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Method for polymerization of diglycol and ethylene oxide

A technology for ethylene oxide and polymerization, applied in the direction of chemical recovery, etc., can solve the problems of difficult recovery and utilization of rectification substrates, cumbersome separation and purification steps, waste of resources and environment, etc., and achieves reduction of neutralization process, easy removal, The effect of increasing production capacity

Active Publication Date: 2017-06-16
SHANGHAI DONGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem solved by the present invention is to overcome the potential safety hazards in the existing triethylene glycol preparation method, the separation and purification steps are cumbersome, the energy consumption is high, the yield is reduced due to the large amount of metal ions contained in the product, and the rectification substrate is difficult. Problems such as recycling and resource waste and potential environmental pollution, thereby provide a kind of method that diethylene glycol and ethylene oxide are carried out polymerization reaction different from prior art, the method reaction activity of the present invention is high, selectivity is good, The catalyst is easy to remove from the product, and the product does not affect the color of the rectification substrate after high-temperature rectification

Method used

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  • Method for polymerization of diglycol and ethylene oxide
  • Method for polymerization of diglycol and ethylene oxide
  • Method for polymerization of diglycol and ethylene oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0031] (1) Drop into 300g diethylene glycol, 1g 75% tetramethylammonium hydroxide aqueous solution in the dry 2L pressure reaction kettle, seal the reaction kettle; Replace the air in the reaction kettle with nitrogen 3 times, start stirring; be heated up to 100 ℃, Slowly add 187g of ethylene oxide to carry out the copolymerization reaction; wherein, by controlling the adding speed of ethylene oxide, the reaction pressure is kept at 0.3MPa, and the reaction temperature is kept at 140°C for 3 hours; after the ethylene oxide is completely introduced, Aging at 140°C for 30 minutes, and then degassing at -0.09MPa for 50 minutes to obtain a colorless and transparent triethylene glycol mixture. The content (weight percentage) of each component was analyzed by gas chromatography, and the results are listed in Table 1. .

[0032](2) Move the triethylene glycol mixture into the rectification tower, heat up, and distill diethylene glycol under reduced pressure at 104°C / 0.66KPa (170°C at...

Embodiment 2

[0035] (1) Put 300g of diethylene glycol and 2.3g of 50% methyltriethoxyammonium hydroxide aqueous solution into a dry 2L pressure reactor, seal the reactor; replace the air in the reactor with nitrogen for 3 times, start stirring; heat up To 100°C, slowly add 162g of ethylene oxide to carry out the copolymerization reaction; wherein, by controlling the adding speed of ethylene oxide to keep the reaction pressure at 0.35MPa, the reaction temperature is kept at 160°C for 6h; the ethylene oxide is completely After passing through, mature at 160°C for 30min, and then degas at -0.09MPa for 50min to obtain a colorless and transparent triethylene glycol mixture. Analyze the content of each component (percentage by weight) by gas chromatography, and the result is Listed in Table 1.

[0036] (2) Rectification process is with embodiment 1.

Embodiment 3

[0038] (1) Put 300g of diethylene glycol and 0.7g of 75% tetramethylammonium hydroxide aqueous solution into a dry 2L pressure reactor, seal the reactor; replace the air in the reactor with nitrogen for 3 times, start stirring; heat up to 100°C , slowly add 149g of ethylene oxide to carry out copolymerization reaction; wherein, by controlling the adding speed of ethylene oxide to keep the reaction pressure at 0.30MPa, the reaction temperature is kept at 150°C for 4h; after the ethylene oxide is completely introduced , matured at 150°C for 30min, and then degassed at -0.09MPa for 50min to obtain a colorless and transparent triethylene glycol mixture. The content of each component (weight percentage) was analyzed by gas chromatography, and the results are listed in the table. 1.

[0039] (2) Rectification process is with embodiment 1.

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Abstract

The invention discloses a method for polymerizing diethylene glycol and ethylene oxide. The method comprises the following steps: under the protection of inert gas and / or nitrogen, and in the presence of a quaternary ammonium base, diethylene glycol It can be polymerized with ethylene oxide at a molar ratio of 1:1 to 1:3. The method of the present invention has high reaction activity and good selectivity, the catalyst can be easily removed, the neutralization process is reduced, and the rectification substrate has a light color, which can be directly used to produce products such as polyethylene glycol and polyethylene glycol dimethyl ether ; The method of the present invention can not only improve the production capacity of triethylene glycol and / or tetraethylene glycol, but also can co-produce other polymerized glycols, such as pentaethylene glycol; through the process of the present invention, not only the vertical development of products can be realized , to create higher economic benefits, but also reduce investment in environmental protection and reduce the impact on the environment.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for polymerizing diethylene glycol and ethylene oxide. Background technique [0002] Triethylene glycol (molecular formula: HOC 2 h 4 OC 2 h 4 OC 2 h 4 OH) is one of the important glycols, mainly used as solvent, desiccant, lubricant, plasticizer. Triethylene glycol is easy to dehydrate from air and other gases, and is currently widely used as a natural gas dehydrating agent. The production method of triethylene glycol is mainly obtained through multi-step separation from the waste liquid produced by the process of producing ethylene glycol from ethylene oxide. Due to the complex composition of waste liquid, water, ethylene glycol, diethylene glycol (molecular formula: HOC 2 h 4 OC 2 h 4 OH) and triethylene glycol, it also contains salts such as sodium sulfate, sodium chloride, sodium nitrate, sodium glycolate, sodium formate, ethyl chloride, and sodium hydro...

Claims

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Application Information

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IPC IPC(8): C08G65/28
CPCY02P20/582C08G65/2609C08G65/2672
Inventor 方洇何志强董建国杨学园时巍平
Owner SHANGHAI DONGDA CHEM
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