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Preparation method of tributyl citrate

A technology of tributyl citric acid and citric acid, which is applied in the field of preparation of tributyl citrate, can solve problems such as unfavorable environmental protection, restricting economic benefits, equipment corrosion, etc. Effect

Active Publication Date: 2019-03-08
安徽新鸿药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process not only corrodes the equipment, but also produces a large amount of waste acid, which will produce a large amount of high-salt waste liquid after neutralization, which is not only not conducive to environmental protection, but also restricts the further improvement of economic benefits

Method used

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  • Preparation method of tributyl citrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A preparation method of catalyzed tributyl citrate, comprising the following steps:

[0027] Catalyst preparation: Take 1.5g of attapulgite clay, add 20mL (7.5g) of prepared 6.25M acetic acid, stir at room temperature for 52 hours, let it stand for aging for 12 hours, centrifuge to separate the lower layer of sediment, and then wash with water until the pH becomes neutral. Dry at 60°C, grind, then dry in a vacuum oven at 110°C for 2 hours, then slowly heat up to 300°C in a muffle furnace to activate for 3 hours to obtain the desired catalyst, which is attapulgite clay catalyst treated with phosphoric acid.

[0028] Esterification: Take 0.500g of the above catalyst, put it into a 500ml three-necked flask with a water separator, add 115.2g of citric acid, 284ml of n-butanol, and react for 5.5h after the system temperature is stabilized at 138°C, stop heating, and the esterification is completed .

[0029] Alcohol distillation: dealcoholize the above system at -0.10Mpa, 8...

Embodiment 2

[0035] Change the catalyst calcination temperature, prepare the catalyst with reference to the method in Example 1, then prepare the tributyl citrate product according to the esterification method of Example 1, and the resulting tributyl citrate product yield results are shown in Table 1.

[0036] Catalyst catalyzed preparation tributyl citrate result prepared with the calcination temperature of table 1

[0037]

Embodiment 4

[0039] A preparation method of catalyzed tributyl citrate, comprising the following steps:

[0040] Catalyst preparation: take 1.5g of attapulgite clay, add 20ml of prepared 4M phosphoric acid, stir at room temperature for 52 hours, let stand for 12 hours of aging, centrifuge to separate the lower sediment, then wash with water until the pH becomes neutral, dry at 60°C, and grind , and then dried in a vacuum oven at 110°C for 2h, and then slowly heated to 300°C in a muffle furnace for activation for 3h to obtain the desired catalyst, which is an attapulgite clay catalyst treated with acetic acid.

[0041] Esterification: Take 0.500g of the above catalyst, put it into a 500ml three-necked flask with a water separator, add 115.2g of citric acid, 284ml of n-butanol, and react for 6h after the temperature is stabilized at 138°C, stop heating, and the esterification is completed.

[0042] Alcohol distillation: dealcoholize the above system at 0.10Mpa, 75°C for 10min.

[0043] Filt...

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Abstract

The invention discloses a preparation method of tributyl citrate and belongs to the technical field of chemical catalysts. The method is characterized by directly preparing a tributyl citrate productfrom citric acid and alcohol under the action of a catalyst, wherein the catalyst is attapulgite clay acidized, loaded and modified by protonic acid; the weight ratio of attapulgite clay to protonic acid is (1 to 5)-(1 to 50). The solid acid catalyst used in the method is high in activity; a trace amount of the catalyst is capable of enabling the esterification effect of polybasic acid to basically reach esterification rate of 100%; the catalyst has high selectivity on product; the yield of triesterification product can reach 95% or more; the catalyst can be repeatedly used, is free of obviousreduction of catalysis efficiency, mild in catalysis condition of esterification reaction and low in cost, is environmentally friendly, and has extremely good application prospects.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysts, and in particular relates to a preparation method of tributyl citrate. Background technique [0002] Tributyl citrate is an environmentally friendly catalyst, widely used as a plasticizer in the fields of food packaging, daily necessities and children's toys. Tributyl citrate has the advantages of good compatibility, high plasticizing efficiency, easy degradation, non-toxicity, low volatility, etc., and has good water resistance, light resistance and cold resistance. It is a plasticizer such as phthalic acid ideal substitute. [0003] At present, citric acid esters mainly use highly corrosive liquid sulfuric acid as a catalyst. Under the catalysis of sulfuric acid, citric acid and butanol undergo dehydration reaction to generate n-butyl citrate crude product, which is produced after a series of washing, neutralization and desolventization processes. Get pure. This process not only c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/704B01J27/02B01J27/138B01J27/182B01J31/04
CPCC07C67/08B01J27/02B01J27/138B01J27/182B01J31/04C07C69/704
Inventor 杨可武林伟杨凤丽宋烨航梁国斌庄苍伟
Owner 安徽新鸿药业有限公司
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