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Method for preparing tributyl citrate by using rare-earth salt binary complex type solid acid as catalyst

A technology catalyzed by tributyl citrate and solid acid, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of corrosion equipment, complicated preparation process, and complicated post-treatment, and achieve The effects of no corrosion to equipment, small dosage, and cheap catalyst

Inactive Publication Date: 2009-03-25
ANHUI XIANGFENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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], there are corrosion equipment, serious pollution, many side reactions, and complicated post-treatment and other shortcomings
Some catalysts that have been studied later, such as solid superacids [Jin Ruidi et al., Applied Chemical Industry, 2005, 34 (1): 32-35], have good catalytic activity for this reaction, but the preparation process is complicated and the cost is high. Good for industrial promotion

Method used

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  • Method for preparing tributyl citrate by using rare-earth salt binary complex type solid acid as catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Step 1 Preparation of compound catalyst

[0023] Weigh 0.63 g of cerium sulfate tetrahydrate and sulfamic acid in a weight ratio of 2:1, and mix them evenly to obtain a binary compound catalyst.

[0024] Step 2 esterification reaction

[0025] Add 0.2mol (42.03g) citric acid monohydrate and 0.8mol n-butanol to a 250mL three-necked flask equipped with electromagnetic stirring, thermometer, reflux condenser, and water separator. At the same time, add 0.63g of compound catalyst and heat to reflux and stir. , The water produced by the reaction is separated from the water trap, and the acid value is measured every one hour. The acid value is determined in accordance with GB / 1668-1995. After 6 hours of reaction, the acid value is reduced to 3.75mgKOH / g, and the esterification rate is 98.7. %, the reaction is completed, and the end temperature does not exceed 150°C.

[0026] Step 3 separation of catalyst and purification of product

[0027] Filter the reaction mixture in the three...

Embodiment 2-5

[0029] Except for the following differences, the rest is the same as in Example 1. The amount of the composite catalyst is 0.63 g, the amount of citric acid is 0.2 mol, and the amount of n-butanol is according to the proportion in Table 1, and the reaction is performed for 6 hours.

[0030] Table 1

[0031] Example Acid to alcohol ratio Esterification rate / % 2 1:3.5 97.5 3 1:4.0 98.7 4 1:4.5 98.1 5 1:5.0 97.9

Embodiment 6

[0033] Step 1 Preparation of compound catalyst

[0034] Weigh 0.63 g of lanthanum chloride heptahydrate and p-toluenesulfonic acid in a ratio of 4:1, and mix them to obtain a binary compound catalyst.

[0035] Step 2 esterification reaction

[0036] Add 0.2mol of citric acid monohydrate and 0.9mol of n-butanol to a 250mL three-necked flask equipped with electromagnetic stirring, thermometer, reflux condenser, and water separator. At the same time, add 0.63g of compound catalyst, and heat to reflux and stir to make the reaction. The water is separated from the water separator, and the acid value is measured every hour. The acid value is measured according to GB / 1668-1995. After 7 hours of reaction, the acid value is reduced to 3.42mgKOH / g, the esterification rate is 99.1%, and the reaction is completed. , The terminal temperature does not exceed 150 ℃.

[0037] Step 3 separation of catalyst and purification of product

[0038] Filter the reaction mixture in the three-necked flask, ...

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Abstract

The invention discloses a method for preparing tributyl citrate by the catalysis of rare-earth salt binary-compound solid acid, which pertains to the technical field of fine chemical and industrial catalysis. The invention adopts the solid acid compounded by rare-earth salt and organic acid as the catalyst in the tributyl citrate synthesizing process, after the reaction is complete, the catalyst is filtered out from the reaction mixture for reuse; the filtrate is treated with dealcoholization, decolourization, neutralization, washing and dehydration to obtain the tributyl citrate; the product purity is more than 99.5 percent. The invention has the advantages that: the catalyst is cheap, does not erode the equipment and has small dosage, good repetitiveness and high rate of esterification; the reaction condition is mild and the reaction time is short; and the reactant, the normal butanol, is directly used as the dehydrant and the environment is not polluted and the like.

Description

Technical field [0001] The invention relates to a method for synthesizing a non-toxic plasticizer, in particular to a method for synthesizing tributyl citrate by using a solid acid compounded with a rare earth salt and an organic acid as a catalyst, and belongs to the technical field of fine chemicals and industrial catalysis. Background technique [0002] At present, as the largest amount of DOP and other phthalate plasticizers in the field of plasticizers, there are continuous reports of its possible carcinogenicity at home and abroad. The U.S. Environmental Protection Agency has restricted the use of six phthalates in applications with high sanitation requirements based on the results of the National Cancer Institute research, and has made clear regulations on the emission standards of DOP in the air and water. , And clearly limit the scope of application of DOP. The Swiss government has decided to ban the use of DOP in children's toys. The European Community (1978), the Feder...

Claims

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Application Information

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IPC IPC(8): C07C69/704C07C67/08B01J31/02B01J27/25B01J27/10
Inventor 蒋平平魏猛杜晓晗
Owner ANHUI XIANGFENG NEW MATERIALS
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