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Preparation process of phenoxyethanol serving as raw material for cosmetics

A phenoxyethanol and preparation technology, which is applied in the field of preparation technology of phenoxyethanol as a raw material for cosmetics, can solve the problem of not being able to reduce phenol, etc., and achieve the effect of low cost and low process production cost

Active Publication Date: 2020-09-29
ZHEJIANG HUANGMA TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, none of the reported patents are capable of reducing phenol residues in phenoxyethanol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 1888g of phenol and 8.56g of NaOH solid catalyst into a 5L pressure-resistant reactor, connect the ethylene oxide metering tank to the pressure-resistant reactor; replace the air in the reactor with nitrogen for 3 times, heat the reactor to about 100°C, and start Pass through 968g ethylene oxide, maintain reaction temperature about 100 ℃, react for 3 hours. After completion of the reaction, degas and cool to obtain about 2860g of crude phenoxyethanol. The purity of the product detected by GC is 91.3%, and the phenol content detected by HPLC is about 5000ppm.

[0031] Add 2125g of crude phenoxyethanol to a 3L three-neck flask with a 70cm rectification column, raise the temperature to 120°C, carry out rectification under reduced pressure, collect the previous fraction, and obtain 1885g of high-purity phenoxyethanol, with a GC detection content of 99.91%.

[0032] At 20°C, the activated macroporous adsorbent was used to adsorb phenol in high-purity phenoxyethanol. Whe...

Embodiment 2

[0035] Add 1888g of phenol and 5.71g of NaOH and KOH mixed solid catalyst in a 5L pressure-resistant reactor, connect the ethylene oxide metering tank to the pressure-resistant reactor; replace the air in the reactor with nitrogen for 3 times, and heat the reactor to about 115 °C, start to feed 968g of ethylene oxide, maintain the reaction temperature at about 115 °C, and react for 2 hours. After the reaction was completed, degas and cool to obtain about 2857g of crude phenoxyethanol. The purity of the product detected by GC is 91.6%, and the phenol content detected by HPLC is about 5000ppm.

[0036] Add 2125g of crude industrial phenoxyethanol to a 3L three-neck flask with a 70cm rectification column, raise the temperature to 110°C for vacuum distillation, collect the previous fraction, and obtain 1855g of high-purity phenoxyethanol, with a GC detection content of 99.92%. At 40°C, the activated macroporous adsorbent was used to adsorb phenol in high-purity phenoxyethanol. Wh...

Embodiment 3

[0039] 1888g of phenol and 2.86g of KOH solid catalyst were added in a 5L pressure-resistant glass reactor, and the ethylene oxide metering tank was connected with the pressure-resistant reactor. Replace the air in the reactor with nitrogen for 3 times, heat the reactor to about 130°C, start to feed 968g of ethylene oxide, maintain the reaction temperature at about 130°C, and react for 2 hours. After completion of the reaction, degas and cool to obtain about 2856g of crude phenoxyethanol. GC detection product purity is 91.0%, HPLC detection phenol content is about 5000ppm.

[0040]Add 2125g of crude phenoxyethanol to a 3L three-neck flask with a 70cm rectification column, raise the temperature to 100°C for vacuum distillation, collect the previous fraction, and obtain 1845g of high-purity phenoxyethanol with a GC detection content of 99.94%. At 60°C, the activated macroporous adsorbent was used to adsorb phenol in high-purity phenoxyethanol. When the phenol residue was detect...

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PUM

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Abstract

The invention discloses a preparation process of phenoxyethanol serving as a raw material for cosmetics, which comprises the following steps: reacting phenol serving as an initiator with ethylene oxide in the presence of a base catalyst to obtain a phenoxyethanol crude product; rectifying the phenoxyethanol crude product under reduced pressure to obtain high-purity phenoxyethanol; adsorbing phenolin high-purity phenoxyethanol by adopting the activated macroporous adsorbent to obtain a saturated macroporous adsorbent and a cosmetic raw material phenoxyethanol; using the saturated macroporous adsorbent for adsorbing phenol in high-purity phenoxyethanol again after being activated and dried by alkaline water. The phenoxyethanol obtained in the invention has high purity (> = 99.9%, GC) and low phenol content (< = 10ppm, LC). The process is simple, the macroporous adsorbent can be recycled after being activated by alkali liquor, the production cost is low, and industrial production is easy.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a preparation process of phenoxyethanol, a raw material for cosmetics. Background technique [0002] Phenoxyethanol is a high boiling point, low volatile solvent, and a low allergen, low toxicity, stable chemical properties, high efficiency, broad-spectrum antiseptic and fungicide. Because it can be dissolved in both oil and water, it has been used more and more frequently in light industry and daily chemical industry in recent years. Among them, the added value of phenoxyethanol for cosmetics is high, and its quality index is also the most stringent. The light industry standard of the People's Republic of China requires that the content of phenoxyethanol used in cosmetics is ≥99.0%, and the content of phenol is ≤10ppm. [0003] At present, the industrial production method of phenoxyethanol is to use phenol and ethylene oxide as raw materials through catalytic ring-openin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/03C07C43/23C07C41/34
CPCC07C41/03C07C41/34C07C43/23Y02P20/52
Inventor 寇然王伟松金一丰万庆梅高洪军
Owner ZHEJIANG HUANGMA TECH
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