Method for synthesizing triethyl citrate

A technology of triethyl citrate and a synthesis method, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of complex post-treatment, three wastes, polluted environment, etc., and achieves simplified post-treatment process. , The effect of high product yield and short reaction time

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

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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 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.

[0030] 2) Esterification reaction

[0031] Add 192g dehydrated ethanol (or 202g recovery ethanol: mass fraction is about 95%), 200g citric acid and 3g catalyst in the reactor equipped with electromagnetic stirring, thermometer, condensing tube, 80 ℃ of heating and stirring, distillate is collected as For the next batch of feeding, absolute ethanol is added every 45 minutes during the reaction, and the volume of the added alcohol is 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 according to GB / T1668-2008.

[0032] 3) Catalyst recovery and product purification

[...

Embodiment 2

[0034] The impact of embodiment 2 dehydrated alcohol consumption on productive rate

[0035] The amount of absolute ethanol was 144g, 168g, and 216g respectively, and other conditions were the same as in Example 1.

[0036] The influence result of table 1 ethanol dosage on reaction yield

[0037]

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

Embodiment 3

[0039] The reaction temperature of embodiment 3 esterification is on the influence of productive rate

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

[0041] The influence result of table 2 temperature of reaction on reaction yield

[0042]

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PUM

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Abstract

The invention provides a method for synthesizing triethyl citrate. According to the method, citric acid and absolute ethyl alcohol are used as raw materials, and kieselguhr immobilized titanium sulfate is used as a catalyst to take esterification reaction for synthesizing the triethyl citrate. The method has the advantages that the catalyst has no obvious corrosivity, in addition, the recovery and the repeated utilization are easy, and the activity is basically maintained unchanged; the product yield is high and can reach 99.7 percent to the highest degree; reactants of ethanol are used as water-carrying agents, the use of noxious solvents such as methylbenzene is avoided, and in addition, the aftertreatment process is simplified; and the reaction condition is mild, the reaction time is short, the process is simple, and the method is suitable for industrial production.

Description

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

Claims

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Application Information

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Patent Type & Authority Applications(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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