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Method for synthesizing high-molecular-weight pentaerythritol polyoxyethylene ether

A technology of pentaerythritol polyoxyethylene ether and high molecular weight, which is applied in the field of synthesis of high molecular weight pentaerythritol polyoxyethylene ether, can solve the problems of dark product color, difficult solvent recovery and processing, complex process, etc., to reduce the generation of side reactants, Fewer varieties, the effect of improving economic efficiency

Pending Publication Date: 2020-08-14
JIAHUA CHEM MAOMING
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At the same time, to synthesize high-molecular-weight pentaerythritol polyoxyethylene ether, only ethylene oxide and PO can be used, and its molecular weight can only reach 4500-7500. There is no single process for purely connecting ethylene oxide to a high molecular weight of 7000-10000.
[0004] Synthesis of high-molecular-weight pentaerythritol polyoxyethylene ether usually uses amine catalysts (triethylamine, ammonia water, trimethylamine) at this stage, which is easy to produce by-products and the color of the synthesized product is too dark. In addition, solvents (ethylene glycol dimethyl ether ) process is too complex, solvent recovery is difficult

Method used

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  • Method for synthesizing high-molecular-weight pentaerythritol polyoxyethylene ether

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Effect test

Embodiment 1

[0034] Embodiment 1: the first step, prepare materials, pentaerythritol is 15%, potassium hydroxide is 0.5%, ethylene oxide is 84%, and glacial acetic acid is 0.5%, under the condition of 90 ℃ of temperature in reactor, in reactor Vacuumize to -95KPa, put in 0.5% potassium hydroxide, stir, use negative pressure to put 15% pentaerythritol into the kettle, after feeding, pump negative pressure to -95KPa in the reactor, replace with nitrogen gas in the reactor, repeat replacement for 4 Then pressurize to make the pressure of the reactor reach -50KPa, control the temperature of the reactor at 80°C, first put in 2.8% ethylene oxide, raise the temperature to 90°C, trigger the reaction activation period, and then continue to put 81.2% cyclooxygen into the reactor Oxygen, during the feeding process, the temperature gradually rises from 90°C to 120°C, and then the temperature of the reactor is controlled to no longer rise, and the pressure in the reactor cannot exceed 350KPa. After the ...

Embodiment 2

[0036] Embodiment 2: prepare materials, pentaerythritol is 17%, potassium hydroxide is 0.5%, oxirane is 82%, glacial acetic acid is 0.5%, under the condition of 90 ℃ of temperature in the reactor, vacuumize in the reactor to - 95KPa, put in 0.5% potassium hydroxide, stir, use negative pressure to put 17% pentaerythritol into the kettle, after feeding, pump the negative pressure to the reaction kettle to -95KPa, replace it with nitrogen in the reaction kettle, repeat the replacement 4 times, and then add Make the pressure of the reaction kettle reach -50KPa, control the temperature of the reaction kettle at 80°C, first put 2.8% ethylene oxide into it, raise the temperature to 90°C, trigger the reaction activation period, and then continue to put 79.2% ethylene oxide into the kettle, During the feeding process, the temperature gradually rises from 90°C to 120°C, and then the temperature of the reactor is controlled to stop rising. The pressure in the reactor should not exceed 350...

Embodiment 3

[0038]Embodiment 3: the first step, prepare materials, pentaerythritol is 16%, potassium hydroxide is 0.5%, ethylene oxide is 83%, and glacial acetic acid is 0.5%, under the condition of 90 ℃ of temperature in reactor, in reactor Vacuumize to -95KPa, put in 0.5% potassium hydroxide, stir, use negative pressure to put 16% pentaerythritol into the kettle, after feeding, pump negative pressure to -95KPa in the reactor, replace with nitrogen gas in the reactor, repeat replacement for 4 Then pressurize to make the pressure of the reactor reach -50KPa, control the temperature of the reactor at 80°C, put in 2.8% ethylene oxide first, raise the temperature to 90°C, trigger the reaction activation period, and then continue to put 80.2% cyclooxygen into the reactor Oxygen, during the feeding process, the temperature gradually rises from 90°C to 120°C, and then the temperature of the reactor is controlled to no longer rise, and the pressure in the reactor cannot exceed 350KPa. After the f...

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Abstract

The invention discloses a method for synthesizing high-molecular-weight pentaerythritol polyoxyethylene ether. The method comprises the following steps: taking pentaerythritol, an alkali metal compound, glacial acetic acid and ethylene oxide as raw materials, and carrying out two-step reaction to prepare the high-molecular-weight pentaerythritol polyoxyethylene ether; the method comprises the steps of feeding, replacing, feeding, curing, neutralizing, discharging and the like. The high-molecular-weight pentaerythritol polyoxyethylene ether can be synthesized; the molecular weight of the pentaerythritol polyoxyethylene ether can reach 7000-10000, an alkali metal compound is adopted as a catalyst, generation of side reactants is reduced, economic benefits are improved, meanwhile, the adoptedraw materials are few in variety, a solvent does not need to be recycled, and production efficiency is improved.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis of new materials, in particular to a synthesis method of high molecular weight pentaerythritol polyoxyethylene ether. Background technique [0002] The existing pentaerythritol polyoxyethylene ethers synthesized by connecting ethylene oxide all have low ethylene oxide numbers, the highest being no more than 100 (the molar ratio of pentaerythritol to ethylene oxide). [0003] At the same time, to synthesize high-molecular-weight pentaerythritol polyoxyethylene ether, only ethylene oxide and PO can be used, and its molecular weight can only reach 4500-7500. There is no single process for purely connecting ethylene oxide to a high molecular weight of 7000-10000. [0004] Synthesis of high-molecular-weight pentaerythritol polyoxyethylene ether usually uses amine catalysts (triethylamine, ammonia water, trimethylamine) at this stage, which is easy to produce by-products and the color of the sy...

Claims

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Application Information

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IPC IPC(8): C08G65/28
CPCC08G65/2609C08G65/2648
Inventor 黎明杰杨礼颖彭延平李玉博
Owner JIAHUA CHEM MAOMING