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Synthesis method of amino-terminated polyolefin

A synthesis method and terminal amination technology, applied in the field of synthesis of terminal amination polyolefin, can solve the problems of high cost of reagents, cumbersome synthesis route, etc., and achieve the effects of simple method, low cost, and promotion of high value-added recovery

Inactive Publication Date: 2021-08-24
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing synthetic routes are cumbersome, such as JP3959043B2, and the cost of reagents involved is relatively high

Method used

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  • Synthesis method of amino-terminated polyolefin
  • Synthesis method of amino-terminated polyolefin
  • Synthesis method of amino-terminated polyolefin

Examples

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[0024] The present invention provides a kind of synthetic method of aminated polyolefin, comprising:

[0025] A) mixing the hydrohalogenation reagent and the polyolefin thermal degradation product, stirring, and reacting to obtain a terminal halogenated polyolefin macromer;

[0026] B) Mix terminal halogenated polyolefin macromonomer with solvent, feed ammonia gas, stir and react to obtain terminal aminated polyolefin.

[0027] The method for synthesizing end-aminated polyolefins provided by the invention firstly mixes a hydrohalogenation reagent and a thermal degradation product of polyolefins.

[0028] The thermal degradation product of polyolefin in the present invention is a thermal degradation product of polyolefin; the heating temperature is preferably 250°C-450°C. The present invention does not limit the thermal degradation time, which may be 0.5h to several hours.

[0029] The polyolefin of the present invention includes but not limited to polyethylene, polypropylene...

Embodiment 1

[0050] Embodiment 1 (taking polypropylene as example)

[0051] In a 500ml flask, add 100g of polypropylene thermal degradation product (Mn: 2800mol / g) into 300ml of hexane, then add 0.65 parts by weight of hydrogen bromide glacial acetic acid solution, stir at room temperature for 12h, then suction filter , washed with ethanol, and dried to obtain a brominated polypropylene macromonomer. Subsequently, the obtained terminal brominated polypropylene macromonomer was added into a high-pressure reactor containing 500 ml of tetrahydrofuran, and then saturated with ammonia gas, and then the reactor was heated to 150° C. and stirred for 10 h. Then, cool to room temperature, filter with suction, wash with ethanol and distilled water, and dry.

[0052] Carry out NMR analysis to the polymer prepared in this embodiment, figure 1 The H NMR spectra of raw materials for functionalized polypropylene, brominated polypropylene, and aminated polypropylene were prepared for this example. NMR ...

Embodiment 2

[0053] Embodiment 2 (taking polyethylene as example)

[0054] In a 500ml flask, add 100g of polyethylene thermal degradation product (Mn: 1474mol / g) and 300ml of toluene, then pass in hydrogen bromide gas, react at room temperature for 12h, and replace the hydrogen bromide gas with nitrogen gas exchange. Subsequently, the obtained terminal brominated polyethylene macromonomer was added into a high-pressure reactor containing 500 ml of tetrahydrofuran, saturated with ammonia gas, and then the reactor was heated to 100° C. and stirred for 10 h. Then, cool to room temperature, filter with suction, wash with ethanol and distilled water, and dry. NMR results show that the product is brominated, the degree of amination is 80%, and the overall functionality is 40-50%.

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Abstract

The invention provides a synthesis method of amino-terminated polyolefin, wherein the synthesis method comprises the steps: A) mixing a hydrohalogenation reagent and a polyolefin thermal degradation product, stirring and reacting to obtain a halogenated-terminated polyolefin macromonomer; and B) mixing the halogenated-terminated polyolefin macromonomer with a solvent, introducing ammonia gas, stirring, and reacting to obtain the aminated-terminated polyolefin. A pyrolysis product of polyolefin containing terminal double bonds is subjected to hydrohalogenation and amination to obtain amino-terminated polyolefin. The method is simple, low in cost and easy to control, raw materials are provided for synthesizing materials such as polyurethane and polyamide containing polyolefin blocks, and high value-added recovery of polyolefin is promoted.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a synthesis method of aminated polyolefin. Background technique [0002] Polyolefin is widely used in daily life due to its wide source of raw materials, low price and excellent performance. However, due to the non-polarity and low surface energy of polyolefin, its dyeability, adhesion, hydrophilicity, antistatic property and poor compatibility with other high molecular polymers limit the expansion of its application field. Therefore, the research on the functionalization of polyolefins has been paid more and more attention. [0003] In recent years, in order to solve these problems, research on new functionalized polyolefins has been actively carried out. One of them is the use of metallocene catalysts, by selecting the polymerization conditions, the β-position hydrogen atom at the growth end is selectively eliminated, and an ethylene-type double bond is formed at on...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F8/30C08F8/20C08F10/06C08F10/02C08F210/16
CPCC08F8/30C08F8/20C08F10/06C08F10/02C08F210/16
Inventor 唐涛蒋汉卿王艳辉马丽
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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