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A kind of preparation method of glyceryl triacetate

A technology of glyceryl triacetate and glyceryl acetate, which is applied in the field of preparation of glyceryl triacetate, can solve the problems of reactants polluting the environment, achieve the effects of low reaction temperature, lower production costs, and lower energy consumption

Active Publication Date: 2015-12-02
吴峰
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is to provide a preparation method of glycerol triacetate, which overcomes the defect that the reactants pollute the environment in the prior art

Method used

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  • A kind of preparation method of glyceryl triacetate

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Embodiment 1

[0027] Such as figure 1 Shown, the preparation method step of triacetin of the present invention is as follows:

[0028] 1. Mix the amino acid ionic liquid and glycerol, the mass ratio of amino acid ionic liquid and glycerin is 20:100; add the mixture of glycerin and amino acid ionic liquid into the reaction kettle, and heat to 120°C.

[0029] 2. Add methyl acetate to the mixed solution of glycerin and amino acid ionic liquid to carry out transesterification reaction with glycerin to generate glyceryl acetate and methanol; discharge part of the mixed gas of methyl acetate and methanol, control the pressure in the reactor at 0.4MPa, and react 8 hours.

[0030] 3. After the transesterification reaction is completed, the reactant is left to settle for 2 hours, and the amino acid ionic liquid catalyst layer in the lower layer is discharged.

[0031] 4. Cool the mixed glycerol acetate in the upper layer to 80°C, stir and add acetic anhydride, the mass ratio of acetic anhydride to...

Embodiment 2

[0036] 1. Mix N-R-N-methylimidazolium hydroxide ionic liquid with glycerol, the mass ratio of N-R-N-methylimidazolium hydroxide ionic liquid to glycerol is 10:100, mix glycerin with N- The R-N-methylimidazolium hydroxide ionic liquid mixture is added into the reaction kettle, and the temperature is raised to 160°C.

[0037] 2. Pump methyl acetate from the bottom of the reactor into the mixture of glycerin and N-R-N-methylimidazole hydroxide ionic liquid in the reactor for transesterification reaction with glycerin to generate glyceryl acetate and methanol; open The exhaust valve on the upper part of the reaction kettle discharges part of the mixed gas of unreacted methyl acetate and methanol, controls the pressure in the reaction kettle at 0.6MPa, and the reaction time is 6 hours.

[0038] 3. After the transesterification reaction is completed, the reactant is left to settle for 4 hours, and the N-R-N-methylimidazolium hydroxide ionic liquid catalyst layer in the lower layer i...

Embodiment 3

[0044] 1. Mix 1-(N,N-dimethylaminoethyl)-2,3-dimethylimidazolium trifluoromethanesulfonate ionic liquid with glycerol, and mix glycerin with 1-(N,N-di Methylaminoethyl)-2,3-dimethylimidazolium trifluoromethanesulfonate salt ionic liquid mixture was added to the reaction kettle and heated to 140°C.

[0045] 2. Pump methyl acetate from the bottom of the reactor into the glycerin and 1-(N,N-dimethylaminoethyl)-2,3-dimethylimidazolium trifluoromethylsulfonate ionic liquid in the reactor Carry out transesterification reaction with glycerol in the mixed solution to generate glyceryl acetate and methanol; open the exhaust valve on the upper part of the reactor to discharge part of the unreacted mixed gas of methyl acetate and methanol, control the pressure in the reactor at 0.5MPa, and react The time is 6 hours.

[0046]3. After the transesterification reaction, the reactant was left to settle for 2 hours, and the 1-(N,N-dimethylaminoethyl)-2,3-dimethylimidazole trifluoromethylsulfo...

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Abstract

A method for preparing the glycerol triacetate comprises the following steps of mixing basic ionic liquid and glycerin, adding the mixed liquid in a reaction kettle and heating the mixed liquid to 120-160DEG C, wherein the weight ratio of the basic ionic liquid and the glycerin is 2:100-20:100; adding methyl acetate in the mixed liquid to carry out transesterification, and generating acetoglyceride and methyl alcohol; controlling the pressure inside the reaction kettle to be 0.4-0.6MPa, and carrying out reaction for 6-8 hours; carrying out still standing and sedimentation for 2-4 hours, and discharging the lower basic ionic liquid catalyst layer; cooling the mixed acetoglyceride in the reaction kettle to 80-120DEG C, adding acetic anhydride with stirring to carry out acetylation action with acetate glyceride and diacetate glyceride in the acetoglyceride for 1-2 hours, wherein the weight ratio of the acetic anhydride and the glycerin is 20:100-30:100; carrying out distillation at 300-400Pa vacuum degree under 120-130DEG C to obtain glycerol triacetate products with purity higher than 99.7%. The method for preparing the glycerol triacetate is free from pollutants, clean and environmentally friendly in technology, low in reaction temperature and energy consumption and low in catalyst loss rate; the catalyst can be used repeatedly, and thus production cost is low.

Description

technical field [0001] The invention relates to a preparation method of glyceryl triacetate. Background technique [0002] Glyceryl triacetate is a good solvent and plasticizer, widely used in food, perfume, printing and dyeing and tobacco industries. The traditional method for preparing glyceryl triacetate is to use glycerin and acetic acid as raw materials to carry out esterification under the action of an acidic catalyst to generate glyceryl triacetate. This method has the following defects: since the method uses acetic acid as an acidic catalyst to carry out the esterification reaction of glycerol, a large amount of acetic acid-containing wastewater is generated in the reactant, which brings great pressure on wastewater treatment to production enterprises, and often becomes a source of environmental pollution. serious pollution source. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a preparation method of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/18C07C67/08C07C67/03
Inventor 韦海斌吴峰
Owner 吴峰