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Method for synthesizing triethyl citrate

A technique for the synthesis of triethyl citrate, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of three wastes, pollute the environment, and complicate post-processing, and achieve high product yields. , short reaction time and simplified post-treatment process

Active Publication Date: 2014-08-27
BENGBU BBCA MEDICINE SCI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These catalysts corrode equipment, complicate post-processing and produce "three wastes", polluting the environment

Method used

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  • Method for synthesizing triethyl citrate
  • Method for synthesizing triethyl citrate
  • Method for synthesizing triethyl citrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Preparation of catalyst

[0029] Take 6g of diatomaceous earth and add it to 100mL of 4% titanium sulfate solution, and place it at 60℃ and stir for 2h, evaporate the water in vacuum, and the remaining solid will be dried at 100℃ for 24h. Calcination at ℃ for 6h.

[0030] 2) Esterification reaction

[0031] Add 192g of absolute ethanol (or 202g of recovered ethanol: about 95% by mass), 200g of citric acid and 3g of catalyst into a reactor equipped with electromagnetic stirring, thermometer and condenser. Heat and stir at 80℃, and collect the distillate as For the next batch of materials, anhydrous ethanol was added every 45 minutes during the reaction, and the volume of the alcohol was equal to the volume of the distillate. The acid value was measured at the beginning of the reaction and at the 10th hour, and the acid value was determined with reference to GB / T1668-2008.

[0032] 3) Catalyst recovery and product purification

[0033] Filter the above crude triethyl citrate,...

Embodiment 2

[0034] Example 2 The influence of the amount of absolute ethanol on the yield

[0035] The amount of anhydrous ethanol was 144g, 168g, and 216g, and other conditions were the same as in Example 1. The results of the effect of the amount of ethanol on the reaction are shown in Table 1.

[0036] Table 1 The effect of the amount of ethanol on the reaction yield

[0037]

[0038] Note: The mass fraction of recovered ethanol in Table 1 is about 95%

Embodiment 3

[0039] Example 3 Effect of the reaction temperature of the esterification reaction on the yield

[0040] The reaction temperature of the esterification reaction was 60° C., 70° C., and 90° C., and other conditions were the same as in Example 1. The effect of the reaction temperature on the reaction yield is shown in Table 2.

[0041] Table 2 Results of the effect of reaction temperature on reaction yield

[0042]

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PUM

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Abstract

The invention provides a method for synthesizing triethyl citrate. In the method, citric acid and absolute ethanol are used as raw materials, and diatomite-supported titanium sulfate is used as a catalyst for esterification to synthesize triethyl citrate. The invention has the advantages that: the catalyst has no obvious corrosiveness and is easy to recycle and reuse, and the activity remains basically unchanged; the product yield is high, up to 99.7%; the reactant ethanol is used as the water-carrying agent, avoiding the use of toxic solvents such as toluene , and the post-treatment process is simplified; the reaction conditions are mild and the reaction time is short; the process is simple and suitable for industrial production.

Description

Technical field [0001] The invention relates to the technical field of organic chemistry synthesis, in particular to a method for synthesizing triethyl citrate. Background technique [0002] Plasticizer is a substance that is added to the polymer system and can increase the plasticity of the polymer system. In recent years, there have been many reports of carcinogenicity induced by plasticizers such as phthalates used in food packaging, children’s toys and other polymeric materials. Legislation has been made both at home and abroad to restrict their use, and they are actively seeking alternatives to phthalates. Toxic or low-toxic plasticizer. [0003] Triethyl citrate is a colorless liquid with a fruity flavor, non-toxic and non-irritating. It is mainly used as a plasticizer for cellulose and vinyl resins. It can replace potentially dangerous traditional phthalate plasticizers. It has been approved by the FDA as a non-toxic new green plasticizer in the United States. It is widely...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/704C07C67/08B01J27/053
Inventor 陶涛汪洪湖张亚孙建华韦亚锋李宏
Owner BENGBU BBCA MEDICINE SCI DEV
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