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 occu

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
Comparison scheme
Effect test

Example Embodiment

[0039] Example 1

[0040] Using water as an initiator and an organic Lewis acid-base pair as a catalyst, ring-opening polymerization of ethylene oxide is carried out to prepare polyethylene oxide glycol. The specific operation is as follows.

[0041] In an inert atmosphere, 1 part (molar part) of purified water is added to the dry glass reactor. Continue to add 0.01 parts of phosphazene base t-BuP 1 Stir and mix with 0.03 parts of triisopropylborane in tetrahydrofuran. Connect the glass reactor to the 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. After the ethylene oxide reaction is completed, it can be seen that solid products are deposited in the glass reactor. The reactor is opened, the polyethylene oxide product is collected and vacuum-dried...

Example Embodiment

[0043] Example 2

[0044] Using water as an initiator and an organic Lewis acid-base pair as a catalyst, the ring-opening polymerization of ethylene oxide is carried out to prepare non-cytotoxic polyethylene oxide glycol. The specific operation is as follows.

[0045] Tetrahydrofuran (THF) and ethylene oxide are used after dewatering. In an inert atmosphere, add 1 part of purified water to a dry glass reactor and add tetrahydrofuran to dissolve. Continue to add t-BuP containing 0.1 part of phosphazene base 1 Stir and mix with 0.3 parts of triethyl boron in tetrahydrofuran solution. Connect the glass reactor to the 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, and react in a sealed glass reactor at room temperature for 3 hours. 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 ...

Example Embodiment

[0047] Example 3

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

[0049] In an inert atmosphere, add 1 part of purified water to a dry glass reactor and add tetrahydrofuran to dissolve. Continue to add t-BuP containing 5 parts of phosphazene base 1 Stir and mix with 15 parts of triethyl boron in tetrahydrofuran solution. Connect the glass reactor to the 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 3h at room temperature. After the reaction is completed, the reactor is opened, and the polyethylene oxide product is taken out from the reaction flask and dried under vacuum to obtain it. The theoretical number average molecular weight M calculated by th...

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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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