Preparation method for hydroxaminopolyether

A technology of hydroxylamino polyether and chlorinated polyether, which is applied in the field of preparation of large molecular weight hydroxylamino polyether, can solve the problems of low catalyst efficiency, many reaction by-products, strict equipment requirements, etc., so as to overcome the low catalyst efficiency and high Conversion rate, the effect of efficient synthesis

Active Publication Date: 2016-05-25
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Aiming at the problems and shortcomings such as high pressure and harsh equipment requirements in the synthesis process of hydroxylamino polyether in the prior art; low catalyst efficiency and difficult recovery; many reaction by-products and difficult post-processing, the invention provides a simple and easy-to-operate, Synthesis method of hydroxyl amino polyether with mild reaction conditions, low catalyst consumption, high conversion rate, high amine value and no environmental pollution

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  • Preparation method for hydroxaminopolyether
  • Preparation method for hydroxaminopolyether
  • Preparation method for hydroxaminopolyether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Polyether polyol, the synthesis initiator is methanol, the polymerization monomer is ethylene oxide, the degree of polymerization is 11, and the number average molecular weight is 516g / mol. The number of terminal hydroxyl groups of polyether polyol / epichlorohydrin molar ratio is 1:1, the concentration of catalyst DMC is 40ppm, and the cocatalyst Sc(CF 3 SO 3 ) 3 The addition amount is 0.2% of the polyether polyol substance amount. Weigh polyether polyol 1mol (516g), epichlorohydrin 1mol (92.5g), 24mg catalyst DMC, 0.98g promoter Sc (CF 3 SO 3 ) 3. Add the above-mentioned substances into a closed reaction kettle, raise the temperature to 110°C, keep the temperature for 1 hour, remove volatile substances under reduced pressure, and remove insoluble substances by filtration to obtain a chlorinated polyether intermediate.

[0031] The molar ratio of the number of terminal hydroxyl groups of polyether polyol to amination reagent is 1:1, and the amount of reaction solve...

Embodiment 2

[0033] Polyether polyol, the synthetic initiator is methallyl alcohol, the polymerized monomers are ethylene oxide and propylene oxide, the degree of polymerization of ethylene oxide is 10, the degree of polymerization of propylene oxide is 5, the number average The molecular weight is 802.6 g / mol. The number of terminal hydroxyl groups of polyether polyols / epichlorohydrin molar ratio is 1:1, the concentration of catalyst DMC is 40ppm, and the cocatalyst AlCl 3 The addition amount is 0.4% of the polyether polyol substance amount. Weigh 1mol (802.6g) of polyether polyol, 1mol (92.5g) of epichlorohydrin, 36mg catalyst DMC, 0.53g cocatalyst AlCl 3 . Add the above-mentioned substances into a closed reaction kettle, raise the temperature to 110°C, keep the temperature for 1.5 hours, remove volatile substances under reduced pressure, and remove insoluble substances by filtration to obtain a chlorinated polyether intermediate.

[0034] The molar ratio of the number of terminal hyd...

Embodiment 3

[0036] Polyether polyol, the synthetic initiator is 1-stearyl alcohol, the polymerized monomers are propylene oxide and tetrahydrofuran, the degree of polymerization of propylene oxide is 5, the degree of polymerization of tetrahydrofuran is 20, and the number average molecular weight is 2003.2g / mol . The number of terminal hydroxyl groups of polyether polyols / epichlorohydrin molar ratio is 1:2, the concentration of catalyst DMC is 50ppm, and the cocatalyst Sc(CF 3 SO 3 ) 3 The addition amount is 0.3% of the polyether polyol substance amount. Weigh polyether polyol 1mol (2003.2g), epichlorohydrin 2mol (185g), 0.11g catalyst DMC, 1.48g promoter Sc (CF 3 SO 3 ) 3 . Add the above-mentioned substances into a closed reaction kettle, raise the temperature to 130°C, keep the temperature for 4 hours, remove volatile substances under reduced pressure, and remove insoluble substances by filtration to obtain a chlorinated polyether intermediate.

[0037] The number of terminal hyd...

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Abstract

The invention discloses a preparation method for hydroxaminopolyether. The preparation method comprises the steps of adding polyether polyol, a catalyst, a co-catalyst and epoxy chloropropane into a sealed high-pressure reaction kettle according to a ratio, wherein an end group is a chloro-substituted polyether intermediate; and adding a reaction solvent and an amination reagent into the filtered chloro-substituted polyether intermediate, and reacting to prepare a pure hydroxaminopolyether product. According to the preparation method, Lewis acid serves as the co-catalyst for the first time and is applied to a ring-opening polymerization reaction of DMC catalyzed polyether polyol and epoxy chloropropane, so that the shortcomings of low catalyst efficiency, high reaction pressure, strict device requirements and a large amount of byproducts in a conventional method are overcome and the efficient synthesis of chloro-substituted polyether is realized; and in addition, hydroxaminopolyether synthesized by taking sodium amide as the amination reagent has relatively high conversion rate and high amine value.

Description

technical field [0001] The invention belongs to the technical field of macromolecule material synthesis, in particular to a preparation method of a large molecular weight hydroxyl amino polyether. technical background [0002] Amino polyether is a kind of polymer whose main chain is polyether structure and the terminal active functional group is amino group, also known as polyetheramine. By choosing different polyoxyalkylene structures, a series of properties such as reactivity, toughness, viscosity and hydrophilicity of amino polyether can be adjusted, and amino groups provide the possibility of reacting polyetheramine with various compounds. Therefore, amino polyether has been widely used in the fields of polyurea ester, isocyanate crosslinking agent and epoxy resin curing agent. [0003] At present, there are four main methods for synthesizing amino polyethers: catalytic reductive amination, cyanoalkylation, aminobutyryl esterification and leaving group method. [0004]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/338C08G65/325C08G65/337
CPCC08G65/3255C08G65/337C08G65/338C08G2650/10C08G2650/06C08G2650/50
Inventor 亓帅王涛冉千平杨勇马建峰范士敏宋峰岩
Owner JIANGSU SOBUTE NEW MATERIALS
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