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A kind of alkyl-based dynamic cross-linking agent and its application

A cross-linking agent and alkyl-based technology, which is applied in the field of polymer material modification, can solve the problems of difficult practical application of materials, expensive raw materials, low mechanical properties of materials, etc., and achieve good repetitive processing characteristics, improved impact strength, improved The effect of mechanical properties

Active Publication Date: 2021-04-30
HUAQIAO UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it has been reported that reversible dynamic cross-linked polymer materials have disadvantages such as cumbersome preparation process of dynamic small molecules, expensive raw materials, and low mechanical properties of materials, which make the practical application of materials difficult, and are mainly concentrated in hydrogel systems. , less used in the field of polymer resin

Method used

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  • A kind of alkyl-based dynamic cross-linking agent and its application
  • A kind of alkyl-based dynamic cross-linking agent and its application
  • A kind of alkyl-based dynamic cross-linking agent and its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Synthesis of alkyl-based dynamic crosslinker DTC7 (heptane-1,7-diylbis(methylazanediyl))bis(2,1-phenylene))diboronic acid):

[0027] Concrete reaction equation is as follows:

[0028]

[0029] The specific implementation steps are as follows: in a round bottom flask, add 2.22g of dibromoheptane, 12.6g of anhydrous potassium carbonate, and then add 300mL of anhydrous chloroform as a solvent. Simultaneously, 10 mL of a solution of (N-methyl) 2-aminophenylboronic acid (3 g) was configured with anhydrous chloroform, and this solution was added dropwise to a chloroform solution of dibromoheptane, under the protection of argon, at 40 Celsius reaction for 16 hours. The product was concentrated by rotary evaporator and purified by reverse phase chromatography. The yield is higher than 85%. The corresponding NMR data of the product are as follows: 1H NMR (500MHz, CD 3 OD): δ7.64, 7.28, 7.18, 6.8, 4.6, 2.97, 2.60, 1.77, 1.42. 13C NMR (125MHz, CD 3 OD): δ133.3, 128.7, 127....

Embodiment 2

[0031] Synthesis of alkyl-based dynamic crosslinker DTC5 (((pentane-1,5-diylbis(methylazanediyl))bis(2,1-phenylene))diboronic acid:

[0032] Concrete reaction equation is as follows:

[0033]

[0034] The specific implementation steps are as follows: in a round bottom flask, add 1.98g of dibromoheptane, 12.6g of anhydrous potassium carbonate, and then add 300mL of anhydrous chloroform as a solvent. Simultaneously, 10 mL of a solution of (N-methyl) 2-aminophenylboronic acid (3 g) was configured with anhydrous chloroform, and this solution was added dropwise to a chloroform solution of dibromoheptane, under the protection of argon, at 40 Celsius reaction for 16 hours. The product was concentrated by rotary evaporator and purified by reverse phase chromatography. The yield is higher than 91%. The corresponding NMR data of the product are as follows: 1H NMR (500MHz, CD 3 OD): δ7.61, 7.27, 7.15, 6.9, 4.8, 3.1, 1.82, 1.45. 13C NMR (125MHz, CD 3 OD): δ136.7, 131.2, 126.1, 124...

Embodiment 3

[0035] The preparation of embodiment 3 reversible cross-linked polyamide 6:

[0036] (1) Preparation of reversible dynamic cross-linked polyamide masterbatch:

[0037] In this example, the alkyl-based dynamic cross-linking agent DTC7 prepared in Example 1 is used as a typical alkyl-based dynamic cross-linking agent for description:

[0038] Add 2% of the antioxidant system (antioxidant 1010:antioxidant 168=1:2) to 1kg polyamide 6, and stir evenly; add 0.2kg of the above-mentioned alkyl dynamic crosslinking agent DTC7 to a high-speed mixer, and Under the conditions, the mixture is fully mixed for 30 minutes to obtain a mixture; the mixture is melted, mixed and granulated in a twin-screw extruder to obtain a dynamic crosslinking agent masterbatch, and the melting temperature is controlled below 280°C.

[0039] (2) Preparation of reversibly crosslinked polyamide 6: in 5kg polyamide 6, add more than 1kg of dynamic crosslinking agent masterbatch, fully disperse in a high-speed mix...

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Abstract

The invention discloses an alkyl-based dynamic cross-linking agent and its application. The structural formula is: wherein n=5-10. The alkyl-based dynamic cross-linking agent of the present invention can effectively realize the dynamic cross-linking process of the polymer material through its phenylboronic acid and the active wave hydrogen of the secondary ammonia in the amide group to generate hydrogen bonds.

Description

technical field [0001] The invention belongs to the technical field of polymer material modification, and in particular relates to an alkyl-based dynamic crosslinking agent and its application. Background technique [0002] Polymers and their composite materials have excellent characteristics such as low density, high specific strength and specific modulus, and good toughness, and are widely used in various fields of the national economy. However, with the development of social economy, higher performance requirements are put forward for materials. Therefore, effectively and fully improving the performance of materials has become a key issue in the research of polymer materials. [0003] The interpenetrating network structure refers to a polymer network formed by two or more polymers interpenetrating with each other. The interaction between different polymer networks is not connected by chemical bonds, but by chain entanglement and non-covalent bond interactions. It is an e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/55C08L77/02C08L77/06C08L79/08
CPCC08K5/55C08L77/02C08L77/06C08L79/08C08L2312/00
Inventor 钱浩张莹雪林志勇王缸荣
Owner HUAQIAO UNIVERSITY