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A kind of oligoglycerol ester/ether derivative and its synthesis method

A technology of oligoglycerol ester and synthesis method, which is applied in the field of oligoglycerol ester/ether and its synthesis, oligomer type nonionic surfactant, can solve problems such as application field limitations, and achieve wide application and low CMC concentration , the effect of improving the reaction efficiency

Active Publication Date: 2017-10-20
重庆市化工研究院有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The polyglycerol ester prepared by the aforementioned method mainly plays the role of emulsification, dispersion, etc., and its application field is also limited, so it is difficult to play an important role in industrial fields other than food, medicine, and cosmetics.

Method used

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  • A kind of oligoglycerol ester/ether derivative and its synthesis method
  • A kind of oligoglycerol ester/ether derivative and its synthesis method
  • A kind of oligoglycerol ester/ether derivative and its synthesis method

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preparation example Construction

[0062] Therefore, the preparation method of the derivative of oligoglycerol ester / ether of the present invention comprises the following steps:

[0063] 1) Put the monoglyceride / ether containing tertiary carbonyl or alkyl group into the reaction kettle as the base material, start stirring, put in the catalyst, replace the air in the reaction kettle with nitrogen, and raise the temperature to 110-180°C;

[0064] 2) Add the glycidyl ester / ether containing tertiary carbonyl or alkyl group dropwise into the reaction kettle, and the dropwise addition is completed within 4 to 12 hours;

[0065] 3) Steam the unreacted glycidyl ester / ether and refine to obtain oligoglycerol ester / ether.

[0066] In a further solution, the molar ratio of the monoglyceride / ether to glycidyl ester / ether of the present invention is 1.0:1.0-5.0.

[0067] In the present invention, the inventor has studied the selection of catalysis, and found in the research process that: when using inorganic bases such as...

Embodiment 1

[0102] The preparation of catalyst, concrete steps are as follows:

[0103] 1) Acidified modified bentonite: Weigh 600g of sodium-based bentonite (infrared spectrogram as attached figure 2 , 1434cm -1 The place is the absorption peak of carbonate), put it into a 5000mL large beaker with 4000mL deionized water in batches, stir until it is completely dispersed; put 400g of 1+1 hydrochloric acid in batches (200g hydrochloric acid dissolved in 200mL deionized water ), to no longer emit air bubbles in the system, the measured pH value is 6, stop stirring, and place overnight. Remove the salt-containing clear liquid in the upper layer, centrifuge the product in the lower layer, wash twice with deionized water, and centrifuge again to obtain a modified bentonite with a moisture content of about 50%; take part of the acidified modified bentonite and dry it at 120 ° C for 24 hours, crush it, and measure it by infrared spectrum, get figure 2 The infrared spectrum shown, 1434cm -1 ...

Embodiment 2

[0108] A kind of oligomeric neodecanoin, the synthetic method is as follows:

[0109] 1) Preparation of monoglyceride neodecanoate: Glycidyl neodecanoate was used as raw material, and hydrolyzed under the action of a hydrolysis catalyst; for the catalyst prepared in Catalyst Example 1, the addition amount of the hydrolysis catalyst in the reaction was 5%; 1250g glycidyl neodecanoate was put into a 2000mL four-neck flask, stirred, and 62.5g hydrolysis catalyst was added. Nitrogen gas was introduced to replace the air, the temperature was gradually raised to 120°C, and deionized water was added dropwise, and the temperature was maintained at 118-122°C for 12 hours. The end point of the reaction is that the epoxy value of the system is ≤0.01. The content of neodecanoin monoglyceride obtained by centrifugation and refining is ≥60%, and the rest is oligomeric neodecanoin glyceride;

[0110] 2) Synthesis of oligomeric neodecanoic acid glycerides: 750 g of neodecanoic acid monoglyc...

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Abstract

The invention discloses low-polyglycerol ester / ether derivatives and a preparation method thereof. The chemical structure formula of the low-polyglycerol ester / ether derivatives is the formula (II), wherein n, x, y, R1, Rn+1 and Rn+2 meet the following relations: n=0-8; the average polymerization degree of the low-polyglycerol ester / ether derivatives is equal to n+2; x+y is any natural number ranging from 0 to 100, x and y are greater than or equal to 0; R1 to Rn+1 and Rn+2 refer to at least two types of alkyl acyls with a carbon atom number of 4-18 or alkyl groups with a carbon atom number of 1-18. According to the preparation method, an addition reaction is performed on monoglyceride or ether and at least one glycidyl ester or ether in the presence of an acid catalyst. The low-polyglycerol ester / ether derivatives can be used in surfactants; compared with traditional polyglycerol surfactants, the low-polyglycerol ester / ether derivatives have the advantages of relatively low CMC concentration and relatively excellent surface activity.

Description

technical field [0001] The invention relates to the technical field of surfactants, in particular to a oligoglycerol ester / ether and a synthesis method thereof. The oligoglycerol ester / ether derivative is an oligomer type nonionic surface with two hydrophilic groups active agent. Background technique [0002] Under the current general trend of water-based coatings and other industrial fields, water-based additives have become a hot spot for research and development by many chemical companies at home and abroad. On the other hand, since most additives will eventually be discharged into the environment, new types of additives with better biodegradability have gradually become a trend. New water-based additives with high performance and environmental friendliness are ready Favored by the market. [0003] Glyceride derivatives are a class of environmentally friendly chemical materials, which can be prepared by modifying animal and vegetable oils that exist in nature, or other ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/03C07C43/11C07C67/29C07C69/30C08G65/28
CPCC07C41/03C07C43/11C07C67/29C07C69/30C08G65/2609
Inventor 王建华
Owner 重庆市化工研究院有限公司
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