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、季戊四醇和异硬脂酰氯按照摩尔比为1:3.8~4.8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80~150 <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。该方法无需用催化剂；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 the pentaerythritol and the isostearyl chloride according to the molar ratio of 1: 3.8-4.8, and putting into a reaction kettle; s2, under the condition that the vacuum pressure is-0.1 to-0.05 MPa, the reaction temperature is 80 to 150 o And C, reacting for 0.5-12 hours to obtain a pentaerythritol tetraisostearate product. The method does not need a catalyst; the reaction condition is mild, the reaction temperature is greatly reduced, and the reaction 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, taking the pentaerythritol and the isostearyl chloride according to the molar ratio of 1: 3.8-4.8, and putting into a reaction kettle;

s2, reacting for 0.5-12 hours at the reaction temperature of 80-150 ℃ under the vacuum pressure of-0.1-0.05 MPa to obtain pentaerythritol tetraisostearate product;

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 for preparing pentaerythritol tetraisostearate according to claim 1, wherein the molar ratio of pentaerythritol to isostearyl chloride is 1: 4.0-4.4.

4. The method according to claim 1, wherein the reaction temperature is 100 to 130 ℃.

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

6. 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 colorless, odorless, transparent oil, and is a hindered ester. Pentaerythritol tetraisostearate has high thermal stability, has the functions of film forming, water resistance, skin moistening and the like, and is a non-viscous humectant. Meanwhile, the pentaerythritol tetraisostearate has good powder dispersibility and suspensibility, prevents sedimentation and has good skin-sticking property, thereby being an excellent cosmetic additive and an excellent substitute of castor oil.

The traditional preparation method is that pentaerythritol and isostearic acid are dehydrated and esterified 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. The method mainly has the following disadvantages:

1. the reaction usually requires a higher reaction temperature (at least equal to or more than 140 ℃ and most of the reaction time is 160-240 ℃), and has large energy consumption and needs special equipment;

2. when the acid catalyst is used, the service life of the reaction kettle can be greatly shortened due to the long-time high temperature;

3. the esterification efficiency is often not high, or excessive acid needs to be added to ensure complete esterification, so that the residual acid is difficult to remove; or a large amount of intermediate states such as pentaerythritol triisostearate and the like remain;

4. the reaction liquid has darker color and difficult decolorization, which affects the product quality.

Therefore, it is highly desirable to provide a synthetic route for preparing pentaerythritol tetraisostearate, which is simple and convenient to operate, light in color, high in purity and suitable 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 the pentaerythritol and the isostearyl chloride according to the molar ratio of 1: 3.8-4.8, and putting into a reaction kettle;

s2, reacting for 0.5-12 hours at the reaction temperature of 80-150 ℃ under the vacuum pressure of-0.1-0.05 MPa, and performing post-treatment to obtain a pentaerythritol tetraisostearate product;

the reaction has the following reaction route:

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 reaction temperature is 100-130 ℃.

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 reaction of the invention does not need a catalyst; the reaction condition is mild, the reaction temperature is greatly reduced, and the reaction 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.

The raw material isostearyl chloride used in the invention can be conveniently prepared by reference to RSC adv.2015,5,80702-80708, US2006062749 and other documents, and can also be prepared by reference to the methods in examples 1-3.