A kind of method utilizing microchannel reactor to prepare polyether polyol

A technology of microchannel reactor and polyether polyol, which is applied in the field of polyether preparation, can solve the problems of uncertainty and complexity of the reaction situation, and achieve the effects of rapid interfacial transfer, lower reaction temperature and higher production capacity

Active Publication Date: 2019-05-03
HONGBAOLI GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the polymerization reaction, due to the uncertainty and complexity of the reaction situation, the use of microchannel reactors still needs further research.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Synthesis of initiator A-1:

[0034] Add 304g of propylene glycol and 4.8g of potassium hydroxide to a 2L reactor, replace with nitrogen twice, raise the temperature to 60-70°C, evacuate to -0.093MPa, keep it for 0.5h, stop vacuuming, raise the temperature to 110-120°C, and continue Add 1300.0g propylene oxide, control the reaction pressure not to exceed 0.30MPa, after the propylene oxide is passed through, keep warm at 120°C until the pressure drop remains unchanged, then vacuumize to -0.093MPa, keep it for 0.5h, and pass nitrogen to normal pressure; Lower the temperature to 60-80°C, add 50g of deionized water, stir for 1h, then add 16.4g of phosphoric acid (50% concentration), stir for 1h, finally add 4.9g of magnesium silicate, stir for 1h, then raise the temperature to 100-120°C, The moisture in the material was removed by vacuum, and filtered under reduced pressure to obtain 1570.0 g of polyether polyol A-1 with a number average molecular weight of 400.

[0035] I...

Embodiment 2

[0039] Add initiator A-1, catalyst double metal cyanide Zn in embodiment 1 in the airtight container with stirring 3 [Co(CN) 6 ] 2 ·ZnNO 3 2H 2 O·C 3 h 8 o 2 20ppm, start stirring, raise the temperature to 125°C, and vacuumize for 1.5 hours to obtain the mixed material B-2, which is stored in a closed material tank; the material B-2 and propylene oxide are injected into the micro In a channel reactor, the molar ratio of material B-2 to propylene oxide is 1:20.7, the temperature in the microchannel reactor is 100°C, the pressure is 0.015MPa, the material stays for 195s, and the material flows out continuously from the reactor outlet to the receiving tank to obtain crude Polyether polyol E-2, the crude polyether polyol enters the stripping tower to remove small molecules to obtain the polyether polyol product F-2.

[0040] Indicators: Appearance: colorless transparent liquid, hydroxyl value: 56.1mgKOH / g, unsaturation 0.0005mmol / g, molecular weight distribution coefficient...

Embodiment 3

[0042] Add initiator A-1, catalyst double metal cyanide Zn in embodiment 1 in the airtight container with stirring 3 [Co(CN) 6 ] 2 ·ZnNO 3 2H 2 O·C 3 h 8 o 2 15ppm, start stirring, heat up to 130°C, and vacuumize for 1.5 hours to obtain material B-3, which is stored in a closed material tank; material B-3 and butylene oxide are injected into the microchannel at the same time with a metering pump In the reactor, the molar ratio of material B-3 to butylene oxide is 1:8.57, the temperature in the microchannel reactor is 115°C, the pressure is 0.02MPa, the material stays for 405s, and the material continuously flows out from the reactor outlet to the receiving tank to obtain crude polymer Ether polyol E-3, the crude polyether polyol enters the stripping tower to remove small molecules to obtain the polyether polyol product F-3.

[0043] Indicators: Appearance: colorless transparent liquid, hydroxyl value: 112.1mgKOH / g, degree of unsaturation 0.0013mmol / g, molecular weight d...

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Abstract

The invention discloses a method of using a microchannel reactor to prepare polyether glycol. Active hydrides are used as the initiator. Alkene oxide is used as the raw material. Bi-metal cyanide is used as the catalyst. The synthesis reaction process of the polyether glycol with the number-average molecular weight of 700-1000 is completed in the micro-channel reactor. The polyether glycol product prepared by using the method has a relatively narrow distribution of molecular weights, the degree of unsaturation of the product is low, and no tailing peak is generated.

Description

technical field [0001] The invention belongs to the field of polyether preparation methods, and in particular relates to a method for preparing polyether polyols by using a microchannel reactor. Background technique [0002] Polyether polyol is an important raw material in the production of polyurethane. It is generally composed of an initiator containing polyhydric alcohol and epoxides such as ethylene oxide, propylene oxide, and butylene oxide through addition polymerization in the presence of a basic catalyst. be made of. Basic catalysts generally use potassium hydroxide, sodium hydroxide, etc. This type of catalyst mainly catalyzes the ring opening of epoxy olefin anions. The disadvantage is that it is easy to form unsaturated bonds in the process of preparing polyether polyols with a number average molecular weight greater than 1000. The presence of these unsaturated bonds reduces the functionality of polyether polyols, which adversely affects the hardness and mechanic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/28C08G65/30
CPCC08G65/2609C08G65/2663C08G65/30
Inventor 黄东平邢益辉刘新迁芮辉辉赵德喜
Owner HONGBAOLI GRP CO LTD
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