阅读说明：本技术 化妆品用原料苯氧乙醇的制备工艺 (Preparation process of phenoxyethanol used as raw material for cosmetics ) 是由 寇然 王伟松 金一丰 万庆梅 高洪军 于 2020-07-28 设计创作，主要内容包括：本发明公开了化妆品用原料苯氧乙醇的制备工艺,该制备方法包括以下步骤：以苯酚为起始剂,在碱催化剂的存在下与环氧乙烷进行反应,得到苯氧乙醇粗品；将苯氧乙醇粗品减压精馏,得到高纯度苯氧乙醇；采用活化处理的大孔吸附剂吸附高纯度苯氧乙醇中的苯酚,得到饱和大孔吸附剂和化妆品用原料苯氧乙醇；饱和大孔吸附剂通过碱水活化和干燥后,可再次用于吸附高纯度苯氧乙醇中的苯酚。本发明得到的苯氧乙醇纯度高(≥99.9％,GC),苯酚含量低(≤10ppm,LC)。本发明工艺简洁,大孔吸附剂经碱液活化后可循环使用,生产成本低,易于工业化生产。(The invention discloses a preparation process of phenoxyethanol used as a raw material for cosmetics, which comprises the following steps: taking phenol as an initiator, and reacting with ethylene oxide in the presence of an alkali catalyst to obtain a phenoxyethanol crude product; rectifying the phenoxyethanol crude product under reduced pressure to obtain high-purity phenoxyethanol; adsorbing phenol in the high-purity phenoxyethanol by using an activated macroporous adsorbent to obtain a saturated macroporous adsorbent and phenoxyethanol used as a raw material for cosmetics; the saturated macroporous adsorbent can be used for adsorbing phenol in the high-purity phenoxyethanol again after being activated and dried by alkaline water. The phenoxyethanol obtained by the invention has high purity (not less than 99.9 percent, GC) and low phenol content (not more than 10ppm, LC). The invention has simple process, the macroporous adsorbent can be recycled after being activated by alkali liquor, the production cost is low, and the method is easy for industrial production.)

1. A preparation process of phenoxyethanol used as a raw material for cosmetics is characterized by comprising the following steps:

s1, reacting phenol serving as an initiator with ethylene oxide in the presence of an alkali catalyst to obtain a phenoxyethanol crude product;

s2, carrying out vacuum rectification on the phenoxyethanol crude product to obtain high-purity phenoxyethanol with the content of more than or equal to 99.9%;

s3, adsorbing phenol in the high-purity phenoxyethanol by using the activated macroporous adsorbent to obtain the saturated macroporous adsorbent and the phenoxyethanol used as the raw material for cosmetics, wherein the content of the phenoxyethanol is more than or equal to 99.9 percent, and the content of the phenol is less than or equal to 10 ppm.

2. The production process according to claim 1,

after the S3, further comprising S4: and the saturated macroporous adsorbent is activated by alkaline water and dried, and then is used for adsorbing phenol in the high-purity phenoxyethanol again.

3. The process of claim 1, wherein the molar ratio of phenol to ethylene oxide in S1 is 1: 1.1; the reaction temperature is 100-130 ℃, and the reaction time is 5-6 hours.

4. The process of claim 1, wherein the base catalyst in S1 is one or a mixture of two of KOH and NaOH; the adding mass of the catalyst is 1-3 per mill of the sum of the mass of the phenol and the mass of the ethylene oxide.

5. The process as claimed in claim 1, wherein the temperature of the vacuum distillation still liquid in S2 is less than or equal to 120 ℃.

6. The process as claimed in claim 1, wherein the macroporous adsorbent in S3 is one or both of a non-polar macroporous adsorbent and a weakly polar macroporous adsorbent; the adsorption temperature is 20-60 ℃.

7. The process of claim 2, wherein the alkaline water in S4 is one or two of KOH and NaOH aqueous solution; the volume of alkaline water used for activation is 2-5 times of the volume of the macroporous adsorbent.

8. The process of claim 7, wherein the alkaline water in S4 is 5% NaOH aqueous solution.

Technical Field

The invention relates to the technical field of fine chemical engineering, and in particular relates to a preparation process of a raw material phenoxyethanol for cosmetics.

Background

The phenoxyethanol is a high-boiling point and low-volatile solvent, and is an efficient broad-spectrum antiseptic bactericide with low sensitization, low toxicity and stable chemical properties. In recent years, it has been used more and more frequently in the light industry and the daily chemical industry because it is soluble in both oil and water. The phenoxyethanol for cosmetics has high added value of products, and the quality index of the phenoxyethanol is the strictest, and the light industry standard of the people's republic of China requires that the content of phenoxyethanol for cosmetics is more than or equal to 99.0 percent, the content of phenol is less than or equal to 10ppm and the like.

At present, the industrial production method of phenoxyethanol takes phenol and ethylene oxide as raw materials and prepares the phenoxyethanol by catalytic ring-opening addition. The obtained industrial grade phenoxyethanol crude product has low phenoxyethanol content (about 90 percent) and high phenol residue (about 5000 ppm). As the phenoxyethanol for cosmetics is required to have high purity and less phenol residue, the industrial phenoxyethanol crude product can meet the use requirement of cosmetics only by purification.

The existing purification process of the industrial-grade phenoxyethanol crude product mainly comprises reduced pressure distillation, reduced pressure rectification or temperature reduction crystallization. Chinese patent CN104926618A discloses a process for preparing phenoxyethanol with a purity of about 95% by vacuum distillation. Chinese patent CN110642706A discloses a process for preparing high-purity phenoxyethanol with the content more than or equal to 99.5 percent by cooling crystallization. However, there is no reported process for reducing phenol residues in phenoxyethanol.

Disclosure of Invention

In order to solve the defects in the prior art, the invention aims to provide a preparation process of a cosmetic raw material phenoxyethanol, which can be implemented by the following technical scheme:

a preparation process of phenoxyethanol used as a raw material for cosmetics comprises the following steps:

s1, reacting phenol serving as an initiator with ethylene oxide in the presence of an alkali catalyst to obtain a crude product of industrial phenoxyethanol;

s2, carrying out vacuum rectification on the industrial-grade phenoxyethanol crude product to obtain high-purity phenoxyethanol with the content of more than or equal to 99.9%;

s3, adsorbing phenol in the high-purity phenoxyethanol by using the activated macroporous adsorbent to obtain the saturated macroporous adsorbent and a cosmetic raw material phenoxyethanol, wherein the phenoxyethanol content is more than or equal to 99.9 percent, and the phenol content is less than or equal to 10 ppm.

After the above process, the method further comprises the step of S4: the saturated macroporous adsorbent is activated and dried by alkaline water and then is used for adsorbing phenol in the high-purity phenoxyethanol again.

The molar ratio of said phenol to ethylene oxide of S1 is 1: 1.1; the reaction temperature is 100-130 ℃, and the reaction time is 5-6 hours; the alkali catalyst is one or a mixture of KOH and NaOH; the adding mass of the catalyst is 1-3 per mill of the sum of the mass of phenol and ethylene oxide. .

The temperature of the residue of the vacuum rectification of S2 is less than or equal to 120 ℃.

The macroporous adsorbent used in S3 is one or two of nonpolar macroporous adsorbent and weak polar macroporous adsorbent; the temperature of the adsorption experiment is controlled to be 20-60 ℃.

The alkaline water in S4 is one or two of KOH and NaOH aqueous solution, preferably 5% NaOH aqueous solution; the volume of alkaline water used for activation is 2-5 times of the volume of the macroporous adsorbent.

Compared with the prior art, the invention has the following advantages:

1. the activated macroporous adsorbent is adopted to adsorb phenol in high-purity phenoxyethanol, so that the content of phenol in phenoxyethanol is reduced, and the method is simple and easy to implement and low in cost;

2. the macroporous adsorbent can be activated and recycled by alkali liquor, so that the process production cost is low, and the method is suitable for industrial production;

3. the phenoxyethanol prepared by the process has high purity (more than or equal to 99.9 percent, GC) and low phenol content (less than or equal to 10ppm, LC), and reaches the standards of the cosmetic raw material phenoxyethanol in the national light industry.

Detailed Description

The embodiment provides a preparation process of phenoxyethanol used as a raw material for cosmetics, which comprises the following steps:

step 1, taking phenol as an initiator, and reacting with ethylene oxide in the presence of an alkali catalyst to obtain a phenoxyethanol crude product;

step 2, carrying out vacuum rectification on the industrial-grade phenoxyethanol crude product to obtain high-purity phenoxyethanol with the content of more than or equal to 99.9 percent;

step 3, adsorbing phenol in the high-purity phenoxyethanol by using the activated macroporous adsorbent to obtain a saturated macroporous adsorbent and phenoxyethanol used as a raw material for cosmetics, wherein the content of the phenoxyethanol is more than or equal to 99.9 percent, and the content of the phenol is less than or equal to 10 ppm;

and 4, activating and drying the saturated macroporous adsorbent by using alkaline water, and then, adsorbing phenol in the high-purity phenoxyethanol again.

The molar ratio of phenol to ethylene oxide in step 1 is about 1: 1.1; the reaction temperature is 100-130 ℃, and the reaction time is 5-6 hours; the alkali catalyst is one or a mixture of KOH and NaOH; the adding mass of the catalyst is 1-3 per mill of the sum of the mass of phenol and ethylene oxide.

The temperature of the residue of the vacuum rectification in the step 2 is less than or equal to 120 ℃.

The macroporous adsorbent used in the step 3 is one or two of a non-polar macroporous adsorbent and a weak-polar macroporous adsorbent; the temperature of the adsorption experiment is controlled to be 20-60 ℃.

The alkaline water in the step 4 is one or two of KOH and NaOH aqueous solutions, and the NaOH aqueous solution with the mass fraction of 5% is preferably selected; the volume of alkaline water used for activation is 2-5 times of the volume of the macroporous adsorbent.

The present invention will be described in detail with reference to examples.