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Process for combining glycerol triacetate through acid ion liquid catalyst

A technology of glycerol triacetate and acidic ionic liquid, which is applied in the field of glycerol triacetate synthesis by acidic ionic liquid catalysts, can solve the problems of catalyst stability affecting the mechanical strength of the catalyst, waste water and waste residue discharge, and environmental protection pressure, etc., to eliminate Effect of alkali refining process, elimination of emissions, cleaning of production process

Inactive Publication Date: 2012-09-19
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although sulfuric acid or p-toluenesulfonic acid can make the reaction obtain a relatively ideal esterification rate, and the price is low, but due to the strong acidity and oxidative properties of sulfuric acid in the reaction process, side reactions such as oxidation, carbonization, polymerization, rearrangement, etc. Occurrence, poor selectivity, darker product color; at the same time, concentrated sulfuric acid will also cause corrosion to equipment, and it is difficult to recycle, resulting in high production costs, high pressure on environmental protection, etc.
[0006] For this reason, scientific and technological workers at home and abroad have carried out a lot of work to improve the process, as U.S. Patent USP3108133 discloses a kind of process of purifying glycerol triacetate under high temperature and low pressure conditions; Method for purifying glyceryl triacetate with methanol or ethanol and deacidifying glyceryl triacetate with carbon dioxide or nitrogen stripping; Chinese patents such as CN1022010330A, CN101973877A and other patents disclose the use of activated carbon adsorption and decolorization methods to refine glyceryl triacetate, from According to the patent report, the purpose is to reduce the acidity of the product triacetin, but the synthesis process of triacetin is not substantially changed, and processes such as washing with water and alkali neutralization are still required, resulting in a large amount of waste water and waste residue emissions
In the Chinese patent CN102020558A, a method for synthesizing triacetin with solid superacid as a catalyst is disclosed, which can reduce pollutant emissions in the synthesis of triacetin from the patent literature, but in the synthesis of triacetin from glycerol and acetic acid In the reaction system, there is still the influence of by-product water on the stability of the catalyst and the influence of the mechanical strength of the catalyst under strong stirring. Only the results of 10 cycles are given in the patent literature, and there are no reports of related industrial applications.

Method used

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  • Process for combining glycerol triacetate through acid ion liquid catalyst

Examples

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Effect test

Embodiment 1

[0022] Weigh 50 g of glycerin (chemically pure), 150 g of acetic acid (chemically pure), 100 g of n-propyl acetate (chemically pure), and Catalyst (BILE-3, alkyl imidazole sulfonate, produced by Enze Biomass Fine Chemical Beijing Key Laboratory) 10g, put into a 500ml glass reactor; the glass reactor is connected to a glass rectifier with 20 theoretical plates Tower, react at 100°C and stirring for 3 hours, control the temperature at the top of the rectification tower between 82-85°C; add 7.5g of acetic anhydride to the reaction kettle after reacting for 3 hours, continue at 100°C and stirring React for 1 hour; after the reaction finishes, open the vacuum pump at the top of the tower to maintain the vacuum of the reaction system at 50KPa, steam the reaction solvent n-propyl acetate and excess acetic acid, and use the mixture of solvent n-propyl acetate and acetic acid as the next batch of raw materials. The residue in the kettle is a mixture of catalyst ionic liquid and product...

Embodiment 2

[0024] Weigh 100 g of glycerin (chemically pure), 350 g of acetic acid (chemically pure), 150 g of n-propyl acetate (chemically pure), and Catalyst (BILE-3, produced by Enze Biomass Fine Chemicals Beijing Key Laboratory) 30g was added to a 1000ml glass reactor; a glass rectification tower with a theoretical plate number of 20 was connected to the glass reactor, and stirred at 120°C Under the condition of reaction for 3 hours, the temperature of the top of the rectification tower is controlled between 82-85°C; after 3 hours of reaction, add 20g of acetic anhydride to the reaction kettle, and continue to react for 1 hour at 120°C under stirring conditions; after the reaction, Turn on the vacuum pump at the top of the tower, maintain the vacuum degree of the reaction system at 20KPa, distill off the reaction solvent n-propyl acetate and excess acetic acid, the mixture of solvent n-propyl acetate and acetic acid is used as the next batch of raw materials, and the remainder in the r...

Embodiment 3

[0026]Weigh 100 g of glycerin (chemically pure), 400 g of acetic acid (chemically pure), 200 g of n-propyl acetate (chemically pure), and Catalyst (BILE-3, produced by Enze Biomass Fine Chemicals Beijing Key Laboratory) 40g was added to a 1000ml glass reactor; a glass rectification tower with a theoretical plate number of 20 was connected to the glass reactor, and stirred at 140°C Under the condition of reaction for 3 hours, control the temperature of the top of the rectification tower between 82-85°C; after reacting for 3 hours, add 30g of acetic anhydride to the reactor, and continue to react for 1 hour at 140°C under stirring conditions; after the reaction, Turn on the vacuum pump at the top of the tower, maintain the vacuum degree of the reaction system at 30KPa, distill off the reaction solvent n-propyl acetate and excess acetic acid, the mixture of solvent n-propyl acetate and acetic acid is used as the next batch of raw materials, and the remainder in the reaction kettle...

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Abstract

The invention relates to a process for combining glycerol triacetate through an acid ion liquid catalyst. The process includes utilizing glycerol, acetic acid, a solvent and the catalyst as raw materials to conduct esterification reaction, then adding acetic anhydride to conduct acylation reaction, separating the solvent with excess acetic acid after the acylation reaction is finished, utilizing the mixture of the solvent and the acetic acid to serve as a raw material of the next batch, separating the mixture of the ion liquid catalyst and a glycerol triacetate product in remainders in a reaction kettle, using the ion liquid catalyst in circulation mode and removing micro acetic acid in glycerol triacetate to produce food-grade glycerol triacetate. Detailed process is shown in an instruction book. The process has the advantages that the ion liquid catalyst does not corrode equipment, and side reactions such as oxidation, carbonization and polymerization caused by a liquid strong acid catalyst are basically removed. The catalyst is repeatedly used, pollution of waste water to environment is removed, and production cost is reduced. Discharge of waste sludge and alkali liquor is removed. The process is short in flow and free of pollutant discharge and achieves clean production process. The yield of the glycerol triacetate is 99%, and acidity of the glycerol triacetate is lower than 0.002%.

Description

technical field [0001] The invention relates to fine chemical product technology, in particular to a process for synthesizing glycerol triacetate with an acidic ionic liquid catalyst. Background technique [0002] Glyceryl triacetate, also known as glycerol triacetate, is a colorless, odorless, oily liquid, non-toxic and non-irritating. Its English name is Glycerol Triacetate, its molecular formula is C9H14O6, and its molecular weight is 218.21. [0003] Glyceryl triacetate is miscible with organic solvents such as alcohol, ether, benzene, and chloroform, and can dissolve high molecular compounds such as nitrocellulose, acrylic resin, and polyvinyl acetate. Because triacetin has good gelling effect and physiological inertness, it is widely used as a plasticizing and curing agent for cellulose acetate in cigarette filters, a food additive, a cosmetic fixative, and a lubricating matrix. Glyceryl triacetate is widely used in tobacco, food and metallurgical industries as a saf...

Claims

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Application Information

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IPC IPC(8): C07C69/18C07C67/08
CPCY02P20/54Y02P20/584
Inventor 姚志龙尹振晏孙培永庞小英袁吴魏秦岩
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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