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Biobase long carbon chain half alicyclic polyamide imide terpolymer and synthetic method thereof

A polyamide-imide terpolymer and a synthesis method technology are applied in the field of bio-based long carbon chain semi-alicyclic polyamide-imide terpolymer and its synthesis, and can solve the problem of toxicity, human body and environment. Risk and other issues, to achieve the effect of convenient operation, good mechanical and thermal properties, and simple 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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Organic solvents have major disadvantages in the use process. On the one hand, additional steps are required for solvent recovery after polymer synthesis, and additional steps are required for the precipitation of polymers in non-good solvents and the recovery of organic solvents used in polymer washing. ; On the other hand, some solvents are toxic and therefore dangerous to humans and the environment

Method used

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  • Biobase long carbon chain half alicyclic polyamide imide terpolymer and synthetic method thereof
  • Biobase long carbon chain half alicyclic polyamide imide terpolymer and synthetic method thereof
  • Biobase long carbon chain half alicyclic polyamide imide terpolymer and synthetic method thereof

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preparation example Construction

[0031] (1) Preparation of maleopimaric acid chloride

[0032] 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.

[0033] Gum rosin was purchased from Guangzhou Lvjin Resin Co., Ltd.

[0034] ①Abietic acid is purified from gum rosin:

[0035] Add 210 parts by w...

Embodiment 1

[0056] A kind of synthetic method of bio-based long carbon chain semialicyclic polyamide-imide terpolymer, comprising the following steps:

[0057] (1) Using gum rosin and castor oil as raw materials, maleopimaric acid chloride, 1,10-decanediamine and 11-aminoundecanoic acid were prepared and dried;

[0058] (2) The molar ratio of maleopimaric acid chloride, 1,10-decanediamine, and 11-aminoundecanoic acid after vacuum drying is 1:0.95:0.5 (mass ratio is 4.190kg: 1.634kg: 1.005kg) , respectively added to the stirring polymerization reactor, evacuated for 1 minute, and then helium was passed for 30 minutes, and this cycle was repeated 20 times, so that the reactants existed in an environment protected by helium, and the system pressure in the reactor was controlled to be 0.3 MPa;

[0059] (3) Airtightly heat the reactor to 110°C, control the system pressure in the reactor to 1.3MPa, keep the temperature and pressure of the reactant for 24 hours, and slowly release the gas to nor...

Embodiment 2

[0062] A kind of synthetic method of bio-based long carbon chain semialicyclic polyamide-imide terpolymer, comprising the following steps:

[0063] (1) Using gum rosin and castor oil as raw materials, maleopimaric acid chloride, 1,10-decanediamine and 11-aminoundecanoic acid were prepared and dried;

[0064] (2) The molar ratio of maleopimaric acid chloride, 1,10-decanediamine, and 11-aminoundecanoic acid after vacuum drying is 1:1:0.3 (mass ratio is 4.190kg: 1.720kg: 0.603kg) 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;

[0065] (3) Airtightly heat the reactor to 140°C, adjust the stirring speed of the polymerization reactor to 200r / min, control the system pressure in the reactor to 1.1MPa, keep the temperature and pressure of the reactant for 0.5h, and slowly...

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Abstract

The invention discloses a synthetic method of a biobase long carbon chain half alicyclic polyamide imide terpolymer, which is as follows: maleopimaric acid acyl chloride, (1, 10) - decamethylene diamine, and 11- amino undecanoic acid are prepared respectively by taking gum rosin and castor oil as raw materials, and then are dried; after drying, maleopimaric acid acyl chloride, (1, 10) - decamethylene diamine, and 11- amino undecanoic acid are added into a stirring polymer reactor and inert gases are fed in after vacuumization, and the process is circulated; the polymer reactor is heated hermetically; after the stirring rate is adjusted, reactants are thermal insulated and pressurized, and then the polymer reactor is released to normal pressure; the polymer reactor is heated once more, thestirring rate is adjusted, the polymer reactor is vacuumized continuously after reaching the constant temperature, and finally the reaction is over. The polyamide imide terpolymer prepared through the method is easy to form, has better mechanical and thermal properties, and is the absolute biological material; the preparation technology is simple and convenient, thereby facilitating management and control; gum rosin and castor oil used in the method are renewable resources easy to get; the synthesizing mechanism adopts fusion polymerization, and no any organic solvent is used, and no danger for the human body and the environement exists; and the safety is high.

Description

technical field [0001] The invention relates to a bio-based long carbon chain 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 chloride. [0003] Castor oil is a r...

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