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

A technology of polyamide-imide and terpolymer, which is applied in the field of material science, can solve the problems of toxicity, no relevant reports on the synthesis of polyamide-imide, human and environmental hazards, etc., and achieves convenient operation and convenience. The effect of simple control and preparation process

Active Publication Date: 2012-10-03
广东中塑新材料股份有限公司
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  • 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 is no relevant report on the method of synthesizing polyamideimide by melt polymerization mechanism

Method used

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

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preparation example Construction

[0034] (1) Preparation of maleopimaric acid chloride

[0035] 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, maleopimaric anhydride reacts with thionyl chloride at room temperature to obtain maleopimaric acid chloride.

[0036] Gum rosin was purchased from Guangzhou Lvjin Resin Co., Ltd.

[0037] ①Abietic acid is purified from gum rosin:

[0038] Add 210 parts by w...

Embodiment 1

[0059] A kind of synthetic method of rosin base semialicyclic polyamide-imide terpolymer, comprises the steps:

[0060] (1) Using gum rosin and castor oil as raw materials, maleopimaric acid chloride and 11-aminoundecanoic acid were prepared respectively, and vacuum-dried together with 1,6-hexanediamine;

[0061] (2) The molar ratio of maleopimaric acid chloride, 1,6-hexanediamine, and 11-aminoundecanoic acid after vacuum drying is 1:0.95:0.5 (mass ratio is 4.190kg: 1.102kg: 1.005kg) Add to the stirring polymerization reactor respectively, vacuumize for 1 minute, and then pass helium for 30 minutes, so that the reactant exists in the environment under the protection of helium, and the system pressure in the reactor is controlled to be 0.3MPa;

[0062] (3) After sealing the reactor and heating it to 120°C, control the system pressure in the reactor to 1.3MPa, keep the reactants warm and pressurized for 24 hours, and slowly release the gas to normal pressure;

[0063] (4) Under...

Embodiment 2

[0066] A kind of synthetic method of rosin base semialicyclic polyamide-imide terpolymer, comprises the steps:

[0067] (1) Using gum rosin and castor oil as raw materials, maleopimaric acid chloride and 11-aminoundecanoic acid were prepared respectively, and vacuum-dried together with 1,6-hexanediamine;

[0068] (2) The molar ratio of maleopimaric acid chloride, 1,6-hexanediamine, and 11-aminoundecanoic acid after vacuum drying is 1:1:0.1 (mass ratio is 4.190kg: 1.160kg: 0.201kg) Add to the stirring polymerization reactor respectively, vacuumize for 30 minutes, and then pass nitrogen for 1 minute, so that the reactant exists in the environment under the protection of nitrogen, and the system pressure in the reactor is controlled to 0.1MPa;

[0069] (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 hour...

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Abstract

The invention discloses a synthetic method for a rosin-base half alicyclic polyamide imide (PAI) terpolymer. According to the method, the rosin-base half alicyclic polyamide imide (PAI) terpolymer is prepared by maleopimaric acid acyl chloride (a derivative of rosin), 11- amino undecanoic acid (a derivative of castor oil), and (1, 6) hexanediamine. 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, andhazards on the human body and the environement are prevented. The polymerized polyamide imide (PAI) terpolymer 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 belongs to the field of material science, in particular to a rosin-based semialicyclic polyamide-imide terpolymer and a synthesis method thereof. Background technique [0002] 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, maleopimaric anhydride reacts with thionyl chloride at room temperature to obtain maleopimaric acid chlor...

Claims

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Application Information

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IPC IPC(8): C08G73/14
Inventor 朱怀才王忠强
Owner 广东中塑新材料股份有限公司
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