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Sulfoacid/carboxylic acid type hydrophilic chain extender and preparation method thereof

A technology of hydrophilic chain extender and carboxylic acid type, which is applied in the field of water-based polyurethane hydrophilic chain extender and its preparation, can solve the problems of few types and single performance, and achieve cheap price, easy raw materials and simple process route Effect

Inactive Publication Date: 2012-07-25
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the problem that there are few types and single performance of the current water-based polyurethane hydrophilic chain extender, the present invention provides a sulfonic acid / carboxylic acid type hydrophilic chain extender and a preparation method thereof

Method used

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  • Sulfoacid/carboxylic acid type hydrophilic chain extender and preparation method thereof
  • Sulfoacid/carboxylic acid type hydrophilic chain extender and preparation method thereof
  • Sulfoacid/carboxylic acid type hydrophilic chain extender and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0022] 1) Amidation reaction:

[0023] see figure 1 99 parts by mass of maleic anhydride are dissolved in 45 parts of acetone to make solvent A, 107 parts by mass of diethanolamine are dissolved in 40 parts of acetone to make solution B, and the solution A is added to the reactor with nitrogen protection, reflux condenser, stirrer, and dropping funnel, and 0.5 parts of catalyst N,N-lutidine is added to the reactor, and the reaction temperature is controlled at 50°C , slowly add solution B into the reactor, fully react under stirring, then distill off the solvent under reduced pressure to obtain a white powder, then recrystallize with ethanol, then filter and dry the crystal to obtain a white powder, the white powder is Amidation intermediate for the reaction of sulfonic acid / carboxylic acid type hydrophilic chain extender;

[0024] 2) Sulfonation reaction:

[0025] see figure 2 , take 100 parts of white powder amidation reaction intermediate and 62 parts of sulfonating ag...

Embodiment 2

[0030] 1) Amidation reaction:

[0031] Get 99 parts by mass of maleic anhydride and dissolve in 50 parts of butanone to make solvent A, get 134 parts by mass of diisopropanolamine and dissolve in 45 parts of butanone to make a solution B. Add solution A to the reactor with nitrogen protection, reflux condenser, stirrer, and dropping funnel, control the reaction temperature at 60°C, slowly add solution B to the reactor, and stir it moderately After sufficient reaction under reduced pressure, the solvent was distilled off to obtain a white powder, which was recrystallized with ethanol, and then the crystal was filtered and dried to obtain a white powder, which was the reaction of sulfonic acid / carboxylic acid type hydrophilic chain extender. amidation intermediates;

[0032] 2) Sulfonation reaction:

[0033] Take 100 parts of white powder amidation reaction intermediate and 45 parts of sulfonating agent sodium bisulfite dissolved in water, add to the reactor, stir well, raise ...

Embodiment 3

[0035] 1) Amidation reaction:

[0036] Get 99 parts by mass of maleic anhydride and dissolve in 190 parts of chloroform to make solvent A, get 107 parts by mass of diethanolamine and dissolve in 180 parts of chloroform to make solution B, and dissolve solution A Add to the reactor with nitrogen protection, reflux condenser, stirrer, dropping funnel, and add 0.5 parts of catalyst N, N-lutidine to the reactor, the reaction temperature is controlled at 80 °C, Slowly add solution B into the reactor, fully react under moderate stirring, and then distill off the solvent under reduced pressure to obtain a white powder, then recrystallize with ethanol, then filter and dry the crystal to obtain a white powder, the white powder is Amidation intermediate for the reaction of sulfonic acid / carboxylic acid type hydrophilic chain extender;

[0037] 2) Sulfonation reaction:

[0038] Take 100 parts of white powder amidation reaction intermediate and 45 parts of sulfonating agent sodium bisul...

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Abstract

The invention discloses a sulfoacid / carboxylic acid type hydrophilic chain extender and a preparation method of the sulfoacid / carboxylic acid type hydrophilic chain extender. The preparation method comprises the following steps: dissolving maleic anhydride, diethanol amine or diisopropanolamine in a solvent, respectively; adding maleic anhydride solution into a reactor and slowly adding diethanol amine or diisopropanolamine solution to perform amidation reaction after the rise of the temperature; removing the solvent by means of reduced-pressure distillation after the mixture is fully reacted to obtain white powder; recrystallizing the white powder by using ethanol; filtering and drying a crystalline substance to obtain white powder which is an amidated reaction intermediate of the sulfoacid / carboxylic acid type hydrophilic chain extender; dissolving the white powder intermediate obtained by the amidation reaction and a sulfonating agent, adding the mixture into the reactor for fully stirring; performing sulfonation reaction at a risen temperature, reducing the temperature until the mixture is reacted fully; filtering and drying the solution to obtain white powder, i.e. the sulfoacid / carboxylic acid type hydrophilic chain extender.A molecular chain of the hydrophilic chain extender prepared by the method contains a sulfonic acid group and a carboxylic acid group.

Description

technical field [0001] The invention relates to a water-based polyurethane hydrophilic chain extender and a preparation method thereof, in particular to a hydrophilic chain extender containing sulfonic acid / carboxylic acid groups and a preparation method thereof. Background technique [0002] Water-based chain extender is one of the important raw materials for synthesizing water-based polyurethane resin. It can introduce hydrophilic groups into the molecular chain of polyurethane resin, so that water-based polyurethane has certain hydrophilicity and self-emulsification. At present, the hydrophilic groups that can be introduced into waterborne polyurethane resins mainly include anionic carboxylic acid groups and sulfonic acid groups, cationic tertiary amino groups, and nonionic ethoxy groups. At present, the most widely used water-based polyurethane resin is an anionic (carboxylic acid or sulfonic acid) hydrophilic group, which has been used in the processing field as water-b...

Claims

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Application Information

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IPC IPC(8): C08G18/32C07C309/17C07C303/32
Inventor 王学川张哲强涛涛
Owner SHAANXI UNIV OF SCI & TECH
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