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Polyamide-imide prepared by adopting microchannel reactor and preparation method of polyamide-imide

A technology of microchannel reactor and polyamide-imide, which is applied in the field of material chemical industry, can solve problems such as incomplete reaction, poor safety performance, and insufficient mixing, so as to facilitate scale-up production, stable product performance, and increase economic cost Effect

Pending Publication Date: 2022-03-04
LANZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional kettle reaction mainly has the following disadvantages: 1). Due to insufficient stirring and uneven heat conduction in the kettle reaction, the reaction degree of the substrate is inconsistent or the reaction is not complete, which affects the molecular weight distribution of the polymer to a certain extent and affects the material. performance
2). The temperature control of the kettle reaction is not accurate
3). The tank reaction has a long production cycle
4). The tank reaction has a large single feeding amount and relatively poor safety performance
5). Kettle reactions are generally batch or semi-batch operations, with high risk factors, poor safety, and low efficiency
Patent CN111909062A discloses a method for preparing methanesulfonyl chloride with a microchannel reactor, which can efficiently, safely and conveniently produce methanesulfonyl chloride continuously, and solves the safety and efficiency problems brought about by traditional kettle production

Method used

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  • Polyamide-imide prepared by adopting microchannel reactor and preparation method of polyamide-imide
  • Polyamide-imide prepared by adopting microchannel reactor and preparation method of polyamide-imide
  • Polyamide-imide prepared by adopting microchannel reactor and preparation method of polyamide-imide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Preparation method of isocyanate excess 5% polyamide imide polymer solution, including the following steps:

[0046] (1) Pretreatment of substrate: 0.5 g of MDi51.96 g, TmA38.04 g, NMP210g, catalyst stearate, in a 500 ml beaker, and the solution was heated to 85 ° C under magnetic stirring conditions and maintained for 5 min. Stand in the substrate clear and restore the room temperature;

[0047] (2) Negative pressure divided CO 2 : The substrate produces a small amount of carbon dioxide gas during the pretreatment stage, and the substrate solution of the above step is poured into a 500 mL single-mouth bottle, and the pump is pulled up to dissolve the carbon dioxide excretion of dissolved in the solution;

[0048] (3) Parameter setting: adjust the constant temperature device, set the temperature of 165 ° C; adjust the constant current pump flow rate of 15 ml / min; pump the solvent NMP into the microreactor, by adjusting the back pressure valve knob to the pressure loss is ...

Embodiment 2

[0054] The preparation method of a polyamide imide polymer solution of a carboxylic acid is, including the following steps:

[0055] Comparative Example 1, the difference is that the substrate pretreatment: MDI49.80G, TmA40.20g, NMP210g, catalyst stearate 0.5 g, sequentially added 500 ml of beaker, and the solution under magnetic stirring conditions Heat until 85 ° C and kept 5 min, and the substrate was clear and transparent and restored at room temperature. The remaining steps are the same.

[0056] Infrared light analysis is performed on the product of this Example 2, and the results are respectively image 3 Indicated. image 3 Medium, at 3462cm -1 The peak appearing is the telescopic vibration absorption peak of amide bond N-H. At 1670cm -1 It is a telescopic vibration absorption peak in the amide in the amide, and its greater direction to the wave number is due to the increase in the PMDA content, resulting in increased imine rings to affect the peak position. 1779CM -1 1725cm...

Embodiment 3

[0058] Preparation of the isocyanate excess 5% PMDA involved in the reaction of the polyamide imide polymer solution, including the following steps:

[0059] Different from the first embodiment, the substrate pretreatment: MDI51.40g, TmA30.88 g, PMDA7.72G, NMP210G, catalyst stearate 0.5 g, sequentially added 500 ml of beaker, in magnetic stirring conditions The solution was heated to 85 ° C and maintained for 5 min, and the contained substance was clear and returned after returning. The remaining steps are the same.

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Abstract

The invention discloses polyamide-imide prepared by adopting a microchannel reactor and a preparation method of the polyamide-imide, and the polyamide-imide is obtained by carrying out solution polycondensation on diisocyanate monomers and difunctional acid anhydride or carboxyl compounds in a continuous flow microchannel reactor according to a certain proportion under a certain condition. The polyamide-imide prepared by the invention has the advantages of high reaction efficiency, simplicity and convenience in operation, good safety, easiness in control, continuous production, cost saving and the like, is beneficial to large-scale production, and has wide application prospects.

Description

Technical field [0001] The present invention belongs to the field of material chemical technology, and more particularly to a polyamide imide, a microchannel reactor, and a preparation method thereof. Background technique [0002] Polyamide imides, referred to as PAI refers to a class of polymer polymers containing an amide bond and an imide ring on the backbone. Since the molecular chain is simultaneously having a strong amide bond and a high heat resistance imide ring, it not only has a polyamide excellent mechanical properties and processability, but also has excellent heat resistance of polyimide. Dielectric, mechanical properties, creep resistance and chemical stability. Polyamide-amide polymer materials have gradually become a well-developed engineering plastics, which is increasingly widely used in aerospace, transportation, chemical equipment, electronics industries, such as enhanced lines, integrated optical path materials, nanocomposites, Electronic package material, ad...

Claims

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Application Information

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IPC IPC(8): C08G73/10
CPCC08G73/1035
Inventor 郭金山杨发虎霍丽霞周晖刘兴妤
Owner LANZHOU UNIVERSITY
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