Preparation method of poly-p-aminobenzoylamonoundecylamine

A technology of aminobenzamide and poly-pair, which is applied in the field of synthesis of polymer materials and can solve the problems of difficult synthesis of PA11T

Inactive Publication Date: 2013-05-29
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem of difficult synthesis of existing PA11T, the present invention provides a preparation method of poly-p-aminobenzamide undecylamine (PA11T) with good heat resistance, mechanical properties and environmental protection

Method used

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  • Preparation method of poly-p-aminobenzoylamonoundecylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 (10 grams per serving)

[0033] The preparation method of poly-p-aminobenzamide undecylamine, its preparation steps are:

[0034] (1) Salt formation: Mix 200 grams of aminoundecanoic acid, 140 grams of p-aminobenzoic acid, 1500 grams of distilled water, and 2 grams of phosphoric acid, stir well, and react at 120 ° C for 3 hours; then filter and wash , dried in vacuum to obtain PA11T salt;

[0035] (2) Adding materials: PA11T salt, distilled water with the same weight as PA11T salt, 0.6% (w / w) acetic acid for PA11T salt, stir evenly to obtain a mixture;

[0036] (3) Reaction synthesis: the mixture is heated up to 270°C in a helium atmosphere, pressurized to 3MPa, and kept at a constant pressure for 2h; then lowered to normal pressure for 2h, raised to 320°C while lowering to normal pressure, and kept for 2h; finally pumped Vacuum to -0.095MPa, keep the temperature and pressure for 1h, and discharge to obtain PA11T.

[0037] The preparation steps are carried...

Embodiment 2

[0039] Example 2 (20 grams per serving)

[0040] The preparation method of poly-p-aminobenzamide undecylamine, its preparation steps are:

[0041] (1) Salt formation: Mix 400 grams of aminoundecanoic acid, 280 grams of p-aminobenzoic acid, 3000 grams of distilled water, and 4 grams of sodium phosphate, stir well, and react at 120 °C for 3 hours; then filter with suction, Washing, vacuum drying, to obtain PA11T salt;

[0042] (2) Adding materials: PA11T salt, methanol with the same weight as PA11T salt, and 1.2% (w / w) butylamine for PA11T salt are stirred evenly to obtain a mixture;

[0043] (3) Reaction synthesis: the mixture was heated up to 280°C in an argon atmosphere, pressurized to 2.5MPa, kept at a constant pressure for 2 hours; then lowered to normal pressure for 2 hours, raised to 310°C while lowering to normal pressure, and kept for 2 hours; finally Vacuumize to -0.095MPa, keep the temperature and pressure for 1h, and discharge the material to obtain PA11T.

[00...

Embodiment 3

[0045] Example 3 (15 grams per serving)

[0046]The preparation method of poly-p-aminobenzamide undecylamine, its preparation steps are:

[0047] (1) Salt formation: Mix 300 grams of aminoundecanoic acid, 210 grams of p-aminobenzoic acid, 2250 grams of distilled water, and 3 grams of phosphorous acid, stir well, and react at 120°C for 3 hours; then filter with suction, Washing and vacuum drying to obtain PA11T salt;

[0048] (2) Adding: Mix PA11T salt, ethanol with the same weight as PA11T salt, and 1.0% (w / w) lauric acid for PA11T salt, and stir evenly to obtain a mixture;

[0049] (3) Reaction synthesis: the mixture was heated up to 290°C in a nitrogen atmosphere, pressurized to 2.7MPa, kept at a constant pressure for 2 hours; then lowered to normal pressure for 2 hours, raised to 330°C while lowering to normal pressure, and kept for 2 hours; finally pumped Vacuum to -0.095MPa, keep the temperature and pressure for 1h, and discharge to obtain PA11T.

[0050] The perform...

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Abstract

The invention relates to the field of synthesis of high polymer materials, particularly a preparation method of poly-p-aminobenzoylamonoundecylamine, which comprises the following steps: (1) salification: uniformly stirring 20 parts by weight of aminoundecanoic acid, 14 parts by weight of p-aminobenzoic acid, 150 parts by weight of distilled water and 0.2 part by weight of catalyst, reacting at 120 DEG C for 3 hours, carrying out vacuum filtration, washing, and carrying out vacuum drying to obtain PA11T salt; (2) feeding: stirring uniformly the PA11T salt, distilled water or organic solvent with the same weight as the PA11T salt, and a blocking agent accounting for 0.6-1.2% (w/w) of the PA11T salt to obtain a mixture; and (3) reaction synthesis: heating the mixture to 270-290 DEG C in a protective gas atmosphere, pressurizing to 2.5-3 MPa, keeping the temperature and pressure for 2 hours, reducing to atmospheric pressure within 2 hours while heating to 310-330 DEG C, keeping the temperature for 2 hours, vacuumizing to -0.095 MPa, keeping the temperature and pressure for 1 hour, and discharging, thereby obtaining the PA11T.

Description

technical field [0001] The invention relates to the field of synthesis of polymer materials, in particular to a preparation method of poly-p-aminobenzamide undecylamine. Background technique [0002] With the continuous development of science and technology and the continuous expansion of market demand, nylon has become a very important variety of engineering plastics. Poly-p-aminobenzamide undecylamine (PA11T) is a new type of long carbon chain semi-aromatic nylon. Generally, among nylon molecules, nylon with a carbon chain length of 10 or more is called long carbon chain nylon. In addition to some common properties of general nylon, long carbon chain nylon also has many unique advantages, such as low density, good molding stability, low water absorption and so on. Semi-aromatic nylon is a nylon resin prepared by polycondensation of diamines or dicarboxylic acids with aromatic rings and aliphatic dicarboxylic acids or diamines. Due to the introduction of aromatic rings i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/12C08G69/08
Inventor 胡国胜李洁刘宇辰曲振王建霞李迎春杨云峰张静婷宋江锋王志强
Owner ZHONGBEI UNIV
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