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A method for preparing homogeneous-distribution polyethylene glycol by utilizing a microchannel reactor

A micro-channel reactor and polyethylene glycol technology, which is applied in the field of preparing single-distribution polyethylene glycol using micro-channel reactors, can solve problems such as single-distribution polyethylene glycol, which has not yet been seen, and achieves increased process safety and mixing. The effect of high efficiency and narrow polydispersity coefficient

Active Publication Date: 2019-03-29
南京威尔药业科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned patents all focus on realizing the continuous production of ethylene oxide polymerization and subsequent production, reducing the generation of by-products, and improving reaction efficiency. So far, there has been no related work on the preparation of single-distribution polyethylene glycol by microchannel reactors. Research

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A method utilizing a microchannel reactor to prepare monopolyethylene glycol, comprising the following steps:

[0022] Add sodium hydroxide to diethylene glycol to prepare a 1% diethylene glycol solution, and pump it into the pre-mixer at 2.0 mL / min and ethylene oxide at 20.0 mL / min at the same time, and control The temperature of the premixed system is 0°C, the pressure is 0.5MPa, and the mixing time is 100ms. Then, the premixed reaction solution is passed into the microchannel reactor, and reacted at 130°C, 2.5 MPa, and the residence time is 4 minutes. Receive the product at 50°C, add purified water to dissolve, pass through the ion exchange resin column, the flow rate is 0.8 mL / s, after filtration, vacuum dehydration, temperature 105°C, dehydration for 4 hours, after dehydration, cool down to room temperature , to obtain the polyethylene glycol product, the yield is 96.7%, its molecular weight is 910, and the molecular weight distribution is 1.0010.

Embodiment 2

[0024] Add potassium hydroxide to ethylene glycol to prepare a 3% ethylene glycol solution, and pump it into the pre-mixer at the same time at 0.4 mL / min and 8.4 mL / min with the injection pump to control the pre-mixing The temperature of the system is 10°C, the pressure is 1.0MPa, and the mixing time is 250ms. Then, the pre-mixed reaction solution is passed into the microchannel reactor, reacted at 170°C, 3.0 Mpa, and the residence time is 10min, and the product is received under nitrogen protection. , after returning to 80°C, add purified water to dissolve, pass through the ion exchange resin column, flow rate 0.4 mL / s, after filtration, vacuum dehydration, temperature 100°C, dehydration for 4 hours, after dehydration, lower to room temperature to obtain poly Ethylene glycol product, yield is 94.1%, and its molecular weight is 991, and molecular weight distribution is 1.0030.

Embodiment 3

[0026] Add potassium methoxide to triethylene glycol to prepare a 5% triethylene glycol solution, and pump it into the pre-mixer at the same time at 0.5 mL / min and 3.9 mL / min of ethylene oxide to control the pre-mixing system The temperature is 5°C, the pressure is 0.7MPa, and the mixing time is 500ms. Then, the pre-mixed reaction solution is passed into the microchannel reactor, reacted at 100°C, 4.5 MPa, and the residence time is 20min, and the product is received under nitrogen protection. After returning to 65°C, add purified water to dissolve, pass through an ion exchange resin column at a flow rate of 1.0 mL / s, filter, and vacuum dehydrate at a temperature of 110°C for 4 hours. After dehydration, cool down to room temperature to obtain polyethylene Diol product, yield is 95.2%, and its molecular weight is 1008, and molecular weight distribution is 1.0040.

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Abstract

A method for preparing homogeneous-distribution polyethylene glycol by utilizing a microchannel reactor is disclosed. The method includes (1) a step of preparing a catalytic system, namely a step of subjecting polyol as an initiator and an alkali metal catalyst as a raw material to ultrasonic vibration dissolving; (2) a step of raw material premixing, namely a step of feeding the catalytic systemand epoxy ethane into a premixer at the same time, and premixing the materials at 0-10 DEG C under 0.5-1.0 MPa for 50-500 ms; (3) a micro reaction step, namely a step of subjecting the premixed raw materials to continuous polymerization through the microchannel reactor to obtain a reaction solution, with the reaction temperature being controlled to be 100-200 DEG C, residence time being 2 to 20 min, the reaction pressure being 1.0 to 4.5 MPa; and (4) a step of aftertreatment, namely a step of adding purified water for dissolution at 50-80 DEG C, allowing the solution to pass through an ion exchange resin column, performing filtration and then vacuum dehydration, and cooling a product to room temperature to obtain a polyethylene glycol product. The reaction efficiency is greatly improved, which is very favorable for reducing the price of the homogeneous-distribution polyethylene glycol. The microchannel reactor has no scale effect and is very suitable for industrial scale production.

Description

technical field [0001] The invention relates to a method for preparing mono-distribution polyethylene glycol, in particular to a method for preparing mono-distribution polyethylene glycol using a microchannel reactor. Background technique [0002] Polyethylene glycol is a water-soluble polymer. There are a series of polymer compounds from low to high molecular weight, which are polymerized from ethylene oxide or ethylene glycol. Polyethylene glycol with a molecular weight in the range of several hundred to tens of thousands is produced by gradual addition polymerization, and polyethylene glycol with a molecular weight of more than tens of thousands or even millions is produced by heterogeneously catalyzed ring-opening polymerization of ethylene oxide. The latter is known in the industry as "polyethylene oxide". Polyethylene glycol is completely soluble in water regardless of its molecular weight, and has good compatibility with many organic solvents, good stability and lubr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28
CPCC08G65/2609C08G65/2648C08G65/2696
Inventor 李欢徐扬朱兵王保成高正松
Owner 南京威尔药业科技有限公司
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