阅读说明：本技术 一种季戊四醇四异硬脂酸酯的制备方法 (Preparation method of pentaerythritol tetraisostearate ) 是由 张健 廖琪林 于 2019-04-26 设计创作，主要内容包括：本发明提供了一种季戊四醇四异硬脂酸酯的制备方法,具体为：S1、季戊四醇和异硬脂酸按照摩尔比为1:3.8~4.8取料,催化剂和季戊四醇按照质量比为0.01~0.3:1取料,投入反应釜中；S2、在真空压力为-0.1~-0.05 MPa条件下,在反应温度为100~160 <Sup>o</Sup>C下反应0.5~12小时,即得季戊四醇四异硬脂酸酯产品。该方法反应条件温和,大大降低了反应温度,常规搪瓷反应釜即可实现；反应时间短、耗能低；产品颜色浅、质量高；反应后处理简便、适合工业化。(The invention provides a preparation method of pentaerythritol tetraisostearate, which comprises the following steps: s1, taking materials of pentaerythritol and isostearic acid according to a molar ratio of 1: 3.8-4.8, taking materials of a catalyst and pentaerythritol according to a mass ratio of 0.01-0.3: 1, and putting the materials into a reaction kettle; s2, under the condition that the vacuum pressure is-0.1 to-0.05 MPa, the reaction temperature is 100 to 160 DEG o And C, reacting for 0.5-12 hours to obtain a pentaerythritol tetraisostearate product. The method has mild reaction conditions, greatly reduces the reaction temperature, and can be realized by a conventional enamel reaction kettle; the reaction time is short, and the energy consumption is low; the product has light color and high quality; the post-reaction treatment is simple and convenient, and is suitable for industrialization.)

1. A preparation method of pentaerythritol tetraisostearate is characterized by comprising the following steps:

s1, feeding pentaerythritol and isostearic acid according to a molar ratio of 1: 3.8-4.8, feeding a catalyst and pentaerythritol according to a mass ratio of 0.01-0.3: 1, and putting into a reaction kettle;

s2, reacting for 0.5-12 hours under the vacuum pressure of-0.1-0.05 MPa and the reaction temperature of 100-160 ℃ to obtain pentaerythritol tetraisostearate;

the reaction route is as follows:

wherein R ═ isostearoyl.

2. The method of claim 1, wherein the reaction is carried out in the absence of a solvent.

3. The method of claim 1, wherein the molar ratio of pentaerythritol to isostearic acid added is preferably 1: 4.0-4.4.

4. The method of claim 1, wherein the catalyst is one or more of stannous oxide, zinc oxide, stannous dichloride, or zinc chloride.

5. The method of claim 1, wherein the catalyst is one or more of stannous oxide or stannous dichloride.

6. The method of claim 1, wherein the mass ratio of the catalyst to pentaerythritol is preferably 0.05 to 0.2: 1.

7. The method according to claim 1, wherein the reaction temperature is 120 to 150 ℃.

8. The method of claim 1, wherein the reaction time is 2 to 6 hours.

9. The method of producing pentaerythritol tetraisostearate according to claim 1, wherein the vacuum pressure is from-0.098 to-0.06 MPa.

Technical Field

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of pentaerythritol tetraisostearate.

Background

Pentaerythritol tetraisostearate is a large molecular weight liquid oil. Pentaerythritol tetraisostearate is basically odorless, has high thermal stability, has the functions of forming a film, resisting water, moistening skin and the like, and is a non-viscous humectant. Meanwhile, pentaerythritol tetraisostearate does not block pores, has good powder dispersibility and suspensibility, prevents sedimentation and has good skin adhesion, thus being an excellent cosmetic additive.

In the literature, pentaerythritol tetraisostearate is mainly prepared by dehydrating and esterifying pentaerythritol and isostearic acid at high temperature and normal pressure under the catalysis of protonic acid such as p-toluenesulfonic acid and the like or Lewis acid such as ferric trichloride and the like. Patent CN101293828 reports a method for preparing pentaerythritol tetraisostearate by performing dehydration esterification at 160-240 ℃ for 5-9 hours under the condition of stannous oxide or zinc chloride or ferric chloride accounting for 0.03-0.1% of total weight of pentaerythritol and isostearic acid, and the preparation examples are described briefly, no post-treatment/purification process is described, and no basic quality indexes such as color, purity and the like of the product are described. Patent CN105801407 reports that zinc-iron composite metal oxide reacts for 4-5 hours at 140-150 ℃ for dehydration and esterification, and the patent describes that the obtained product has excellent chroma and acid value. However, the preparation process of the composite metal oxide is complex, and the composite metal oxide needs to be subjected to rapid nucleation, microwave treatment, crystallization and drying and then is transferred to 600 ℃ for roasting. However, the esterification reaction was found to be very slow after repeated patent operations in the laboratory, and the technical effect described in the patent was far from being achieved. Patent CN101298417 reports that 0.1-1% of p-toluenesulfonic acid based on the weight of isostearic acid is used for catalyzing dehydration esterification for 10-24 hours at 160-240 ℃, nonpolar and polar solvents are added after the reaction is finished, alkaline water is added for neutralization, the solvent is removed by evaporation under reduced pressure after the reaction is washed to be neutral, and the product has excellent chroma and acid value. However, when the conditions were reproduced in the laboratory, the product was found to be darker in color and a large amount of isostearic acid remained in the reaction.

Therefore, it is urgently needed to provide a preparation method for preparing pentaerythritol tetraisostearate, which has the advantages of light color, high purity, stable process, simple and convenient operation and suitability for industrial production.

Disclosure of Invention

Aiming at the defects of the prior art, the invention aims to provide a preparation method of pentaerythritol tetraisostearate, which is simple and feasible, stable in process, easy to control, convenient in post-reaction treatment, good in product yield, high in purity, light in color, and capable of being economically and conveniently used for industrial production.

In order to achieve the technical purpose, the invention adopts the following technical scheme:

a preparation method of pentaerythritol tetraisostearate comprises the following steps:

s1, taking materials of pentaerythritol and isostearic acid according to a molar ratio of 1: 3.8-4.8, taking materials of a catalyst and pentaerythritol according to a mass ratio of 0.01-0.3: 1, and putting the materials into a reaction kettle;

s2, reacting for 0.5-12 hours under the vacuum pressure of-0.1-0.05 MPa and the reaction temperature of 100-160 ℃ to obtain pentaerythritol tetraisostearate product;

the reaction scheme is as follows:

wherein R ═ isostearoyl.

Preferably, the reaction takes place in the absence of a solvent.

Preferably, the feeding molar ratio of the pentaerythritol to the isostearyl chloride is 1: 4.0-4.4.

Preferably, the catalyst is one or more of stannous oxide, zinc oxide, stannous dichloride or zinc chloride.

Preferably, the catalyst is one or more of stannous oxide or stannous dichloride.

Preferably, the mass ratio of the catalyst to the pentaerythritol is 0.05-0.2: 1.

Preferably, the reaction temperature is 120-150 ℃.

Preferably, the reaction time is 2 to 6 hours.

Preferably, the vacuum pressure is-0.098 to-0.06 MPa.

Compared with the prior art, the invention has the following beneficial effects: the invention has mild reaction conditions, greatly reduces the reaction temperature, and can be realized by a conventional enamel reaction kettle; the reaction time is short, and the energy consumption is low; the product has light color and high quality; the post-reaction treatment is simple and convenient, and is suitable for industrialization.

Detailed Description

The invention is further illustrated by the following examples, which are intended to be purely exemplary of the invention. These examples are not meant to impose any limitation on the invention. It will be apparent that those skilled in the art can make various changes and modifications to the present invention within the scope and spirit of the present invention. It is to be understood that the invention is intended to cover such alternatives and modifications as may be included within the scope of the appended claims.