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Polyether amine and preparation method thereof

A polyetheramine and polymer technology, applied in the field of polymer material synthesis and preparation, can solve the problems of strict process requirements, high yield and high cost, and achieve the effects of reducing side reactions, reducing costs and avoiding strict requirements.

Inactive Publication Date: 2013-06-05
FUZHOU BAISHENG FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

US005510535A discloses a method for synthesizing amino-terminated polyether, which is prepared by amine initiators and alkylene oxide compounds under double metal cyanide catalyzed conditions. The yield is high, but the process requirements are strict and the pollution is large. high cost

Method used

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  • Polyether amine and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] (1) In a three-necked flask, dissolve triethylenetetramine and acetone in toluene at a molar ratio of 1:2.5, control the reaction temperature at 90-130°C, react for 6-10 hours, separate the liquid and produce water, and the conversion rate is 95%; Remove toluene, water and excess acetone in the system to obtain triethylenetetramine protected by ketimine;

[0028] (2) Add triethylenetetramine (2mol) and sodium ethoxide (0.3wt%) protected by ketimine into the polymerization reactor, pass through argon protection, add propylene oxide (50mol) dropwise to react, and control the pressure to 0.1~10MPa, after the feeding is completed, continue to react for 5h to obtain polyetheramine protected by ketimine; then add phosphoric acid (0.4mol), deionized water (30mol) and adsorbent (5wt%), at 60~150℃ Hydrolyze for 1 hour to remove the ketimine protecting group, then remove the acetone in the system at a temperature range of 50-130°C, and finally filter to obtain the polyetheramine ...

Embodiment 2

[0030] (1) In a three-necked flask, dissolve tetraethylenepentamine and butyraldehyde in toluene at a molar ratio of 1:3, control the reaction temperature at 90-130°C, react for 5-9 hours, separate the liquid and effluent, and the conversion rate is 93% ; Remove toluene, water and excessive butyraldehyde in the system to obtain the tetraethylenepentamine of aldimine protection;

[0031] (2) Add aldimine-protected tetraethylenepentamine (1mol) and potassium oxide (0.3wt%) into the polymerization reactor, pass through argon protection, add dropwise ethylene oxide (20mol), and control the pressure to 0.1 ~10MPa, after the addition, continue to react for 5h to obtain aldimine-protected polyetheramine; then add oxalic acid (0.5mol), deionized water (35mol) and adsorbent (5wt%), hydrolyze at 60~150℃ Remove the aldimine protecting group for 1 hour, then remove butyraldehyde in the system at a temperature range of 50-130°C, and filter to obtain the polyetheramine product.

Embodiment 3

[0033] (1) In a three-necked flask, dissolve N-aminoethylpiperazine and acetone in toluene at a molar ratio of 1:4, control the reaction temperature at 60-100°C, react for 5-8 hours, and separate the liquid to produce water; remove the system Toluene in, water and excess acetone, obtain the aminoethylpiperazine of ketimine protection;

[0034] (2) Add ketimine-protected aminoethylpiperazine (1mol) and sodium methoxide (0.5wt%) into the polymerization reactor, pass through argon protection, add dropwise butylene oxide (40mol), and control the pressure to 0.1~10MPa, after the feeding is completed, continue to react for 5h to obtain polyetheramine protected by ketimine; then add oxalic acid (0.5mol), deionized water (40mol) and adsorbent (8wt%), at 60~150℃ Hydrolyze for 1 hour to remove the ketimine protecting group, then remove the acetone in the system at a temperature range of 50-130°C, and filter to obtain the polyetheramine product.

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Abstract

The invention discloses a polyether amine and a preparation method thereof, and belongs to the technical field of high polymer material synthesis and preparation. According to the polyether amine and the preparation method thereof, a ketone, an aldehyde or an acid anhydride is reacted with primary amine for the first time to generate ketimine, aldimine or acyl protected amine compounds, and secondary amine or active hydroxyl and an alkylene oxide monomer are subjected to anionic polymerization so as to successfully synthesize polyether amine containing primary amine. The defects that the conventional method, namely, direct hydroxyl amination, requires harsh conditions of the equipment and the process, and side reaction is likely to happen when the amine compound is bonded with a polyether chain, are overcome, and polyether amine which is moderate in reaction condition and tidy in structure is successfully synthesized. The polyether amine has potential application in the fields of machine manufacturing, electrical equipment and electronic devices, communication and transportation, petrochemical engineering, national defense construction, electrophoretic paint, anticorrosive paint and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis and preparation, and specifically relates to a polyetheramine and a preparation method thereof. Background technique [0002] Polyether amine is a kind of tough curing agent for epoxy resin and the main raw material for preparing polyurethane urea and polyurea materials. When polyetheramine is used as a curing agent for epoxy resin, it not only reduces the brittleness of the cured product, improves the flexibility and thermomechanical properties of the cured product, but also overcomes the volatile nature of small molecular polyamine compounds, the tendency to absorb water in the air and Disadvantages of carbon dioxide and high toxicity. And it is used to prepare polyurethane urea and polyurea materials, which can greatly improve the reaction rate and the physical properties of the materials. [0003] At present, there are three main structures of polyether amines: (1) linear ...

Claims

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Application Information

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IPC IPC(8): C08G65/32C08G65/26
Inventor 石孟泽王贵友蒋冠兰高孝贵林荣乐
Owner FUZHOU BAISHENG FINE CHEM
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