Preparation method of high-purity phenoxyethanol

Abstract

The invention discloses a preparation method of high-purity phenoxyethanol. The preparation method comprises the following steps: dissolving industrial phenoxyethanol in an organic solvent; performingwashing with alkaline water; and performing cooling and crystallizing to obtain high-purity phenoxyethanol. The phenoxyethanol obtained by the method has high purity (GC purity >= 99.5%, a single impurity <= 0.1%), production can be carried out by conventional equipment, the production cost is low, the process is simple and concise, and thereby the method is easy for industrial production.

Description

technical field

[0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a preparation method of high-purity phenoxyethanol. Background technique

[0002] Phenoxyethanol is a colorless slightly viscous liquid at room temperature, is relatively low in toxicity, and is chemically inactive towards copper and lead. It can be used as a preservative and is widely used in cosmetics, skin care products, vaccines and medicines. Phenoxyethanol has a strong killing effect on Pseudomonas aeruginosa, so it can also be used as a disinfectant for surgical medicine. In addition, it is also widely used in aquaculture, dyes, inks, resins and other fields.

[0003] In the field of medicine, in order to reduce the toxic and side effects of drugs on the human body, not only high requirements are placed on the quality of raw materials, but also high requirements on pharmaceutical excipients. Phenoxyethanol also needs to be of high quality as a su...

Examples

Embodiment 1

[0020] The preparation of embodiment one high-purity phenoxyethanol:

[0021] In a 250ml reaction bottle with a magnet, add 10.0g of industrial phenoxyethanol, 90ml of n-hexane, and 10ml of ethyl acetate, stir to dissolve, add 30ml of 5% aqueous sodium hydroxide solution, stir at room temperature for 0.5-1h, pour the solution Put into a separatory funnel and let stand to separate the liquid. Stir and lower the temperature of the organic layer to -20~-15°C, keep stirring and crystallize for more than 4 hours. Filter, rinse the filter cake with ice n-hexane, and dry to obtain 8.8 g of high-purity phenoxyethanol, with a yield of 88.0%, a GC purity of 99.91%, and a maximum of 0.09% of impurities, such as figure 1 shown.

[0022] With reference to the method of Example 1, the effects of different dissolving solvents or proportions on the product yield and purity were compared and investigated at the same time. Table 1 shows the data comparison results of Comparative Examples 1-4 ...

Embodiment 2

[0038] The preparation of embodiment two high-purity phenoxyethanol:

[0039] In a 50L reaction kettle, add 3.0kg of industrial phenoxyethanol, 17.6kg of n-hexane, and 2.7kg of ethyl acetate, stir to dissolve, add 9.0kg of 5% sodium hydroxide aqueous solution, stir at room temperature for 0.5-1h, and let stand to separate the liquid . The organic layer was cooled down to -15~-20°C under stirring, and kept stirring for more than 4 hours for crystallization. Filter, rinse the filter cake with ice n-hexane, and dry to obtain 2.65kg of high-purity phenoxyethanol, with a yield of 88.3%, a GC purity of 99.98%, and a maximum of 0.01% of impurities, such as figure 2 shown.

technical field

[0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a preparation method of high-purity phenoxyethanol. Background technique

[0002] Phenoxyethanol is a colorless slightly viscous liquid at room temperature, is relatively low in toxicity, and is chemically inactive towards copper and lead. It can be used as a preservative and is widely used in cosmetics, skin care products, vaccines and medicines. Phenoxyethanol has a strong killing effect on Pseudomonas aeruginosa, so it can also be used as a disinfectant for surgical medicine. In addition, it is also widely used in aquaculture, dyes, inks, resins and other fields.

[0003] In the field of medicine, in order to reduce the toxic and side effects of drugs on the human body, not only high requirements are placed on the quality of raw materials, but also high requirements on pharmaceutical excipients. Phenoxyethanol also needs to be of high quality as a su...

Examples

Embodiment 1

[0020] The preparation of embodiment one high-purity phenoxyethanol:

[0021] In a 250ml reaction bottle with a magnet, add 10.0g of industrial phenoxyethanol, 90ml of n-hexane, and 10ml of ethyl acetate, stir to dissolve, add 30ml of 5% aqueous sodium hydroxide solution, stir at room temperature for 0.5-1h, pour the solution Put into a separatory funnel and let stand to separate the liquid. Stir and lower the temperature of the organic layer to -20~-15°C, keep stirring and crystallize for more than 4 hours. Filter, rinse the filter cake with ice n-hexane, and dry to obtain 8.8 g of high-purity phenoxyethanol, with a yield of 88.0%, a GC purity of 99.91%, and a maximum of 0.09% of impurities, such as figure 1 shown.

[0022] With reference to the method of Example 1, the effects of different dissolving solvents or proportions on the product yield and purity were compared and investigated at the same time. Table 1 shows the data comparison results of Comparative Examples 1-4 ...

Embodiment 2

[0038] The preparation of embodiment two high-purity phenoxyethanol:

[0039] In a 50L reaction kettle, add 3.0kg of industrial phenoxyethanol, 17.6kg of n-hexane, and 2.7kg of ethyl acetate, stir to dissolve, add 9.0kg of 5% sodium hydroxide aqueous solution, stir at room temperature for 0.5-1h, and let stand to separate the liquid . The organic layer was cooled down to -15~-20°C under stirring, and kept stirring for more than 4 hours for crystallization. Filter, rinse the filter cake with ice n-hexane, and dry to obtain 2.65kg of high-purity phenoxyethanol, with a yield of 88.3%, a GC purity of 99.98%, and a maximum of 0.01% of impurities, such as figure 2 shown.

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