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Preparation method and system of ethylene glycol monopropyl ether

A technology of monopropyl ether and preparation system, which is applied in the direction of ether preparation, separation method, and alkylene oxide preparation ether, etc., which can solve the problems of low purity of synthetic crude products, high production cost, and many by-products, so as to avoid the possibility of material contamination , less waste, less by-products

Active Publication Date: 2020-10-09
ZHEJIANG HUANGMA TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems of low purity of synthetic crude product, many by-products, complex procedures and high production cost in the current synthesis process route of ethylene glycol monopropyl ether, the present invention provides a catalyst with high catalytic selectivity, low production cost, few by-products, Easy-to-operate, efficient preparation method and system for ethylene glycol monopropyl ether

Method used

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  • Preparation method and system of ethylene glycol monopropyl ether
  • Preparation method and system of ethylene glycol monopropyl ether
  • Preparation method and system of ethylene glycol monopropyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Such as figure 1 and 2 As shown, this embodiment provides a preparation system for ethylene glycol monopropyl ether, including an integrated reaction kettle for addition and rectification. The top is connected with rectifying tower 5. The main body 4 of the reaction kettle is provided with an interlayer 17 for feeding a temperature control medium, such as steam, cooling water (the inlet and outlet of steam and cooling water are just opposite), oil and the like. Reactor main body 4 comprises reaction feed port 10, reaction discharge port 11, protective gas port 13 and material vapor outlet, and reaction feed port 10 and reaction discharge port 11 are respectively arranged on the top and the bottom of reaction kettle main body 4, and reaction feed The feed port 10 and the reaction discharge port 11 are provided with a control valve 18; the reaction discharge port 11 is also connected to the reaction feed port 10 through a return pipe 23, and the return pipe 23 is provid...

Embodiment 2

[0032] Add 60kg of n-propanol and 0.4‰ (accounting for the ratio of n-propanol and ethylene oxide total material, the same below) zinc methanesulfonate catalyst to the addition reaction and rectifying integrated kettle, vacuumize with vacuum pump, adopt N 2Replace the air in the reactor. After three replacements, the degree of evacuation is ≥-0.096MPa. After the material is heated to 100°C, the temperature is raised while adding ethylene oxide. Control the reaction temperature at 165-180° C., and control the total amount of ethylene oxide added to 14 kg. After adding ethylene oxide, keep warm and continue to react until the pressure no longer drops. After the reaction, cool down to 50°C and fill with N 2 To 0.02MPa, take a sample to detect the composition of the crude product, open the control valve of the return pipe, the reaction outlet and the reaction inlet, and filter and recover the catalyst. After the catalyst is recovered, close the control valves of the reaction ou...

Embodiment 2～7

[0046] Table 2 Embodiment 2~7 finished product index

[0047]

[0048] Obtained by table 2 data, the product ethylene glycol monopropyl ether content that rectification method of the present invention makes is more than 99.85%, n-propanol is lower than 0.002%, diethylene glycol monopropyl ether is lower than 0.003% .

[0049] 3. Application of catalyst

[0050] Synthetic reaction process condition is the same as embodiment 3, only changes catalyst type and catalyst mechanical application times (catalyst recovery cover amount is not enough to add new catalyst slightly again), this is example mechanically with zinc methanedisulfonate and p-toluenesulfonic acid zinc, actual It doesn't stop there. The specific indicators of the crude product are shown in Table 3 and Table 4.

[0051] Table 3 Mechanical parameters and crude product index of zinc methanedisulfonate catalyst

[0052]

[0053] Table 4 Application parameters and crude product index of zinc p-toluenesulfonate ...

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Abstract

The invention provides a preparation method and system of ethylene glycol monopropyl ether. The preparation method adopts the following reaction equations: n-propanol and ethylene oxide react under the action of a catalyst to synthesize an ethylene glycol monopropyl ether crude product; and rectification under vacuum is carried out on the crude product to obtain an ethylene glycol monopropyl etherfinished product. The preparation system comprises an addition and rectification integrated reaction kettle; the addition and rectification integrated reaction kettle comprises a reaction kettle mainbody; a rectification tower is connected above the reaction kettle main body; the reaction kettle main body comprises a reaction feed port, a reaction discharge port and a material steam outlet; thematerial steam outlet is connected with the rectification inlet of the rectification tower; the rectification tower is provided with the rectification inlet and a rectification outlet and is also connected with a vacuum device. The ethylene glycol monopropyl ether prepared by the method has high purity (more than or equal to 99.8%) and few byproducts.

Description

technical field [0001] The invention belongs to the technical field of organic compound synthesis, and in particular relates to a preparation method and system of ethylene glycol monopropyl ether. Background technique [0002] Ethylene glycol monopropyl ether, also known as propoxyethanol, is a colorless transparent liquid, soluble in organic solvents such as ethanol and acetone, and miscible with water. The dissolving power of ethylene glycol monopropyl ether is very strong, and its kauri butanol value (KB value) is 5 times that of aromatic hydrocarbon solvents and 17 times that of aliphatic hydrocarbon solvents, so ethylene glycol monopropyl ether is Excellent solvent, widely used in nitrocellulose, industrial coatings and other fields. Due to the slow evaporation rate of ethylene glycol monopropyl ether, it has obvious effects on improving the gloss of varnishes and preventing peeling, so it can be used as a thinner in quick-drying paints and enamel paints to increase th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/03C07C43/13B01J19/18B01D3/14B01D3/00
CPCC07C41/03B01J19/18B01D3/009B01D3/14C07C43/13Y02P20/584
Inventor 马定连金一丰王新荣余渊荣王敏
Owner ZHEJIANG HUANGMA TECH
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