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Method for preparing polyether based on three-component metal-free catalytic initiation system

A technology of metal-free catalysis and initiation system, applied in the field of polyether synthesis, can solve the problems of low catalytic activity, ineffectiveness, destructive side reactions of polymerization efficiency, etc., and achieve the effect of narrow dispersion and adjustable molecular structure.

Inactive Publication Date: 2019-03-26
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the ring-opening polymerization of epoxy relies only on the activation of the initiator or the terminal hydroxyl group of the growing chain, the polymerization efficiency and selectivity / controllability are contradictory, that is, the improvement of polymerization efficiency is often accompanied by the occurrence of destructive side reactions or an increase in the degree
Relatively mild organic bases have better catalytic efficiency and selectivity for partial ring-opening polymerization, but for the ring-opening polymerization of epoxy monomers, there are problems of low catalytic activity or even complete ineffectiveness.

Method used

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  • Method for preparing polyether based on three-component metal-free catalytic initiation system
  • Method for preparing polyether based on three-component metal-free catalytic initiation system
  • Method for preparing polyether based on three-component metal-free catalytic initiation system

Examples

Experimental program
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Effect test

Embodiment 1

[0040] The ring-opening polymerization of ethylene oxide is carried out with water as the initiator and organic Lewis acid-base couple as the catalyst to prepare polyethylene oxide glycol. The specific operation is as follows.

[0041] In an inert atmosphere, add 1 part (mole part) of purified water into a dry glass reactor. Continue to add phosphazene base t-BuP containing 0.01 parts 1 With 0.03 parts of triisopropylborane in tetrahydrofuran solution, stir and mix evenly. Connect the glass reactor to a vacuum line, remove part of the gas in the bottle, and cool down with an ice-water bath. Add 2400 parts of dry ethylene oxide at 0-4°C, seal the glass reactor and react at room temperature (20-25°C) for 24h. In this embodiment, the molar concentration of ethylene oxide is 20 mol / L, and after the ethylene oxide reaction is completed, it can be seen that a solid product is precipitated in the glass reactor. The reactor is opened, and the polyethylene oxide product is collecte...

Embodiment 2

[0044] The ring-opening polymerization of ethylene oxide was carried out with water as the initiator and organic Lewis acid-base couple as the catalyst to prepare non-cytotoxic polyethylene oxide diol. The specific operation is as follows.

[0045] Both tetrahydrofuran (THF) and ethylene oxide were used after water removal treatment. In an inert atmosphere, add 1 part of pure water to a dry glass reactor and add THF to dissolve. Continue to add t-BuP containing 0.1 part of phosphazene base 1 With 0.3 parts of tetrahydrofuran solution of triethylboron, stir and mix evenly. Connect the glass reactor to a vacuum line, remove part of the gas in the bottle, and cool down with an ice-water bath. Add 240 parts of dry ethylene oxide at 0-4°C, seal the glass reactor and react at room temperature for 3h. In this embodiment, the molar concentration of ethylene oxide is 12 mol / L. After the reaction is completed, the reactor is opened, and the polyethylene oxide product is taken out fr...

Embodiment 3

[0048] The ring-opening polymerization of ethylene oxide is carried out with water as initiator and organic Lewis acid-base couple as catalyst to prepare high molecular weight polyethylene oxide glycol. The specific operation is as follows.

[0049] In an inert atmosphere, add 1 part of pure water to a dry glass reactor and add THF to dissolve. Continue to add t-BuP containing 5 parts of phosphazene base 1 With 15 parts of tetrahydrofuran solution of triethylboron, stir and mix evenly. Connect the glass reactor to a vacuum line, remove part of the gas in the bottle, and cool down with an ice-water bath. Add 24,000 parts of dry ethylene oxide at 0-4°C, and react in a sealed glass reactor for 3 hours at room temperature. After the reaction is completed, the reactor is opened, and the polyethylene oxide product is taken out from the reaction bottle and vacuum-dried to obtain the product. The theoretical number average molecular weight M calculated by the ratio of ethylene oxi...

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Abstract

The invention discloses a method for preparing polyether based on a three-component metal-free catalytic initiation system. The method comprises the steps of adding an epoxy monomer into a three-component metal-free catalytic initiation system containing hydroxy compounds, organic alkali and boron alkyl to react to obtain the polyether. The method is a currently known ethylene oxide room-temperature open-ring polymerization method with highest catalytic activity since the usage of organic alkali can be reduced to 40ppm and the conversion frequency can be 6000h / l. The polyether has the advantages of no metal residue and no cytotoxicity. The three-component catalytic initiation system adopts ethylene oxide open-ring polymerization, the chain transfer reaction toward the monomer and solvent can be completely avoided while the conversion frequency of 2720h / l can be obtained, and the polyether has the molecular weight of 0.1-400kg / mol, which can be accurately controlled. Furthermore, by utilizing the catalytic initiation system, the (poly) block polyether with controllable molecular weight, block sequence, block proportion and side base combination can be conveniently prepared by continuously adding materials.

Description

technical field [0001] The invention belongs to the field of polyether synthesis, and in particular relates to a method for preparing polyether based on a three-component metal-free catalytic initiation system. Background technique [0002] Polyether is a polymer whose main chain structure is mainly composed of ether bonds (-R-O-R-), and is the most widely used synthetic base oil with the largest market demand. Aliphatic polyethers are mainly prepared from epoxy compounds such as ethylene oxide, propylene oxide, and butylene oxide through ring-opening polymerization or copolymerization. Polyethylene oxide (also known as polyethylene glycol) has many advantages such as water solubility, biocompatibility, and lubricity, and has a wide range of applications in metal processing, spinning and papermaking, biomedicine, and even energy materials. Polypropylene oxide (also known as polypropylene glycol) is widely used in the production of polyurethane foam, and is also used as a pl...

Claims

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Application Information

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IPC IPC(8): C08G65/28
CPCC08G65/2609C08G65/2672C08G65/2687
Inventor 赵俊鹏陈烨张广照
Owner SOUTH CHINA UNIV OF TECH
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