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Catalyzing synthesis of citric tributyl ester from carbon-base sulfoacid

A technology of tributyl citrate and carbon-based sulfonic acid is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc. The effect of mild conditions, small amount of catalyst, and cheap catalyst

Inactive Publication Date: 2006-08-16
EAST CHINA NORMAL UNIVERSITY
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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 catalyzers that develop later are as catalyzer [Xie Wenlei etc., fine petrochemical industry, 1998, (4): 7-9] with p-toluenesulfonic acid, all have good catalytic activity to this reaction, but catalyzer is expensive, and Cannot be reused

Method used

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  • Catalyzing synthesis of citric tributyl ester from carbon-base sulfoacid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Preparation of the first step carbonyl sulfonic acid

[0019] Add 10ml of concentrated sulfuric acid to 15g of cracked C9 fraction, heat and react at 250°C for 4h, then add boiling water to reflux and stir for 3h, filter with suction, and dry at 140°C to obtain carbonylsulfonic acid;

[0020] Step 2 Esterification Reaction

[0021] Add 0.1 mol of citric acid, 0.45 mol of n-butanol and 0.3 g of carbonyl sulfonic acid into a 100 mL three-neck flask equipped with electromagnetic stirring, thermometer, reflux condenser, and water separator, heat and reflux and stir to make the water produced by the reaction Separated from the water separator, reacted until there was no water, then entered the water separator to stop, and obtained the crude product of tributyl citrate and took a sample to measure the acidity. The acid value was determined in accordance with GB / T1668-1995;

[0022] Step 3 Separation of catalyst and purification of product

[0023] Filter the crude product, ...

Embodiment 2-4

[0025] Except following difference, all the other are identical with embodiment 1, be 0.3g in the carbon base sulfonic acid consumption, be 0.1mol in the citric acid consumption, see table 1 on the impact result of n-butanol consumption on reaction.

[0026] Example

Embodiment 5-8

[0028] Except following difference, all the other are identical with embodiment 1, and the impact result of carbon base sulfonic acid consumption is shown in Table 2

[0029] Example

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Abstract

Synthesis of tributyl citrate with carbylic sulfoacid catalyst is carried out by taking carbylic sulfoacid as catalyst while ester synthesizing, filtering, decompress distilling the filtrate to obtain tributyl citrate and circulation using the filtered carbylic sulfoacid. It is cheap, short reactive time and gentle reactive condition, has more yield and higher activity.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for catalyzing and synthesizing tributyl citrate with carbonyl sulfonic acid. Background technique [0002] Tributyl citrate is a non-toxic and tasteless "green" environmental plastic plasticizer, widely used in food and medical instrument packaging, cosmetics, daily necessities, toys, military supplies, etc., with good compatibility, high plasticizing efficiency, 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 also be used as a ...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/34B01J31/02
CPCY02P20/582
Inventor 杨建国高珊梁学正于心玉刘彩华王雯娟何鸣元
Owner EAST CHINA NORMAL UNIVERSITY
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