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Method for synthesizing tributyl citrate

A technology of tributyl citrate and citric acid, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of high cost, toxicity and degradability of ionic liquids, and achieve short reaction time. , low cost, mild reaction conditions

Active Publication Date: 2015-03-25
XIAN ORIGIN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A series of studies have shown that conventional ionic liquids such as imidazole and pyridine have high cost, certain toxicity and poor degradability, and are not easy to degrade through the most widely used biological treatment process or biological self-purification.

Method used

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  • Method for synthesizing tributyl citrate
  • Method for synthesizing tributyl citrate
  • Method for synthesizing tributyl citrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step 1. Preparation of choline chloride acidic ionic liquid: add 0.5 mol choline chloride to a 500 mL flask, then add 0.5 mol citric acid, and heat and stir for 1.5 hours at a temperature of 100°C under a nitrogen atmosphere , And obtain choline chloride acid ionic liquid after cooling;

[0029] Step 2. Esterification reaction: Add 2.0 mol of n-butanol and the choline chloride acid ionic liquid described in step 1 to a four-necked flask equipped with mechanical stirring, thermometer, reflux condenser and water separator, and heat to reflux with stirring , The water produced by the reaction is separated from the water trap, and the reaction is stopped when the reaction reaches no water and then enters the water trap, and choline chloride precipitates out of the reaction system; the temperature of heating, reflux and stirring is 110°C, and the stirring rate 1500rpm;

[0030] Step 3. Separation of choline chloride: filter the reaction system after the reaction in step 2 to obt...

Embodiment 2

[0033] The methods of Example 2 and Example 3 are the same as Example 1, except that the molar amount of citric acid is 0.25 mol and 1 mol, respectively, and the molar amount of n-butanol is 1 mol and 4 mol, respectively, as shown in Table 1.

[0034] Table 1 Conversion rate and yield of Example 1 to Example 3

[0035] Example

Embodiment 4

[0037] Step 1. Preparation of choline chloride-based acidic ionic liquid: add 0.5 mol of choline chloride to a 500 mL flask, then add 0.25 mol of citric acid, and heat and stir under a nitrogen atmosphere at a temperature of 120°C for 1 hour. Obtain choline chloride acid ionic liquid after cooling;

[0038] Step 2. Esterification reaction: Add 1.0 mol of n-butanol and the choline chloride acid ionic liquid described in step 1 to a four-necked flask equipped with mechanical stirring, thermometer, reflux condenser and water separator, and heat to reflux with stirring , The water produced by the reaction is separated from the water trap, and the reaction is stopped when the reaction reaches no water and then enters the water trap, and choline chloride precipitates out of the reaction system; the temperature of heating, reflux and stirring is 160°C, and the stirring rate Is 800rpm;

[0039] Step 3. Separation of choline chloride: filter the reaction system after the reaction in step 2...

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Abstract

The invention discloses a method for synthesizing tributyl citrate. The method comprises the following steps: I, preparing a choline chloride acidic ionic liquid; II, performing esterification reaction; III, filtering the reaction system after reaction, thereby obtaining solid choline chloride and a liquid phase product; and IV, performing atmospheric distillation on the liquid phase product, washing residues generated after atmospheric distillation by using an alkali solution, adding activated carbon to decolor, filtering to remove the activated carbon, performing reduced pressure distillation on residues generated after filtration, and collecting fraction of 197-200 DEG C, thereby obtaining tributyl citrate. According to the method, choline chloride and citric acid are adopted to synthesize the acidic ionic liquid, the synthesized acidic ionic liquid is both a raw material and a catalyst, the acidic ionic liquid has esterification reaction with n-butyl alcohol to synthesize n-butyl alcohol, the efficiency of the esterification reaction is improved, the conversion rate can be greater than 90%, the choline chloride after esterification can be recycled and utilized, and the cost is low.

Description

Technical field [0001] The invention belongs to the technical field of organic chemistry synthesis, and specifically relates to a method for synthesizing tributyl citrate. Background technique [0002] Tributyl citrate is a new type of plasticizer that is non-toxic, tasteless, green and environmentally friendly. It has attracted widespread attention for its non-toxic, light fast, heat resistant, stable, and durable properties. It has become a "green substitute" for traditional phthalate plasticizers, and can be used in food packaging, medical appliances, children's toys, and personal hygiene products. Tributyl citrate has excellent compatibility with all types of cellulose, and also has good solubility for vinyl resins and certain natural resins. It can be used as a solvent-based plasticizer for vinyl acetate and other celluloses. Agent. In addition, due to its low solubility in oils, it can also be used in oil-resistant ester formulations. As a new type of non-toxic green pla...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/704B01J31/02
CPCC07C67/08C07C69/704
Inventor 王宪沛刘卫涛李小安李潇雷东卫张辉辉李文张立龙闫俊
Owner XIAN ORIGIN CHEM TECH
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