Method for synthesizing polyether amine

A synthesis method and polyetheramine technology are applied in the field of obtaining polyetheramine by selective hydrogenation of polyether nitrile, which can solve the problems of reducing brittleness and high toxicity, and achieve the effects of improving conversion rate, improving safety and reducing pressure.

Active Publication Date: 2010-12-22
YUEYANG KIMOUTAIN SCI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The curing agent of polyether amine used in epoxy resin not only reduces the brittleness of the cured product, but also improves the flexibility of the cured product, and overcomes the disadvantage of high toxicity of the simple polyamine curing agent.

Method used

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  • Method for synthesizing polyether amine
  • Method for synthesizing polyether amine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-9

[0028] Add solvent and polyethernitrile into a 2L autoclave, reflux at the reflux temperature of the solvent, reduce the water in the solution to below 20mg / kg, replace the autoclave with nitrogen, and control the temperature of the autoclave at 60-120°C , add the main catalyst dicyclopentadiene titanium dichloride, the first co-catalyst, or the second co-catalyst, feed hydrogen, control the reaction pressure to 0.8-2.0 MPa, and react for 120 minutes to complete the hydrogenation reaction. The experimental results are shown in Table 1:

[0029]

Embodiment 10-13

[0030] Embodiment 10-13: The formula is the same as that of Embodiment 2, but the temperature and pressure are different. The data show that the method of the present invention is obviously superior to the prior art. The data show that the method of the present invention is obviously superior to the prior art.

[0031] Description A: Triisobutylaluminum;

[0032] B: n-butyllithium;

[0033] C: dibutyl magnesium;

[0034] D: n-butyllithium;

[0035] E: methyl benzoate;

[0036]F: Dimethyl phthalate.

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Abstract

The invention relates to a method for synthesizing polyether amine. The method comprises the following steps of: polymerizing epoxy ethane, epoxy propane or mixture thereof into polyether with different molecular weights; reacting the polyether with acrylonitrile under the catalytic action of sodium hydroxide or potassium hydroxide to prepare polycyanoarylether; and selectively hydrogenating carbon-nitrogen double bond in the polycyanoarylether by using a catalyst complex, wherein the catalyst complex is prepared by compounding a titanocene compound serving as a main catalyst, alkyl aluminum, alkyl lithium or an alkyl compound of another alkaline metal and an alkali earth metal serving as a first cocatalyst and a lewis base such as benzoic ether, siloxane and the like serving as a second cocatalyst; 0.05 to 0.2mmol of titanocene compound, 0.1 to 6mmol of alkyl metal compound and 0.01 to 0.4mmol of lewis base are used in every 100g of polymer; the hydrogenation is performed for 0.5 to 2.0 hours at a certain temperature under the hydrogen pressure; the degree of hydrogenation of a nitrile group in the polymer is over 98 percent; and the degree of hydrogenation of an ether bond is less than 1 percent. The method effectively solves the problem of side reaction of ether bond hydrogenation breakage brought by hydrogenating the conventional polycyanoarylether with raney nickel, and the yield of the polyether amine serving as the target product is over 90 percent.

Description

technical field [0001] The invention relates to a synthesis method of polyether amine, more specifically a method for obtaining polyether amine through selective hydrogenation of polyether nitrile. Background technique [0002] Polyetheramine is a tough curing agent for epoxy resin and soft segment component of polyurethane elastomer. Polyetheramine used as a curing agent for epoxy resin not only reduces the brittleness of the cured product, improves the flexibility of the cured product, but also overcomes the disadvantage of high toxicity of the simple polyamine curing agent. Polyether amine reacts with toluene diisocyanate to obtain polyurethane elastomer coatings for corrosion protection of various materials. [0003] The existing synthesis of polyether amine is divided into three steps. First, ethylene oxide, propylene oxide or their mixtures are used to polymerize polyethers of different molecular weights, and then polyether is reacted with acrylonitrile to obtain poly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/333
Inventor 赫炜李洪伟
Owner YUEYANG KIMOUTAIN SCI TECH
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