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Method for preparing tributyl citrate through diatomite immobilized titanium sulfate used as catalyst

A technology for the catalytic preparation of tributyl citrate, applied in the chemical industry, can solve the problems of complex post-treatment process, many side reactions, complex preparation process, etc., achieve easy recovery and reuse, improve the efficiency of esterification reaction, simplify the The effect of the treatment process

Inactive Publication Date: 2012-07-18
BENGBU BBCA MEDICINE SCI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the traditional process, concentrated sulfuric acid is usually used as a catalyst for the synthesis of tributyl citrate. However, this catalyst has many side reactions, difficult refining, serious equipment corrosion, complicated post-treatment process, and environmental pollution from waste acid. Its application has been widely accepted. big limit
Some catalysts that have been studied more later, such as solid superacids, have good catalytic activity for this reaction, but their preparation process is complicated and costly, which is not conducive to industrial production.

Method used

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  • Method for preparing tributyl citrate through diatomite immobilized titanium sulfate used as catalyst
  • Method for preparing tributyl citrate through diatomite immobilized titanium sulfate used as catalyst
  • Method for preparing tributyl citrate through diatomite immobilized titanium sulfate used as catalyst

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Experimental program
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Effect test

Embodiment 1

[0022] 1) Preparation of catalyst

[0023] Take 6g of diatomaceous earth and add it to 100mL of titanium sulfate solution with a mass fraction of 4%, and place it at 60°C and stir for 2h, evaporate the water in a vacuum, and dry the remaining solid at 100°C for 24h. Baking under the condition of ℃ for 6h.

[0024] 2) Esterification reaction

[0025] Add 270g of n-butanol, 200g of citric acid and 2g of catalyst in the reactor equipped with electromagnetic stirring, thermometer, reflux condenser, and water separator, heat and reflux at 120°C and stir, and the water produced by the reaction is separated from the water separator. The reaction stops when it enters the water separator until there is no water, and the crude product of tributyl citrate is obtained.

[0026] 3) Catalyst recovery and product purification

[0027] The crude product of tributyl citrate is filtered, and the catalyst filtered out is directly used in the next reaction; the filtrate is distilled under norm...

Embodiment 2-4

[0029] Only change n-butanol consumption, all the other are with embodiment 1. The results are shown in Table 1.

[0030] Table 1

[0031]

[0032]

Embodiment 5-7

[0034] Only change the esterification reaction temperature, all the other are with embodiment 1. The results are shown in Table 2.

[0035] Table 2

[0036]

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Abstract

The invention provides a method for preparing tributyl citrate through diatomite immobilized titanium sulfate used as a catalyst. According to the method, diatomite immobilized titanium sulfate is used as the catalyst, and citric acid and n-butyl alcohol take esterification reaction for synthesizing the tributyl citrate. The method has the advantages that the diatomite immobilized titanium sulfate is used as the catalyst, obvious corrosivity does not exist, in addition, the recovery and the repeated utilization are easy, and the activity is basically maintained unchanged; the esterification reaction efficiency is improved, and the product yield can reach 99.5 percent to the highest degree; reactants of the n-butyl alcohol are used as water-carrying agents, the use of noxious solvents such as methylbenzene and the like is avoided, and in addition, the aftertreatment process is simplified; and the esterification reaction condition is mild, the process is simple, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for preparing tributyl citrate by catalyzing diatomite-supported titanium sulfate. Background technique [0002] At present, the plasticizers commonly used in industry are phthalates. Because they can induce cancer, their use has been strictly controlled abroad, and non-toxic plasticizers that can replace phthalates are actively sought. my country has also formulated relevant laws and regulations, which will phase out its use in food packaging materials, medical appliances, and toys, and recommend the use of tributyl citrate. Tributyl citrate has the characteristics of good compatibility, high plasticizing efficiency, non-toxic, low volatility, cold resistance, mildew resistance, light resistance, water resistance, etc., especially in food packaging, children's toys, medical products, etc. Field applications have significant advantages. Therefore, tributyl ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/704C07C67/08B01J27/053
Inventor 汪洪湖陶涛张亚孙建华韦亚锋王栋
Owner BENGBU BBCA MEDICINE SCI DEV
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