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Catalytic system for preparing polyether-containing polymers and preparation method of various polyether-containing polymers

A catalytic system and polymer technology, applied in the field of polymer material synthesis, can solve problems such as low catalytic efficiency and low industrial application value

Active Publication Date: 2018-12-28
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst used is azacarbene, which has little value for industrial application due to its low catalytic efficiency

Method used

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  • Catalytic system for preparing polyether-containing polymers and preparation method of various polyether-containing polymers
  • Catalytic system for preparing polyether-containing polymers and preparation method of various polyether-containing polymers
  • Catalytic system for preparing polyether-containing polymers and preparation method of various polyether-containing polymers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] Example 1 PO homopolymerization

[0071] Before the polymerization reaction, put the 10mL Shrek tube at 110°C for about 2 hours to remove water and cool it to room temperature in a desiccator; add several masses of Lewis base 1 1-tert-butyl-2,2, 4,4,4-Penta(dimethylamino)-2Λ5,4Λ5-di(phosphorus nitrogen compound) (pKa value in acetonitrile is 33.5), methanol and triethylboron; then add 1mL has cooled to - Propylene oxide (PO) at 10°C. The molar ratio of propylene oxide, Lewis base, initiator to triethyl boron is 250 / 1 / 5 / 2. Placed in a low-temperature reactor at -10°C for 0.2h under autogenous pressure. After the reaction was completed, the crude product was first dissolved in tetrahydrofuran, and then the polymer was precipitated in a mixture of 100 mL of methanol / hydrochloric acid (the molar concentration of HCl was 5%), washed three times, and dried in vacuo to constant weight. The molecular weight and molecular weight distribution of the polymer were determined by ...

Embodiment 2

[0073] Example 2 PO homopolymerization

[0074]Before the polymerization reaction, put the 10mL Shrek tube at 110°C for about 2 hours to remove water and cool it to room temperature in a desiccator; add several masses of Lewis base 1 1-tert-butyl-2,2, 4,4,4-Penta(dimethylamino)-2Λ5,4Λ5-di(phosphorus nitrogen), ethanol and triethylboron; then 1 mL of propylene oxide (PO) which had been cooled to 0°C was added. The molar ratio of propylene oxide, Lewis base, initiator to triethylboron is 200 / 1 / 20 / 1.1. Placed in an ice-water bath at 0°C for 2 h under autogenous pressure. After the reaction was completed, the crude product was first dissolved in tetrahydrofuran, and then the polymer was precipitated in 100 mL of methanol / hydrochloric acid mixture (the molar concentration of hydrochloric acid was 5%), washed three times repeatedly, and vacuum-dried to constant weight. The molecular weight and molecular weight distribution of the polymer were determined by gel chromatography, and ...

Embodiment 3

[0075] Example 3 PO homopolymerization

[0076] Before the polymerization reaction, put the 10mL Shrek tube at 110°C for about 2 hours to remove water and cool it to room temperature in a desiccator; add several masses of Lewis base 1 1-tert-butyl-2,2, 4,4,4-Penta(dimethylamino)-2Λ5,4Λ5-dipyrazine, benzyl alcohol and triethylboron and 1 mL THF; then 1 ml propylene oxide (PO) at 25°C was added. The molar ratio of propylene oxide, Lewis base, initiator and triethyl boron is 10000 / 1 / 1 / 10; Placed at 25°C for 12h under autogenous pressure. After the reaction was completed, the crude product was first dissolved in tetrahydrofuran, and then the polymer was precipitated in 100 mL of methanol / hydrochloric acid mixture (the molar concentration of hydrochloric acid was 5%), washed three times repeatedly, and vacuum-dried to constant weight. The molecular weight and molecular weight distribution of the polymer were determined by gel chromatography, and the test results are shown in Tabl...

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Abstract

The invention discloses a catalytic system for preparing polyether-containing polymers and a preparation method of various polyether-containing polymers. The catalytic system comprises an initiator, an organic Lewis base and a Lewis acid; the initiator is selected from a small molecule compound or a polymer compound containing -OH and / or -SH terminal groups, wherein the number of -OH or-SH terminal groups is 1-8; the organic Lewis base is selected from at least one of nitrogen-containing compounds such as phosphazene, guanamine, amidine, imidazole and pyridine, and the PKa value of acetonitrile is 9.6-33.5; and the Lewis acid is selected from a trialkylboron compound. The catalytic system has extremely high catalytic efficiency, is readily commercially available, and avoids the problem ofmetal residue caused by the conventional metal catalytic system. In the presence of the catalytic system, polyether-containing polymers and block copolymers having clear chain structure, controlled molecular weight and narrow distribution, and by-products containing no terminal double bonds can be synthesized by anion ring opening.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis, and in particular relates to a catalytic system for preparing polyether-containing polymers and a preparation method of various polyether-containing polymers. Background technique [0002] Polyether is a widely used chemical raw material. It can be used as an important intermediate in the synthesis of polyurethane (PU), nonionic surfactants and water-based functional liquids. It is widely used in papermaking, textiles, printing and dyeing, synthetic leather, adhesives, etc. , coatings, lubricants, cooling, elastomers, foam products, sealants and petroleum development and other industrial sectors. There are also many applications in high-tech aerospace fields (such as missile propellants). Polyether-containing block copolymers can combine the excellent properties of various polyethers to obtain functional polymer materials with superior performance. For example, polyoxypropylene-b-polyo...

Claims

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Application Information

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IPC IPC(8): C08G65/10C08G65/16C08G64/18
CPCC08G64/183C08G65/10C08G65/16
Inventor 张兴宏张成建
Owner ZHEJIANG UNIV
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