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Water-soluble cationic polyaspartic ester, preparation method and application thereof

A technology of aspartic acid ester and water-soluble cation, which is applied in polyurea/polyurethane coatings, coatings, organic chemistry, etc., can solve the problems that it is difficult to meet the various needs of water-based polyurea, achieve good stability, and improve mechanical properties. The effect of intensity

Active Publication Date: 2018-12-18
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] To sum up, waterborne polyurea currently relies on external water-soluble monomers to introduce hydrophilic groups, which is difficult to meet the diverse needs of waterborne polyurea and polyurea / polyurethane coating resin downstream applications

Method used

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  • Water-soluble cationic polyaspartic ester, preparation method and application thereof
  • Water-soluble cationic polyaspartic ester, preparation method and application thereof
  • Water-soluble cationic polyaspartic ester, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Add 103.17g (1mol) of diethylenetriamine into a 1L four-neck round bottom flask equipped with a mechanical stirring paddle, a thermometer, a constant pressure dropping funnel, and a N 2 Air line pipe, bubbler, add 344.36g (2mol) diethyl maleate into the constant pressure dropping funnel, pass N into the system 2 For 10 minutes, replace the air in the system; slowly drop diethyl maleate into the flask with stirring at 25°C, drop it at a constant speed for 1 hour, control the reaction temperature to 30°C, then raise the temperature to 60°C for 3 hours, and stop the reaction.

[0044] Add 380g of distilled water to the above system, increase the stirring speed to 800rpm, emulsify the system, then reduce the speed to 400rpm, add 92.52g (1mol) epichlorohydrin into the constant pressure dropping funnel, slowly drop into the emulsion, 1h After dripping, the temperature was raised to 50°C to keep the temperature for reaction. After 50 minutes of reaction, the emulsion became c...

Embodiment 2

[0051] Add 103.17g (1mol) of diethylenetriamine into a 1L four-neck round bottom flask equipped with a mechanical stirring paddle, a thermometer, a constant pressure dropping funnel, and a N 2 Air line pipe, bubbler, add 344.36g (2mol) diethyl fumarate into the constant pressure dropping funnel, pass N into the system 2 For 30 minutes, replace the air in the system; slowly drop diethyl maleate into the flask under stirring at 25°C, drop it at a constant speed for 1 hour, control the reaction temperature to 30°C, then raise the temperature to 50°C for 6 hours, and stop the reaction.

[0052] Add 380g of distilled water to the above system, raise the stirring speed to 800rpm, emulsify the system, then reduce the speed to 400rpm, add 92.52g (1mol) epichlorohydrin in the constant pressure dropping funnel, slowly drop into the emulsion, 1.5 After dropping for h, the temperature was raised to 55°C and the temperature was kept for reaction. After 55 minutes of reaction time, the emu...

Embodiment 3

[0059] Add 116.99g (0.8mol) of triethylenetetramine into a 1L four-neck round bottom flask equipped with a mechanical stirring paddle, a thermometer, a constant pressure dropping funnel, and a N 2 Air pipe, bubbler, 275.49g (1.6mol) diethyl maleate was added to the constant pressure dropping funnel, and N was introduced into the system. 2 20min, replace the air in the system; slowly drop diethyl maleate into the flask under the condition of stirring at 25°C, drop it at a constant speed for 0.5h, control the reaction temperature at about 30°C, then raise the temperature to 40°C for 5h, stop the reaction .

[0060] Add 785g of distilled water to the above system, raise the stirring speed to 800rpm, emulsify the system, then reduce the speed to 400rpm, add 148.04g (1.6mol) epichlorohydrin into the constant pressure dropping funnel, slowly drop into the emulsion, After 1.5 hours of dripping, the temperature was raised to 55°C and the temperature was kept for reaction. After 50 m...

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Abstract

The invention provides a water-soluble cationic polyaspartic ester and a synthesis method thereof. The substance has a 3-hydroxyazetidine structure. During synthesis, firstly butene diacid diester reacts with polyethylene polyamine to obtain polyaspartic ester polyamine with unreacted secondary amine group, and then adding epoxy chloropropane for reaction with the secondary amine group so as to obtain water-soluble polyaspartic ester with azetidine cationic group. The cationic polyaspartic ester monomer can be compounded with isocyanate to develop water-soluble polyurea or polyurea / polyurethane coating resin.

Description

technical field [0001] The invention belongs to the field of polyaspartic acid ester synthesis, and in particular relates to a water-soluble cationic polyaspartic acid ester and its preparation method and application. Background technique [0002] Polyaspartic Ester (Polyaspartic Ester, PAE), as a special kind of sterically hindered secondary amine, due to the steric hindrance and inductive effect of the ester group, reduces the activity of the secondary amine when it reacts with NCO, thus overcoming the traditional polyaspartic acid. The disadvantages of urea materials are short construction time, poor coating adhesion and many surface defects. [0003] At present, most of the commercially available PAE products are difunctional oil-soluble PAE products, which are used to prepare oil-soluble high-solid polyaspartate polyurea coatings. Chinese patent CN1952029 reports a method for preparing amino-terminated polyether-type polyaspartic acid ester using a two-step method. Li...

Claims

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Application Information

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IPC IPC(8): C07D205/04C09D175/02C09D175/04
CPCC07D205/04C09D175/02C09D175/04
Inventor 郑超何光文崔乾王鹏从鑫董科黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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