps of supercritical carbon dioxide countercurrent extraction are as follows: add an extractant to the filtrate, mix well, and send it into an extraction tower, and pass supercritical carbon dioxide to the bottom of the extraction tower to perform countercurrent extraction to precipitate o-phenylphenol and ethylene oxide in the filtrate, and collect the residual liquid remaining after extraction.

[0012] Preferably, during extraction, the pressure in the tower is controlled to be 8-12 MPa and the extraction temperature is controlled to be 40-60° C.; after extraction, the pressure and temperature are reduced to room pressure and room temperature, and the residual liquid is collected.

[0013] Preferably, the specific operation steps of molecular distillation are as follows: the residual liquid after supercritical carbon dioxide extraction is sent to a molecular distiller, molecular distilled at 120-150° C., and the distillate and residue are collected separately.

[0014] Preferably, during molecular distillation, the vacuum degree in the molecular distiller is controlled to be less than 1 Pa.

[0015] Preferably, the specific operation steps of nanofiltration membrane separation are as follows:

[0016] The fraction after molecular distillation is sent to a nanofiltration membrane system, filtered using a nanofiltration membrane with a molecular weight cutoff of 200-400 Da, and the filtered liquid is collected to obtain the o-phenylphenoxyethanol.

[0017] Preferably, during nanofiltration, the pressure is controlled at 0.5-2 MPa.

[0018] Preferably, in step S2, the preheating temperature is 50-80°C, and the temperature during the heating reaction is 80-150°C; in step S3, the mixed product is cooled to 40-50°C.

[0019] Preferably, in step S1, the amount of the basic catalyst added is 0.01-0.1 of the molar mass of o-phenylphenol, and the amount of the Lewis acid added is 0.001-0.05 of the molar mass of ethylene oxide.

[0020] Preferably, the ratio of premix I to premix II is 0.96-1.1:1 by mole.

[0021] The technical solution of the present invention has the following beneficial effects:

[0022] The present invention mainly improves the post-treatment of the crude o-phenylphenoxyethanol product after the synthesis reaction, and sequentially uses different methods to remove different types of by-product impurities, which can significantly improve the purity and quality of the product, and greatly reduces the use and discharge of organic solvents and the like in the post-treatment, which can solve the current serious environmental pollution problem and meet the goals and requirements of green sustainable production.

[0023] Specifically, in the post-processing stage, supercritical carbon dioxide extraction, molecular distillation and nanofiltration membrane separation technology are combined to remove unreacted raw materials, catalysts, high-boiling point by-products, small molecule impurities, etc. in the o-phenylphenoxyethanol product in turn, which can reduce the use and emissions of organic solvents, reduce environmental pollution, and realize integrated post-processing of catalyst removal, unreacted raw material recovery and product refining. It has high processing efficiency, simple operation, low energy consumption, and has a significant effect on improving the purity of the product and collecting and treating harmful substances. DETAILED DESCRIPTION

[0024] In order to make the purpose, technical scheme and advantages of the embodiments of the present invention clearer, the technical scheme in the embodiments of the present invention will be described clearly and completely below. Where specific conditions are not specified in the embodiments, they are carried out under conventional conditions or conditions recommended by the manufacturer; where the manufacturers of the instruments, equipment, reagents and raw materials used are not specified, they are all conventional products that can be purchased commercially.

[0025] The present invention provides a micro-chemical process for synthesizing o-phenylphenoxyethanol, comprising the following steps:

[0026] (1) adding a basic catalyst to o-phenylphenol at a molar ratio of 1:0.01-0.1 and mixing well to obtain a premix I; taking ethylene oxide, adding Lewis acid at a molar ratio of 1:0.001-0.05 and mixing well to obtain a premix II;

[0027] Alkaline catalysts may include sodium hydroxide, potassium hydroxide, sodium carbonate, tertiary amines (such as triethylamine), and the like.

[0028] (2) Premix I and premix II are respectively heated to 50-80° C. for preheating, and then the preheated premix I and premix II are introduced into a microchannel reactor at a molar mass ratio of 0.96-1.1:1 for mixing, heated to 80-150° C., and reacted for 5-20 minutes to obtain a mixed product of crude o-phenylphenoxyethanol.

[0029] (3) cooling the mixed product to 40-50° C., adding a small amount of stabilizer, mixing, and coarsely filtering using a plate and frame filter or a centrifuge to preliminarily remove solid impurities such as catalyst particles in the mixed product, and collecting the filtrate;

[0030] Adding a stabilizer can prevent the o-phenylphenoxyethanol product from being oxidized or polymerized in subsequent processing steps, that is, improve the stability of the product; the stabilizer can be an antioxidant such as BHT.

[0031] (4) adding an extractant, such as ethanol or ethyl acetate (0.5-2wt%), to the filtrate, mixing well, adding the extractant to an extraction tower, and adopting supercritical carbon dioxide (scCO2) countercurrent extraction, that is, introducing scCO2 from the bottom of the extraction tower, discharging it from the top after countercurrent extraction, and introducing it into the bottom of the extraction tower again after being treated by a compressor to achieve recycling; during extraction, the pressure in the tower is controlled to be 8-12MPa, and the extraction temperature is 40-60°C; after extraction, the pressure and temperature are reduced to room temperature, and the o-phenylphenol and ethylene oxide that are not involved in the synthesis are precipitated and recovered, and can be reused to reduce production costs, and the remaining residual liquid is recovered and processed in the next step.

[0032] Supercritical carbon dioxide countercurrent extraction has the advantages of being non-toxic, easy to separate, and having mild operating conditions. The extraction efficiency is further improved under the action of the extractant, and it can also reduce organic solvent emissions and environmental pollution.

[0033] (5) sending the residual liquid after supercritical carbon dioxide extraction into a molecular distiller, spreading the material into a thin film by a scraper or a turntable, and performing molecular distillation under the conditions of vacuum degree <1Pa and temperature of 120-150°C, and collecting the distillate and the residue respectively; wherein the distillate is the o-phenylphenoxyethanol product, and the residue is the high-boiling point by-products such as diethoxylate of o-phenylphenol and polyethylene glycol, and a large amount of by-product impurities can be removed by molecular distillation, thereby improving the product purity of o-phenylphenoxyethanol.

[0034] Molecular distillation can be operated at extremely low temperatures, which can reduce the risk of thermal decomposition of the o-phenylphenoxyethanol product while achieving efficient separation.

[0035] (6) The fraction obtained by distillation separation is sent to a nanofiltration membrane system, a nanofiltration membrane with a molecular weight cutoff of 200-400 Da is selected, and filtration is performed at a pressure of 0.5-2 MPa to remove the residual Na + , K + The catalytic ions and small molecular impurities are removed, and the filtered liquid is collected, decolorized with activated carbon, placed in a nitrogen environment, and stored away from light to obtain a high-purity o-phenylphenoxyethanol product.

[0036] Example 1

[0037] Take 511g of o-phenylphenol and 6g of sodium hydroxide, mix them evenly to obtain premix I; take 132g of ethylene oxide and 8g of aluminum chloride, mix them evenly to obtain premix II; heat premix I and premix II to 75±3°C respectively, and then pass them into a microchannel reactor for mixing reaction, and the reaction is heated to 120±5°C and reacted for 12 minutes to obtain a mixed product containing crude o-phenylphenoxyethanol.

[0038] The mixed product obtained by the above reaction was cooled to 45±3°C, 22g of antioxidant BHT was added, and after mixing, it was coarsely filtered with a plate-frame filter, and the filtrate was collected; 1.2wt% ethanol or ethyl acetate was added to the filtrate, and after mixing, it was sent to an extraction tower, and scCO2 was introduced to the bottom of the extraction tower for countercurrent extraction, and the pressure in the tower was controlled to be 10MPa during extraction, and the extraction temperature was controlled to be 50±3°C. After the extraction was completed, it was reduced to room pressure and room temperature, and then the residual liquid remaining after extraction was collected; the residual liquid was sent to The product was put into a molecular distiller, and the material was spread into a thin film by a scraper. Under the conditions of vacuum degree <1Pa and temperature of 135±5°C, molecular distillation was carried out, and the fractions and residues were collected; the fractions were sent to a nanofiltration membrane system, and filtered at a pressure of 1.5MPa using a nanofiltration membrane with a molecular weight cutoff of 300Da. The filtered liquid was collected, placed in a nitrogen environment, and stored in a cool place away from light to obtain 624g of o-phenylphenoxyethanol product, and its purity was 99.8% as determined by GC-FID method.

[0039] Example 2

[0040] Take 511 g of o-phenylphenol and 6.1 g of sodium hydroxide, mix them evenly to obtain premix I; take 132 g of ethylene oxide and 8 g of Lewis acid, mix them evenly to obtain premix II; respectively introduce premix I and premix II into a microchannel reactor for mixing reaction, and heat the reaction to 120±5°C for 12 minutes to obtain a mixed product containing crude o-phenylphenoxyethanol.

[0041] The mixed product obtained by the above reaction is cooled to room temperature, 22g of antioxidant BHT is added, and after mixing, it is roughly filtered with a plate and frame filter to collect the filtrate; 1.2wt% ethanol or ethyl acetate is added to the filtrate, and after mixing, it is sent to an extraction tower, and scCO2 is introduced to the bottom of the extraction tower for countercurrent extraction, and the pressure in the tower is controlled to be 10MPa during extraction, and the extraction temperature is 50±3°C. After the extraction is completed, it is reduced to room pressure and room temperature, and then the residual liquid remaining after the extraction is collected; the residual liquid is sent to a molecular distiller, and the material is spread into a thin film by a scraper, and molecular distillation is performed under the conditions of vacuum degree <1Pa and temperature of 135±5°C, and the fraction and residue are collected; the fraction is sent to a nanofiltration membrane system, and a nanofiltration membrane with a molecular weight cutoff of 300Da is used for filtering at a pressure of 1.5MPa, and the filtered liquid is collected, placed in a nitrogen environment, and stored in a cool place away from light to obtain 622g of o-phenylphenoxyethanol product, and its purity is 99.2% as determined by GC-FID method.

[0042] Example 3

[0043] Take 511 g of o-phenylphenol and 2 g of sodium hydroxide, mix them evenly to obtain premix I; take 132 g of ethylene oxide and 2 g of Lewis acid, mix them evenly to obtain premix II; heat premix I and premix II to 75±3° C. respectively, and then pass them into a microchannel reactor for mixing reaction, and the reaction is heated to 120±5° C. and reacted for 18 minutes to obtain a mixed product containing crude o-phenylphenoxyethanol.

[0044] The mixed product obtained by the above reaction was cooled to 45±3°C, 10g of antioxidant BHT was added, and after mixing, it was coarsely filtered with a plate-frame filter, and the filtrate was collected; 1.2wt% ethanol or ethyl acetate was added to the filtrate, and after mixing, it was sent to an extraction tower, and scCO2 was introduced to the bottom of the extraction tower for countercurrent extraction, and the pressure in the tower was controlled to be 10MPa during extraction, and the extraction temperature was controlled to be 50±3°C. After the extraction was completed, it was reduced to room pressure and room temperature, and then the residual liquid remaining after extraction was collected; the residual liquid was sent to The product was put into a molecular distiller, and the material was spread into a thin film by a scraper. Under the conditions of vacuum degree <1Pa and temperature of 135±5°C, molecular distillation was carried out, and the fractions and residues were collected; the fractions were sent to a nanofiltration membrane system, and filtered at a pressure of 1.5MPa using a nanofiltration membrane with a molecular weight cutoff of 300Da. The filtered liquid was collected, placed in a nitrogen environment, and stored in a cool place away from light to obtain 619g of o-phenylphenoxyethanol product, and its purity was 99.4% as determined by GC-FID method.

[0045] Comparative Example 1

[0046] Take 511g of o-phenylphenol and 6g of sodium hydroxide, mix them evenly to obtain premix I; take 132g of ethylene oxide and 8g of Lewis acid, mix them evenly to obtain premix II; heat premix I and premix II to 75±3°C respectively, and then pass them into a microchannel reactor for mixing reaction, and the reaction is heated to 120±5°C and reacted for 12 minutes to obtain a mixed product containing crude o-phenylphenoxyethanol.

[0047] The mixed product obtained by the above reaction is cooled to 45±3°C, 22g of antioxidant BHT is added, and after mixing, it is roughly filtered with a plate and frame filter to collect the filtrate; then 1.2wt% ethanol or ethyl acetate is added to the filtrate, and after mixing, it is sent to an extraction tower, and scCO2 is introduced to the bottom of the extraction tower for countercurrent extraction, and the pressure in the tower is controlled to be 10MPa during extraction, and the extraction temperature is 50±3°C. After the extraction is completed, it is reduced to room pressure and room temperature, and then the residual liquid remaining after the extraction is collected; the residual liquid is sent to a molecular distiller, and the material is spread into a thin film by a scraper, and molecular distillation is performed under the conditions of vacuum degree <1Pa and temperature of 135±5°C, and the fractions are collected, and they are placed in a nitrogen environment and stored in a cool place away from light to obtain 620g of o-phenylphenoxyethanol product, and its purity is 98.0% as determined by GC-FID method.

[0048] Comparative Example 2

[0049] Take 511g of o-phenylphenol and 6g of sodium hydroxide, mix them evenly to obtain premix I; take 132g of ethylene oxide and 8g of aluminum chloride, mix them evenly to obtain premix II; heat premix I and premix II to 75±3°C respectively, and then pass them into a microchannel reactor for mixing reaction, and the reaction is heated to 120±5°C and reacted for 12 minutes to obtain a mixed product containing crude o-phenylphenoxyethanol.

[0050] The mixed product obtained by the above reaction is cooled to 45±3°C, 22g of antioxidant BHT is added, and after mixing, it is coarsely filtered with a plate and frame filter to collect the filtrate; then 1.2wt% ethanol or ethyl acetate is added to the filtrate, and after mixing, it is sent to an extraction tower, and scCO2 is introduced into the bottom of the extraction tower for countercurrent extraction. During the extraction, the pressure in the tower is controlled to be 10MPa, and the extraction temperature is 50±3°C. After the extraction is completed, it is cooled to room temperature, and then the residual liquid remaining after the extraction is collected, and it is placed in a nitrogen environment and stored in a cool place away from light to obtain 619g of o-phenylphenoxyethanol product, and its purity is 97.3% as determined by GC-FID method.

[0051] Comparative Example 3

[0052] Take 511g of o-phenylphenol and 6g of sodium hydroxide, mix them evenly to obtain premix I; take 132g of ethylene oxide and 8g of Lewis acid, mix them evenly to obtain premix II; heat premix I and premix II to 75±3°C respectively, and then pass them into a microchannel reactor for mixing reaction, and the reaction is heated to 120±5°C and reacted for 12 minutes to obtain a mixed product containing crude o-phenylphenoxyethanol.

[0053] The mixed product obtained by the above reaction was cooled to 45±3°C, 22g of antioxidant BHT was added, and after mixing, it was filtered with a plate and frame filter, the filtrate was collected, and placed in a nitrogen environment and stored in a cool place away from light to obtain 616g of o-phenylphenoxyethanol product, and its purity was 96.5% as determined by GC-FID method.

[0054] Comparative Example 4

[0055] Take 511g of o-phenylphenol, 132g of ethylene oxide and 10g of sodium hydroxide, mix them evenly, and then pass them into a microchannel reactor for a mixing reaction. The reaction is heated to 120±5°C and reacted for 12min to obtain a mixed product containing a crude product of o-phenylphenoxyethanol.

[0056] The mixed product obtained by the above reaction was cooled to 45±3°C, 22g of antioxidant BHT was added, and after mixing, it was coarsely filtered with a plate-frame filter, and the filtrate was collected; 1.2wt% ethanol or ethyl acetate was added to the filtrate, and after mixing, it was sent to an extraction tower, and scCO2 was introduced to the bottom of the extraction tower for countercurrent extraction, and the pressure in the tower was controlled to be 10MPa during extraction, and the extraction temperature was controlled to be 50±3°C. After the extraction was completed, it was reduced to room pressure and room temperature, and then the residual liquid remaining after extraction was collected; the residual liquid was sent to The product was put into a molecular distiller, and the material was spread into a thin film by a scraper. Under the conditions of vacuum degree <1Pa and temperature of 135±5°C, molecular distillation was carried out, and the fractions and residues were collected; the fractions were sent to a nanofiltration membrane system, and filtered at a pressure of 1.5MPa using a nanofiltration membrane with a molecular weight cutoff of 300Da. The filtered liquid was collected, placed in a nitrogen environment, and stored in a cool place away from light to obtain 612g of o-phenylphenoxyethanol product, and its purity was 97.8% as determined by GC-FID method.

[0057] Comparative Example 5

[0058] Take 511g of o-phenylphenol, 132g of ethylene oxide and 10g of sodium hydroxide, mix them evenly, and then pass them into a microchannel reactor for a mixing reaction. The reaction is heated to 120±5°C and reacted for 12min to obtain a mixed product containing a crude product of o-phenylphenoxyethanol.

[0059] The mixed product obtained by the above reaction was cooled to 45±3° C., 22 g of antioxidant BHT was added, and the mixture was filtered using a plate and frame filter. The filtrate was collected and placed in a nitrogen environment and stored in a cool place away from light to obtain 609 g of o-phenylphenoxyethanol product, which had a purity of 96.3% as determined by GC-FID.

[0060] It can be seen from the above Examples 1-3 and Comparative Examples 1-5 that Examples 1-3 adopt the micro-chemical process for synthesizing o-phenylphenoxyethanol proposed by the present invention, and in the post-treatment process of crude product purification, the introduction of harmful pollutants such as organic solvents is avoided, and the purity of the o-phenylphenoxyethanol product after treatment is significantly improved, which can illustrate that the micro-chemical process for synthesizing o-phenylphenoxyethanol provided by the present invention can not only achieve high-purification treatment of o-phenylphenoxyethanol products, but also control the emission of harmful substances generated during the treatment process, that is, reduce the environmental hazards caused by chemical production.

[0061] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A micro-chemical process for synthesizing o-phenylphenoxyethanol, characterized in that: The following steps are involved: S1: adding a basic catalyst to o-phenylphenol and mixing well to obtain a premix Ⅰ; taking ethylene oxide, adding Lewis acid and mixing well to obtain a premix Ⅱ; S2 preheats the premix I and the premix II, introduces them into a microchannel reactor for mixing, and heats them for reaction to obtain a mixed product containing crude o-phenylphenoxyethanol; S3 cools the mixed product, adds a stabilizer, filters, and collects the filtrate; and then sequentially performs supercritical carbon dioxide countercurrent extraction, molecular distillation, and nanofiltration membrane separation on the filtrate to obtain the o-phenylphenoxyethanol.

2. The micro-chemical process for synthesizing o-phenylphenoxyethanol according to claim 1, characterized in that: In step S3, the specific operation steps of supercritical carbon dioxide countercurrent extraction are as follows: Add an extractant to the filtrate, mix well, and send it into an extraction tower. Supercritical carbon dioxide is introduced into the bottom of the extraction tower to perform countercurrent extraction to precipitate o-phenylphenol and ethylene oxide in the filtrate, and collect the residual liquid remaining after extraction.

3. The micro-chemical process for synthesizing o-phenylphenoxyethanol according to claim 2, characterized in that: During extraction, the pressure in the tower is controlled to be 8-12MPa and the extraction temperature is 40-60°C; after extraction, the pressure and temperature are reduced to room pressure and room temperature, and the residual liquid is collected.

4. The micro-chemical process for synthesizing o-phenylphenoxyethanol according to claim 2, characterized in that: The specific steps of molecular distillation are as follows: The residual liquid after supercritical carbon dioxide extraction is sent to a molecular distiller for molecular distillation at 120-150°C, and the distillate and residue are collected separately.

5. The micro-chemical process for synthesizing o-phenylphenoxyethanol according to claim 4, characterized in that: During molecular distillation, control the vacuum degree in the molecular distiller to be less than 1Pa.

6. The micro-chemical process for synthesizing o-phenylphenoxyethanol according to claim 4, characterized in that: The specific operation steps of nanofiltration membrane separation are as follows: The fraction after molecular distillation is sent to a nanofiltration membrane system, filtered using a nanofiltration membrane with a molecular weight cutoff of 200-400 Da, and the filtered liquid is collected to obtain the o-phenylphenoxyethanol.

7. The micro-chemical process for synthesizing o-phenylphenoxyethanol according to claim 6, characterized in that: When filtering with nanofiltration membrane, the pressure is controlled at 0.5-2MPa.

8. The micro-chemical process for synthesizing o-phenylphenoxyethanol according to claim 1, characterized in that: In step S2, the preheating temperature is 50-80°C, and the temperature during the heating reaction is 80-150°C; in step S3, the mixed product is cooled to 40-50°C.

9. The micro-chemical process for synthesizing o-phenylphenoxyethanol according to claim 1, characterized in that: In step S1, the amount of the basic catalyst added is 0.01-0.1 of the molar mass of o-phenylphenol, and the amount of the Lewis acid added is 0.001-0.05 of the molar mass of ethylene oxide.

10. The micro-chemical process for synthesizing o-phenylphenoxyethanol according to claim 9, characterized in that: Based on molar mass, the dosage ratio of premix I to premix II is 0.96-1.1:1.

Citation Information

Patent Citations

  • Preparation method of high-purity o-phenyl phenoxyethanol

    CN119552060A