Preparation method of ethylene glycol monoacetate and ethylene glycol diacetate

A technology of monoacetate and ethylene glycol 2, applied in the field of organic compound synthesis, can solve problems such as difficulty in product separation, and achieve the effects of simple process, less three wastes and fast reaction speed

Active Publication Date: 2013-07-03
深圳市飞扬特化新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the reaction produces water, and the target product is miscible with water and unreacted raw materials to form a s

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Preliminary transesterification reaction

[0025] Add 400g (6.451mol) of ethylene glycol into a four-necked flask with a separation column, reflux condenser, and thermometer, add 15g (0.2674mol) of KOH, add 1000g (8.621mol) of sec-butyl acetate, and raise the temperature to 110 The reaction was carried out at ℃ for 2h.

[0026] (2) break the balance of transesterification chemical reaction

[0027] After the previous step reaction is completed, keep the temperature at 110°C, distill the produced sec-butanol (which contains a small amount of sec-butyl acetate and ethylene glycol monoacetate), and analyze the distilled mixture by gas chromatography every 2h The content of sec-butyl acetate in the middle, calculate the amount of the sec-butyl acetate that evaporates in this section of time interval, and add sec-butyl acetate in the reaction system, the amount of sec-butyl acetate added each time is distilled 2 times the amount of sec-butyl acetate out. The duration ...

Embodiment 2

[0047] Pilot production of 150L stainless steel reactor. The reaction steps are similar to Example 1.

[0048] (1) Preliminary transesterification reaction:

[0049] Put 40kg (655.7mol) of ethylene glycol, 100kg (862mol) of sec-butyl acetate and 1.5kg (26.7mol) of KOH into a clean and dry reaction distillation column, start stirring and raise the temperature to 120°C within 2 hours , the transesterification reaction starts, keep warm at 120°C for 2 hours, and the transesterification reaction reaches equilibrium;

[0050] (2) breaking the balance of transesterification chemical reaction:

[0051] A, after preliminary transesterification reaction 2 hours, slowly warming up to reflux, the control reflux ratio is 3, extracts sec-butanol crude product (with a little sec-butyl acetate that does not participate in reaction) from tower top, along with sec-butanol Continuously separate out, the balance of transesterification reaction shifts to the right, and along with the carrying ...

Embodiment 3

[0072] 1m 3 Stainless steel reactor production, this step is similar to the operation step in the embodiment one.

[0073] The equipment used is composed of a batch reactive rectification tower and a sec-butanol-sec-butyl acetate separation tower, and the detection equipment is an Agilent 7820A gas chromatograph detector.

[0074] The batch reactive distillation tower is a packed tower with a diameter of 0.3m and a height of 2m, filled with 1m high wire mesh corrugated packing, and the number of theoretical plates is 7.

[0075] The sec-butanol-sec-butyl acetate separation tower is a packed tower with a diameter of 300mm and a height of 16000mm, with structured packing inside, and the number of theoretical plates is 100.

[0076] (1) Preliminary transesterification reaction

[0077] Put 300kg (4838.7mol) of raw material ethylene glycol, 700kg (6034.5mol) of sec-butyl acetate and 2.7kg KOH (213.9mol) into a clean and dry reactive distillation column, start stirring and raise ...

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Abstract

The invention discloses a preparation method of ethylene glycol monoacetate and ethylene glycol diacetate. The preparation method is to take sec-butyl acetate and ethylene glycol as raw materials, perform transesterification in the presence of a base catalyst to prepare ethylene glycol monoacetate and ethylene glycol diacetate, and comprises the specific steps of primary transesterification, chemical reaction equilibrium breaking of transesterification, final-phase transesterification, separation and purification of the products ethylene glycol monoacetate and ethylene glycol diacetate, and the like. The preparation method of ethylene glycol monoacetate and ethylene glycol diacetate is high in product yield, quick in reaction speed, low in power consumption, easy to separate and purify the products, low in cost and simple in technique. In addition, the synthesis method provided by the invention can prepare an important common solvent sec-butyl alcohol. The products are all required by application, so that the utilization ratio of the products is high, the three wastes are less, and the preparation method is green and environment-friendly.

Description

technical field [0001] The invention relates to the field of synthesis of organic compounds, in particular to a method for simultaneously preparing ethylene glycol monoacetate and ethylene glycol diacetate by using a transesterification method. Background technique [0002] Ethylene glycol diacetate (EGDA) is a new generation of high boiling point environmentally friendly strong solvent, which has the advantages of good smell, narrow distillation range, stable composition, and quick drying in winter. It is not only miscible with alcohol, ether and benzene, but also has good water solubility. It is an excellent solvent for various organic resins, especially nitrocellulose. It is often used in paints and coatings as nitro spray paint, printing ink, fiber Solvent for plain esters and fluorescent paints. Like EGDA, ethylene glycol monoacetate is also an important non-optical pollution-free high-boiling solvent. It is slightly soluble in water, soluble in ethanol, ether, and ben...

Claims

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Application Information

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IPC IPC(8): C07C67/03C07C69/16C07C31/12C07C29/128
CPCY02P20/52
Inventor 傅兵李启玉蒋茶胡江陈建良
Owner 深圳市飞扬特化新材料有限公司
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