Method for preparing tributyl citrate using mesoporous molecular sieve as catalyst

A technology of tributyl citrate and mesoporous molecular sieves, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of severe equipment corrosion, complicated post-processing, and difficult refining, and achieve mild reaction conditions. , The amount of catalyst is small, and there is no effect of environmental pollution

Inactive Publication Date: 2006-04-26
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional method of synthesizing tributyl citrate is to use concentrated sulfuric acid as a catalyst [Edited by Song Qihuang, Fine Chemical Technology, Beijing: Chemical Industry Press, 1995: 95]. This catalyst has many side reactions, difficult refining, and serious equipment corrosion , complicated post-processing, producing industrial "three wastes", polluting the environment and other shortcomings, its application has been greatly restricted
Some catalysts developed later, such as p-toluenesulfonic acid [Xie Wenlei et al., Fine Petrochemical Industry, 1998, (4): 7-9], all have good catalytic activity for this reaction, but the catalyst is expensive and cannot be repeated. recycle

Method used

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  • Method for preparing tributyl citrate using mesoporous molecular sieve as catalyst

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Experimental program
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Effect test

Embodiment 1

[0019] Preparation of the first step catalyst HAl-MCM-41 mesoporous molecular sieve

[0020] With the Al-MCM-41 mesoporous molecular sieve that prior art makes, through the NH of 4mol / L 4 NO 3 Exchange the aqueous solution and roast at 550°C (three times) to obtain HAl-MCM-41 mesoporous molecular sieve;

[0021] Step 2 Esterification Reaction

[0022] Add 0.1mol citric acid and 0.45mol n-butanol into a 100mL three-necked bottle equipped with electromagnetic stirring, thermometer, reflux condenser, and water separator for heating and stirring. After the citric acid is completely dissolved, take a sample to determine the acid value, and then add 0.3 g of HAl-MCM-41 molecular sieve, heat and reflux and stir, separate the water produced by the reaction from the water separator, react until anhydrous (about 4h), take a sample to measure the acid value, the acid value is determined according to GB / T1668-1995 Determination;

[0023] Step 3 Separation of catalyst and purification ...

Embodiment 2-4

[0026] Except for the following differences, the rest are the same as in Example 1, the amount of HAl-MCM-41 molecular sieve is 0.3g, the amount of citric acid is 0.1mol, the amount of n-butanol is according to the ratio in Table 1, and the reaction is 4h.

[0027] Example

Embodiment 5-7

[0029] Except the following difference, all the other are identical with embodiment 1, and the consumption of HAl-MCM-41 molecular sieve is according to table 2 respectively.

[0030] Example

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Abstract

The tributyl citrate preparing process features using mesoporous molecular sieve as catalyst for the synthesis of tributyl citrate, filtering out the catalyst from the reacted product after reaction for reuse, and treating the filtrate through distillation, water washing, alkali washing, and re-distillation to obtain tributyl citrate. The catalyst has relatively high catalytic activity on the esterification of citric acid and n-butanol. The present invention has the advantages of high yield, cheap catalyst, small catalyst consumptlion, mild reaction condition, short reaction period, reusability of the catalyst, no environmental pollution, direct use of non-toxic reactant n-butanol as water entrainer, etc.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for preparing tributyl citrate by using mesoporous molecular sieve as a catalyst. Background technique [0002] Tributyl citrate is a non-toxic, odorless "green" environmental plasticizer, widely used in food and medical equipment packaging, cosmetics, daily necessities, toys, military supplies, etc., with good compatibility, high plasticizing efficiency, non-toxic , Easy to be biodegraded and low volatility, etc., excellent cold resistance, light resistance and water resistance, and has mildew resistance in the resin, and does not grow mold. The combination of tributyl citrate and other non-toxic plasticizers can increase the hardness of the product, especially for soft fiber ether. At the same time, it can improve the anti-ultraviolet ability of nitrocellulose, and is a solvent for various spices, and can also be used as a d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08B01J29/06C07C69/704
Inventor 杨建国高珊梁学正刘彩华于心玉何鸣元
Owner EAST CHINA NORMAL UNIV
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