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Polyglycol synthesizing method

A synthesis method, the technology of polyethylene glycol, applied in the field of synthesis of polyethylene glycol, can solve the problems of increasing the load of circulating pumps, and achieve the effects of avoiding working pressure, improving mass transfer efficiency, and reducing by-products

Inactive Publication Date: 2017-08-25
JIANGSU LINGFEI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a method for synthesizing polyglycol, which can reduce the problem of sudden stop caused by the increase of the load of the circulation pump caused by the viscosity of the material caused by the circulation reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The reactor is replaced with nitrogen to remove the air, and filled with nitrogen protection; heated to 100 ° C, vacuum dehydration; the mass fraction of 30% ethylene oxide is added to the reactor, and the upper end of the reactor is filled with ethylene oxide in a gaseous state; Ethylene glycol with a fraction of 5% and potassium hydroxide with a mass fraction of 0.2% are sent into the reactor through the nozzle for atomization reaction, and the circulation pump is turned on at the same time; the product at the bottom of the reactor is recycled to the nozzle through the circulation pump and sprayed into the reactor Middle; when the reaction temperature reaches 140°C and the pressure reaches 0.2 MPa, add the remaining amount of ethylene oxide, turn off the circulating pump, and turn on the stirrer; continue to react for 40 minutes, and when the reaction temperature and reaction pressure gradually decrease, the reaction ends.

Embodiment 2

[0020] The reactor was replaced with nitrogen to remove all the air, and filled with nitrogen protection; heated to 100 ° C, vacuum dehydration; 30% mass fraction of propylene oxide was added to the reactor, and the propylene oxide was in a gaseous state. The upper end of the reactor was filled; the mass fraction was 5% ethylene glycol and potassium hydroxide with a mass fraction of 0.2% are sent into the reactor through the nozzle for atomization reaction, and the circulation pump is turned on at the same time; the product at the bottom of the reactor is recycled to the nozzle through the circulation pump and sprayed into the reactor; When the reaction temperature reaches 140° C. and the pressure reaches 0.2 MPa, add a surplus of propylene oxide, turn off the circulation pump, and turn on the stirrer; continue the reaction for 40 minutes, and when the reaction temperature and the reaction pressure gradually decrease, the reaction ends.

Embodiment 3

[0022] The reactor was replaced with nitrogen to remove the air, and filled with nitrogen protection; heated to 100 ° C, vacuum dehydration; the mass fraction of 35% ethylene oxide was added to the reactor, and the ethylene oxide filled the upper end of the reactor in a gaseous state; Ethylene glycol with a fraction of 8% and potassium hydroxide with a mass fraction of 0.2% are sent to the reactor through the nozzle for atomization reaction, and the circulation pump is turned on at the same time; the product at the bottom of the reactor is recycled to the nozzle through the circulation pump and sprayed into the reactor Middle; when the reaction temperature reaches 140°C and the pressure reaches 0.2 MPa, add the remaining amount of ethylene oxide, turn off the circulating pump, and turn on the stirrer; continue to react for 40 minutes, and when the reaction temperature and reaction pressure gradually decrease, the reaction ends.

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Abstract

The invention discloses a polyglycol synthesizing technology, relates to the field of polymer synthesis and can achieve high-efficiency safe reaction. The polyglycol synthesizing technology comprises the steps of replacing air in a reactor with nitrogen to thoroughly remove the air and inflating nitrogen for protection; heating to 100 to 120 DEG C and performing vacuum dewatering; adding ethylene oxide / dimethylmethane in mass fraction of 25% to 40% into the reactor and filling the upper end of the reactor with the ethylene oxide / dimethylmethane in a gas state; sending ethylene glycol in mass fraction of 5% to 10% and potassium hydroxide in mass fraction of 0.2% into the reactor through a spray head to perform atomizing reaction and starting a circulating pump at the same time; circulating a product at the bottom of the reactor through the circulating pump to the spray head again to be sprayed into the reactor; when reaction temperature reaches 140 DEG C to 150 DEG C and pressure reaches 0.2 to 0.4MPa, adding the balance of ethylene oxide / dimethylmethane, shutting up the circulating pump and starting a stirrer; continuing to react for 40 minutes and finishing reaction when the reaction temperature and the reaction pressure both gradually decrease.

Description

technical field [0001] The invention belongs to the field of polymer synthesis, in particular to a method for synthesizing polyglycol. Background technique [0002] In the prior art, conventional reactors and Prius reactors are generally used to produce polymers. Prius external circulation ethoxylation equipment has the advantages of high efficiency, safety, energy saving, and fast reaction rate, and is widely used in gas-liquid chemical product reaction, but Prius external circulation ethoxylation equipment is only suitable for the synthesis of low and medium molecular weight products. When producing and stirring high viscosity materials and products with large molecular weight, the load of the circulating pump is increased, which is prone to sudden stop. , and there is a greater safety risk in the continued reaction of materials in the kettle. [0003] Polyethylene glycol is a linear chain structure composed of repeated oxyethylene groups, with a hydroxyl group at each en...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28
CPCC08G65/2609C08G65/2648C08G2650/58
Inventor 钱飞
Owner JIANGSU LINGFEI CHEM
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