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Purification method of glycerol triacetate

A technology of triacetin and a purification method, applied in the field of triacetin purification, can solve problems such as failure to meet high standard requirements, and achieve the effects of optimized production process, simple separation device and easy operation

Active Publication Date: 2018-11-30
云南省玉溪市溶剂厂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This technology can indeed remove some volatile impurities contained in triacetin, but it still cannot meet the high standard requirements of the tobacco and fine chemical industries for fine chemicals triacetin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A method for purifying triacetin, comprising the following steps:

[0020] A. Stock solution preparation:

[0021] ①Feeding: Add acetic acid and glycerin according to the mass ratio (3-4):1, add catalyst and dehydrating agent at the same time, start heating after feeding;

[0022] ② Esterification: Rely on the dehydrating agent and water to form an azeotrope to continuously remove the water generated by the reaction. When the speed of the dehydrating agent to take out the water slows down to the point where only the water-carrying agent returns, the esterification ends;

[0023] ③ Preliminary deacidification: control the temperature and steam most of the excess acetic acid;

[0024] ④ Acylation: Acetic anhydride is added at a temperature of 100-110°C for acylation and heating at the same time;

[0025] ⑤ High deacidification, refining, washing, adsorption, filtration, and drying: After acylation, add alkali to neutralize, heat up to deacidify, and finally wash, absorb...

Embodiment 2

[0029] The specific implementation method is the same as in Example 1, except that the internal pressure modified PTFE ultrafiltration membrane with a molecular weight cut-off of 160 is used, the pressure drop is 0.3MPa, and the stock solution obtained in step 5 is passed through ultrafiltration at a temperature of 28-32°C. Membrane device, the permeate is directly returned to the feeding recovery, and the concentrated liquid, that is, the product, directly enters the product storage tank. The purity of the concentrate reaches 99.68%.

[0030] The specific modification method of the internal pressure modified PTFE ultrafiltration membrane is as follows: through the chemical reaction between the corrosive liquid and the PTFE ultrafiltration membrane, part of the fluorine atoms on the surface of the material are torn off, so that a carbonized layer and a carbonized layer are left on the surface. Some polar groups increase the surface energy, reduce the contact angle, and change ...

Embodiment 3

[0032] The specific implementation is the same as in Example 1, except that the internal pressure modified PTFE ultrafiltration membrane with a molecular weight cut-off of 170 is used, the pressure drop is 0.3MPa, and the stock solution obtained in step 5 is passed through ultrafiltration at a temperature of 28-32°C. Membrane device, the permeate is directly returned to the feeding recovery, and the concentrated liquid, that is, the product, directly enters the product storage tank. The purity of the concentrate reaches 99.68%.

[0033] The specific modification method of the internal pressure modified PTFE ultrafiltration membrane is as follows: through the chemical reaction between the corrosive liquid and the PTFE ultrafiltration membrane, part of the fluorine atoms on the surface of the material are torn off, so that a carbonized layer and a carbonized layer are left on the surface. Some polar groups increase the surface energy, reduce the contact angle, and change from di...

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PUM

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Abstract

The invention discloses a purification method of glycerol triacetate. The existing glycerol triacetate cannot meet the high-standard requirements of tobacco industry and fine chemical industry on a fine chemical glycerol triacetate. According to the purification method provided by the invention, an internal-pressure-type modified polytetrafluoroethylene (PTFE) ultra-filtration membrane with a molecular weight cutoff of 150-170 is adopted, the pressure drop is 0.25-0.35MPa, a prepared stock solution flows through a ultrafiltration membrane device at a temperature of 28-32 DEG C, the obtained permeate liquid is directly returned for feeding and recycling, and the obtained concentrated solution, namely the product, directly enters a product storage tank. Phase change does not occur in the purification process by using the ultrafiltration membrane, and secondary pollution is avoided. Only pressure is adopted as separation power of the ultrafiltration membrane in the filtering process, so that the separation device is simple, the operation is simple and convenient, and the process parameters are easy to control. The separation precision is high, and an adsorption function is achieved while the separation is carried out. The method is high in processing efficiency, continuous production can be realized, the purity of the obtained glycerol triacetate reaches 99.6% or above, and no peculiar smell is generated.

Description

technical field [0001] The invention relates to the technical field of separation and purification, in particular to a method for purifying triacetin. Background technique [0002] Triacetin is a colorless, odorless oily liquid, slightly soluble in water, easily soluble in alcohol, ether and other organic solvents. The boiling point is usually in the range of 258-260°C. It is non-toxic, non-irritating, has good gelling effect and physiological inertness, and is mainly used as a plasticizer for acetate fiber tip rods for cigarette filters, and a fixed flavoring agent for spices and essences. , cosmetics manufacturing, edible gum-based products manufacturing, special solvents and non-toxic plasticizers for food plastic products, curing agents for casting resins, etc. It is mainly used as an adhesive plasticizer for cigarette filters in China, and its market demand is increasing year by year, and its application prospect is broad. [0003] At present, the production of glycer...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/48C07C67/56C07C69/18B01D67/00B01D61/14
CPCB01D61/145B01D67/0093B01D2323/36C07C67/08C07C67/48C07C67/56C07C69/18
Inventor 蒋海明赖正波潘光亮杜云忠陈艳琼普江涛
Owner 云南省玉溪市溶剂厂有限公司