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Method for preparing amine-terminated polyether by leaving group method

A technology of amino-terminated polyether and leaving group method, which is applied in the field of preparing amino-terminated polyether by leaving group method, and achieves the effects of good reaction selectivity, less by-products and mild reaction conditions

Active Publication Date: 2013-05-08
山西省建筑科学研究院集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned synthesis techniques for preparing amino-terminated polyethers by the above-mentioned leaving group method have disadvantages such as difficult purchase of raw materials, environmental pollution, and many reaction by-products.
In particular, the post-treatment of the aminated product requires the use of a large amount of alkali to neutralize the acid generated by the reaction, resulting in a large amount of inorganic salts. Due to the compatibility between the amino-terminated polyether and the inorganic salts, it is difficult to separate the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0043]Example 1: Add the mixed solution of 48.2g (0.30mol) cyclohexyl chloroformate and 50 gram toluene in the four-necked flask that agitator, nitrogen inlet, thermometer and reflux device are equipped, feed nitrogen, 200.0g (0.10 mol) functionality of 2, polyethylene oxide polyol with a molecular weight of 2000 and 23.7g (0.30mol) pyridine mixed solution was added dropwise, the temperature of the reaction system was controlled not to exceed 20°C, and the reaction solution was heated to 40°C after dropping , reacted for 2 hours, and vacuum filtered to obtain a cyclohexyl carbonate-terminated polyether solution containing toluene; then, drop the cyclohexyl carbonate-terminated polyether into 30 g (0.50 mol) of ethylenediamine, and stir at room temperature for 30 min. Then pass the reaction solution through a molecular still (German UIC KDL5 series) at a distillation temperature of 130 ° C and a pressure of 10 Pa to remove excess ethylenediamine, toluene and cyclohexanol produce...

example 2

[0044] Example 2: Add 39.0g (0.24mol) cyclohexyl chloroformate and 50g xylene in a four-necked flask equipped with stirrer, nitrogen inlet, thermometer and reflux device, feed nitrogen, and 200.0g (0.10 mol) functionality of 2, polyethylene oxide polyol with a molecular weight of 2000 and 19.0g (0.24mol) of pyridine was added dropwise, and the temperature of the reaction system was controlled not to exceed 20°C. After the drop, the reaction solution was heated to 50°C ℃, reacted for 2 hours, and vacuum filtered to obtain a cyclohexyl carbonate-terminated polyether solution containing xylene; then drop the cyclohexyl carbonate-terminated polyether into 22.2g (0.30mol) of 1,3-propylenediamine , and stirred at room temperature for 30 minutes. Then pass the reaction solution through a molecular still (German UIC KDL5 series) at a distillation temperature of 130°C and a pressure of 10 Pa to remove excess 1,3-propylenediamine, toluene and cyclohexanol produced by the reaction to obt...

example 3

[0045] Example 3: Add 48.2g (0.30mol) mixed solution of cyclohexyl chloroformate and 100g diethyl carbonate in a four-necked flask equipped with stirrer, nitrogen inlet, thermometer and reflux device, feed nitrogen into 200.0g (0.067mol) a mixed solution of polypropylene oxide polyol with a functionality of 3 and a molecular weight of 3000 and 30.3g (0.30mol) of triethylamine is added dropwise, and the temperature of the reaction system is controlled not to exceed 20°C. After the drop is completed, the reaction solution is heated to 50°C, react for 2 hours, and vacuum filter to obtain a cyclohexyl carbonate-terminated polyether solution containing diethyl carbonate; then drop the cyclohexyl carbonate-terminated polyether into 27.2g (0.20mol) m-phthalylene In the amine, stir at room temperature for 30 min. Then pass the reaction solution through a molecular still (German UIC KDL5 series) at a distillation temperature of 150 °C and a pressure of 1.0 Pa to remove excess m-xylylen...

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Abstract

The invention relates to a method for for preparing amine-terminated polyether by a leaving group method, including esterification reaction and amination reaction. The method comprises the following steps of: dropping the mixed solution of polyols and a catalyst into the mixed solution of chloro-carbonic ester and solvent, ventilating nitrogen, controlling the temperature of a reaction system not bigger than 20 degrees centigrade, heating the reaction liquid to 20-150 degrees centigrade after dropping, carrying out vacuum filtration after adequate reaction to obtain the solvent-containing carbonate seal end polyether; adding the solvent-containing carbonate seal end polyether into polyamine, stirring the same for 10-120 minutes under normal temperature and pressure, removing excess polyamine, solvent and by-product of mother solution by a molecular still at distillation temperature of 110-170 degrees centigrade and under pressure of 1*10<-2>Pa-200Pa, thereby obtaining the mine-terminated polyether containing carbamate group. The method for preparing amine-terminated polyether by the leaving group method disclosed by the invention has the advantages of mild reaction conditions, low operation cost, no high temperature and pressure and few by-product during the whole process, and is simple in process and by-product is easy remove.

Description

technical field [0001] The invention relates to a preparation method of amino-terminated polyether, specifically, a method for preparing amino-terminated polyether by a leaving group method. Background technique [0002] Amino-terminated polyether is a kind of compound whose main chain contains a polyoxyalkylene structure, and the end of the molecule is capped by a primary or secondary amino group. It is usually obtained by chemically treating the terminal hydroxyl group with the corresponding polyether polyol, also known as polyether amine, polyether polyamine. [0003] Compared with polyether polyols, the reactivity of amino-terminated polyethers and isocyanates has increased by about 3 orders of magnitude, so that the preparation of polyurethane (polyurea) materials can be rapidly molded even without heating and catalyst-free conditions, improving the Production efficiency of polyurethane (polyurea) products. [0004] At the same time, because the polarity of the urea ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/333C08G65/332C07C271/20C07C269/04
Inventor 季宝翟现明郑力菲
Owner 山西省建筑科学研究院集团有限公司
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