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Preparation method of polyether

A technology of polyether and ring-opening polymerization, which is applied in the field of polymer synthesis, can solve problems such as complex processes, and achieve the effects of simple post-processing, saving cost and time, and mild reaction conditions

Active Publication Date: 2021-12-10
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the method disclosed in the above content needs to pre-synthesize the low molecular weight polymer, and then use the low molecular weight polymer as the initiator to synthesize the target product, and the process is relatively complicated.

Method used

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  • Preparation method of polyether
  • Preparation method of polyether
  • Preparation method of polyether

Examples

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preparation example Construction

[0049] The raw materials in the preparation method of the polyether that the embodiment of the present invention and comparative examples provide are as follows:

[0050] 1,2-Butylene oxide: purchased from Shanghai Aladdin Biochemical Technology Co., Ltd., CAS No.: 106-88-7, used after refluxing in calcium hydride for 8 hours;

[0051] Tetrahydrofuran: purchased from Shanghai Aladdin Biochemical Technology Co., Ltd., CAS number: 106-88-7, ultra-dry solvent;

[0052] 1,4-Butanediol: purchased from Shanghai Aladdin Biochemical Technology Co., Ltd., CAS No.: 110-63-4;

[0053] Scandium trifluoromethanesulfonate: purchased from Shanghai Aladdin Biochemical Technology Co., Ltd., CAS number: 144026-79-9;

[0054] Yttrium trifluoromethanesulfonate: purchased from Shanghai Aladdin Biochemical Technology Co., Ltd., CAS number: 52093-30-8;

[0055] Lanthanum trifluoromethanesulfonate: purchased from Shanghai Aladdin Biochemical Technology Co., Ltd., CAS number: 52093-26-2;

[0056] C...

Embodiment 1

[0061] The present embodiment provides a kind of preparation method of polyether, concrete steps are as follows:

[0062] Weigh scandium trifluoromethanesulfonate (295mg, 0.60mmol) and add it to a dry three-necked round-bottomed flask. After three vacuum-nitrogen cycles, add 1,4-butanediol (900mg, 10mmol) and tetrahydrofuran under nitrogen protection. (18000mg, 250mmol), after stirring and mixing evenly, at 25°C, add 1,2-epoxybutane (18000mg, 250mmol) dropwise at a rate of 0.05mL / min through a convection pump, and immediately add 3mL water, continue to stir for 1 h, transfer the reaction solution to a 500 mL separating funnel, add 3×50 mL of water for extraction three times, collect the oil phase, and distill off the water under reduced pressure to obtain the polyether (PBT-1).

[0063] The proton nuclear magnetic resonance spectrum figure of described polyether (PBT-1) is as figure 1 As shown, the test instrument is a 600MHz nuclear magnetic resonance spectrometer, and the d...

Embodiment 2

[0066] The present embodiment provides a kind of preparation method of polyether, concrete steps are as follows:

[0067] Weigh scandium trifluoromethanesulfonate (295mg, 0.60mmol) and add it to a dry three-necked round-bottomed flask. After three vacuum-nitrogen cycles, add 1,4-butanediol (1350mg, 15mmol) and tetrahydrofuran under nitrogen protection. (18000mg, 250mmol), after stirring and mixing evenly, at 25°C, add 1,2-epoxybutane (18000mg, 250mmol) dropwise at a rate of 0.05mL / min through a convection pump, and immediately add 3mL water, continue stirring for 1 h, transfer the reaction solution to a 500 mL separatory funnel, add 3×50 mL of water for extraction three times, collect the oil phase, and distill off the water under reduced pressure to obtain the polyether (PBT-2).

[0068] The gel permeation chromatogram of described polyether (PBT-2) is as figure 2 shown.

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Abstract

The invention provides a preparation method of polyether. The preparation method comprises the following steps: mixing a catalyst, dihydric alcohol and C4 alkylene oxide in a protective atmosphere, and then carrying out cationic ring-opening polymerization reaction, and adding a terminator after the reaction to obtain the polyether. According to the preparation method, dihydric alcohol is used as an initiator to initiate C4 alkylene oxide to perform cationic ring-opening polymerization reaction, reaction conditions are mild, post-treatment is simple, controllable polymerization of polyether molecular weight is realized by regulating and controlling the content of the initiator, a target product can be obtained in one step, the reaction efficiency is high, the reaction time is short, the method can be widely applied to preparation of base oil of polyurethane prepolymers, surfactants and lubricants, and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to a preparation method of polyether. Background technique [0002] Aliphatic polyethers are usually formed by ring-opening polymerization of epoxy monomers such as ethylene oxide and propylene oxide. They are a type of highly commercialized and widely used polymers with a large demand for products. The characteristics of polyether materials are due to their unique -C-O-C-main chain, which endows them with high flexibility, and can be used as polyurethane prepolymers, surfactants and lubricating base oils. In addition, polyether products are also widely used Applied in the fields of biomedicine and beauty. [0003] C4 alkylene oxide is a chemical substance with three-membered, four-membered, five-membered ring structure, molecular formula C 4 h 8 O, mainly including 1,2-epoxybutane, 2,3-epoxybutane, 1,4-epoxybutane (tetrahydrofuran), among which 1,2-epoxybut...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28
CPCC08G65/2609C08G65/266C08G65/2654
Inventor 王利国曾宪强李会泉曹妍贺鹏陈家强郑征徐爽
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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