Bio-based long-carbon-chain semi-alicyclic polyamide-imide PA10I and synthesizing method thereof

A technology of polyamideimide and its synthetic method, which is applied in the field of bio-based long carbon chain semialicyclic polyamideimide PA10I and its synthesis, and can solve the problem of no relevant reports and toxicity of synthetic polyamideimide. , human body and environmental hazards, and achieve the effects of low dimensional stability, convenient operation, and easy control

Active Publication Date: 2012-10-10
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 is no relevant report on the method of synthesizing polyamideimide by melt polymerization mechanism

Method used

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  • Bio-based long-carbon-chain semi-alicyclic polyamide-imide PA10I and synthesizing method thereof
  • Bio-based long-carbon-chain semi-alicyclic polyamide-imide PA10I and synthesizing method thereof
  • Bio-based long-carbon-chain semi-alicyclic polyamide-imide PA10I and synthesizing method thereof

Examples

Experimental program
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Effect test

preparation example Construction

[0027] (1) Preparation of maleopimaric acid chloride

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

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

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

[0031] Add 210 parts by w...

Embodiment 1

[0050] Embodiment 1 A kind of synthetic method of bio-based long carbon chain semialicyclic polyamide-imide PA10I

[0051] Include the following steps:

[0052] (1) Using gum rosin and castor oil as raw materials, maleopimaric acid chloride and 1,10-decanediamine were prepared respectively, and vacuum-dried;

[0053] (2) Add the dried maleopimaric acid chloride and 1,10-decanediamine in a mass ratio of 4.190kg: 1.462kg (molar ratio 1:0.85) into the stirred polymerization reactor, vacuumize for 1min, and pass through helium Gas for 30min, so circulated 20 times, so that the reactant exists in the environment under the protection of nitrogen, and the system pressure in the control reactor is 0.3MPa;

[0054] (3) Airtightly heat the reactor to 110° C., control the system pressure in the reactor to 1.1 MPa, keep the reactant at a pressure-holding temperature for 24 hours, and slowly release the gas to normal pressure;

[0055] (4) Reheat to 250° C., keep vacuuming for 24 hours a...

Embodiment 2

[0056] Embodiment 2 A kind of synthetic method of bio-based long carbon chain semialicyclic polyamide-imide PA10I

[0057] Include the following steps:

[0058] (1) Using gum rosin and castor oil as raw materials, maleopimaric acid chloride and 1,10-decanediamine were prepared respectively, and vacuum-dried;

[0059] (2) Add the dried maleopimaric acid chloride and 1,10-decanediamine in a mass ratio of 4.190kg: 1.634kg (molar ratio 1:0.95) into the stirring polymerization reactor, vacuumize for 30min, and pass nitrogen gas 1min, such cycle 1 time, so that the reactants exist in the environment under the protection of nitrogen, control the system pressure in the reactor to 0.1MPa;

[0060] (3) Airtightly heat the reactor to 140°C, and adjust the stirring speed of the polymerization reactor to 500r / min, control the system pressure in the reactor to 1.3MPa, keep the temperature and pressure of the reactant for 0.5 hours, and slowly release the gas to normal pressure;

[0061] ...

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Abstract

The invention discloses a synthesizing method for bio-based long-carbon-chain semi- alicyclic polyimide-imide. Maleopimaric acid acyl chloride and 1,10-decamethylene diamine respectively made of gum rosin and castor oil as raw materials are put into a stirring-type polymerization reaction container; inert gases are fed after the stirring-type polymerization reaction container is vacuumized; the polymerization reaction container is heated hermetically; after the stirring speed of the polymerization reaction container is adjusted, the reactants are thermally insulated and pressurized, and the gases are discharged so as to obtain ordinary pressure; the polymerization reaction container is heated again, the stirring speed of the polymerization reaction container is adjusted, and the polymerization reaction container is continually vacuumized after constant temperature is obtained; and the bio-based long-carbon-chain semi-alicyclic polyimide is obtained after the reaction is over. The synthesizing method of the invention is based on the principle of melt polycondensation and the whole synthesis process does not require any organic solvent, so that no additional steps to recover organic solvent are needed , and no toxin or harm is generated to people and the environment. The synthesized polyamide-imide PA10I has the advantages of good heat resistance, high-temperature rigidity, dimensional stability and low water absorption. The polyamide-imide PA10I can be used for engineering plastics or film materials and the like.

Description

technical field [0001] The invention relates to a bio-based long carbon chain semialicyclic polyamide-imide PA10I 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, maleopimaric anhydride reacts with thionyl chloride at room temperature to obtain maleopimaric acid chlo...

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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