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Rosin-base half alicyclic polyamide imide copolymer and synthetic method thereof

A technology of polyamide-imide copolymer and synthesis method, which is applied in the field of rosin-based semi-alicyclic polyamide-imide copolymer and its synthesis, which can solve the problem of human and environmental hazards, toxicity, and no related reports and other problems, to achieve the effect of low dimensional stability, convenient operation and simple process

Active Publication Date: 2012-10-03
SINOPLAST NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Organic solvents have major disadvantages during use. On the one hand, additional steps are required for solvent recovery after polymer synthesis, and the precipitation of polymers in non-good solvents and the recovery of organic solvents used in polymer washing also require additional steps. steps; on the other hand, some solvents are toxic and therefore dangerous to humans and the environment
There are no relevant reports on the method of synthesizing polyamideimide polymers by melt polymerization mechanism

Method used

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  • Rosin-base half alicyclic polyamide imide copolymer and synthetic method thereof
  • Rosin-base half alicyclic polyamide imide copolymer and synthetic method thereof
  • Rosin-base half alicyclic polyamide imide copolymer and synthetic method thereof

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preparation example Construction

[0027] (1) Preparation of maleopimaric dianhydride

[0028] Gum rosin is a renewable natural chemical raw material, which contains about 90% resin acid and about 10% ester and unsaponifiable substances. The main component of resin acid is abietic acid with conjugated double bonds, and the conjugated double bonds in the molecular structure of abietic acid are not in the same alicyclic ring, so it cannot perform Diels-Alder reaction with double bond compounds such as maleic anhydride, but in At high temperature, abietic acid can be converted into pimaric acid through isomerization equilibrium reaction. Pimaric acid is obtained through Diels-Alder reaction with maleic anhydride to obtain maleopimaric anhydride. Finally, 2 mol of maleopimaric anhydride can be catalyzed by p-toluenesulfonic acid to produce 1 mol of maleopimaric dianhydride.

[0029] Gum rosin was purchased from Guangzhou Lvjin Resin Co., Ltd.

[0030] ①Abietic acid is purified from gum rosin:

[0031] Add 210 p...

Embodiment 1

[0051] Embodiment 1 A kind of synthetic method of rosin-based semialicyclic polyamide-imide copolymer

[0052] Include the following steps:

[0053] (1) Taking gum rosin and castor oil as raw materials, prepare maleopimaric acid dianhydride and 11-aminoundecanoic acid respectively, and vacuum-dry;

[0054] (2) Add maleopimaric acid dianhydride, 1,6-hexanediamine and 11-aminoundecanoic acid in a molar ratio of 1:0.9:0.5 (mass ratio of 7.390kg:1.044kg:1.005kg) into the stirring formula In the polymerization reactor, after evacuating for 1 minute, helium is passed for 30 minutes, and this cycle is repeated 20 times, so that the reactant exists in an environment protected by helium, and the system pressure in the reactor is controlled to be 0.3 MPa;

[0055] (3) After sealing the reactor and heating it to 120°C, control the system pressure in the reactor to 1.3MPa, keep the reactant under pressure for 24 hours, and slowly release the gas to normal pressure;

[0056] (4) Under no...

Embodiment 2

[0058] Embodiment 2 A kind of synthetic method of rosin-based semialicyclic polyamide-imide copolymer

[0059] Include the following steps:

[0060] (1) Taking gum rosin and castor oil as raw materials, prepare maleopimaric acid dianhydride and 11-aminoundecanoic acid respectively, and vacuum-dry;

[0061] (2) Add maleopimaric acid dianhydride, 1,6-hexanediamine and 11-aminoundecanoic acid in a molar ratio of 1:1:0.3 (mass ratio of 7.390kg:1.160kg:0.603kg) into the stirring formula In the polymerization reactor, after evacuating for 30 minutes, pass nitrogen for 1 minute, and cycle like this once, so that the reactant exists in an environment under nitrogen protection, and the system pressure in the reactor is controlled to be 0.1 MPa;

[0062] (3) Airtightly heat the reactor to 170°C, and adjust the stirring speed of the polymerization reactor to 500r / min, control the system pressure in the reactor to 1.1MPa, keep the temperature and pressure of the reactant for 0.5 hours, a...

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Abstract

The invention discloses a rosin-base half alicyclic polyamide imide copolymer and a synthetic method thereof. According to the invention, maleopimaric acid dianhydride, 11- amino undecanoic acid and (1, 6) -hexanediamine, which are prepared by taking gum rosin and castor oil as raw materials, are added into stirring polymer reactor together, and the polymer reactor is vacuumized and then fed with inert gases; the polymer reactor is heated hermetically, the stirring rate of the polymer reactor is adjusted, then reactants are thermal insulated and pressurized, and the polymer reactor is released to normal pressure; the polymer reactor is heated once more, the stirring rate of the polymer reactor is adjusted, the polymer reactor is vacuumized continuously after reaching the constant temperature, the reaction is over, and the copolymer is obtained. The synthetic method disclosed by the invention is based on the fusion polymerization principle, and no organic solvent is used during the whole polymerization process, therefore, additional steps for recovering the organic solvent are avoided, and hazards on the human body and the environement are prevented. The polymerized polyamide imide copolymer has good thermal resistance, high-temperature rigidity, size stability and low water absorption, and can be applied to engineering plastics, membrane materials and the like.

Description

technical field [0001] The invention relates to a rosin-based semialicyclic polyamide-imide copolymer and a synthesis method thereof. Background technique [0002] China is a big producer of gum rosin. Gum rosin is a renewable natural chemical raw material, which contains about 90% resin acid and about 10% ester and unsaponifiable substances. The main component of resin acid is abietic acid with conjugated double bonds, and the conjugated double bonds in the molecular structure of abietic acid are not in the same alicyclic ring, so it cannot perform Diels-Alder reaction with double bond compounds such as maleic anhydride, but in At high temperature, abietic acid can be converted into pimaric acid through isomerization equilibrium reaction. And pimaric acid is obtained maleopimaric anhydride by carrying out Diels-Alder reaction with maleic anhydride. Finally, 2 mol of maleopimaric anhydride can be catalyzed by p-toluenesulfonic acid to produce 1 mol of maleopimaric dianhydr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/14
Inventor 朱怀才王忠强
Owner SINOPLAST NEW MATERIAL
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