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Method for preparing tributyl citrate by using modified cation exchange resin as catalyst

A technology of tributyl citrate and cation exchange, used in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate and other directions, can solve the problems of equipment corrosion, many side reactions, and many by-products, etc., and achieves reaction conditions The effect of mildness, good catalytic effect and short reaction time

Inactive Publication Date: 2012-01-18
SICHUAN 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]. Although concentrated sulfuric acid is cheap and has high catalytic activity, it exists in many Disadvantages: (1) Many side reactions, difficult to refine
There are carbonization and oxidation side reactions in the catalysis of concentrated sulfuric acid, and there are many by-products. At the same time, concentrated sulfuric acid is not easy to remove, which brings difficulties to the purification and recovery of reaction products.
(2) The concentrated sulfuric acid corrodes the equipment seriously, which increases the production cost
(3) A large amount of acid waste water and waste gas will be produced during the production process, which will seriously pollute the environment
Therefore, its application is very limited
Some catalysts developed later, such as p-toluenesulfonic acid catalyst [Xie Wenlei et al., Fine Petrochemical Industry, 1988, (4): 7-9], have better catalytic activity, but the catalyst is expensive and cannot be reused

Method used

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  • Method for preparing tributyl citrate by using modified cation exchange resin as catalyst
  • Method for preparing tributyl citrate by using modified cation exchange resin as catalyst
  • Method for preparing tributyl citrate by using modified cation exchange resin as catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1 Preparation of modified macroporous strongly acidic cation exchange resin

[0025] Convert the sodium-type macroporous (the pore size generally considered in the industry) strongly acidic cation exchange resin to the hydrogen-type by conventional methods, and then dry it at about 80° C. for about 24 hours under vacuum conditions. The dried 3.5g hydrogen-type macroporous strongly acidic cation exchange resin was reacted with 25.2g carbon disulfide and 11.2g anhydrous tin tetrachloride under reflux for about 5 hours. After the reaction was completed, it was poured into water and washed with water until dry Cl - , then washed 3 times with absolute ethanol, and then washed 3 times with acetone, and finally dried the resin at about 70°C for about 24 hours under vacuum conditions to obtain a macroporous strongly acidic cation exchange resin modified with anhydrous tin tetrachloride resin.

[0026] 2 Esterification reaction

[0027] Add 0.2mol monohydrate citric acid, 0.8...

Embodiment 2-4

[0031] Except for the following differences, the others are the same as in Example 1, and the dosage of the modified macroporous strongly acidic cation exchange resin in each example is shown in Table 1 respectively.

[0032] Table 1

[0033]

Embodiment 5-7

[0035] Except for the following differences, all the other are the same as Example 1, and the n-butanol consumption of each example is shown in Table 2 respectively.

[0036] Table 2

[0037]

[0038]

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Abstract

The invention discloses a method for preparing tributyl citrate by using modified cation exchange resin as a catalyst, which comprises the following main steps of: carrying out esterification reaction on citric acid monohydrate, n-butyl alcohol and the catalyst at 140-160 DEG C, wherein the catalyst is macroporous strong acid cation exchange resin modified by anhydrous stannic chloride; after reaction is finished, separating to remove the catalyst in an esterification reaction product; and carrying out alkali washing, water washing and distillation purification on separated liquid to obtain tributyl citrate. The separated catalyst can be recycled and basically keeps the activity unchanged. According to the method for preparing the tributyl citrate,, disclosed by the invention, the modified macroporous strong acid cation exchange resin is used as the catalyst, and the reactant n-butyl alcohol is used as a water entrainer, therefore the use of toxic benzene, toluene, and the like is avoided, and no pollution is brought in the preparation process; and the method disclosed by the invention has the advantages of mild reaction conditions, short reaction time, low production cost and citric acid reaction conversion rate capable of reaching more than 98 percent.

Description

technical field [0001] The invention relates to the technical field of tributyl citrate preparation, in particular to a method for preparing tributyl citrate with a modified cation exchange resin as a catalyst. Background technique [0002] Tributyl citrate is a non-toxic and tasteless "green" environmental plastic plasticizer. It is widely used in food and medical instrument packaging, cosmetics, daily necessities, toys, military supplies, etc. It has good compatibility, high plasticizing efficiency, and no It has the advantages of toxicity, easy biodegradation and low volatility, 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/704C07C67/08
CPCY02P20/584
Inventor 李瑞海张萌萌谢利平周鹏肖慧李涛胡祥
Owner SICHUAN UNIV
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