Rosin-based semi-alicyclic polyamide-imide PA6I and synthesizing method thereof

A polyamide-imide and synthesis method technology, applied in the field of rosin-based semi-alicyclic polyamide-imide PA6I and its synthesis, can solve the problems of inconvenient control, large consumption of organic solvent, complicated polymerization process, etc., and achieve convenient The effect of control, convenient operation and simple preparation process

Active Publication Date: 2012-10-10
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

[0005] Based on this, it is necessary to provide a synthetic method of rosin-based semi-alicyclic polyamide-imide PA6I for the problems of large organic solvent consumption, many process procedures, complicated polymerization process and inconvenient control in the preparation process of polyamide-imide.

Method used

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  • Rosin-based semi-alicyclic polyamide-imide PA6I and synthesizing method thereof
  • Rosin-based semi-alicyclic polyamide-imide PA6I and synthesizing method thereof
  • Rosin-based semi-alicyclic polyamide-imide PA6I and synthesizing method thereof

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preparation example Construction

[0033] ③Preparation of maleopimaric anhydride:

[0034] Add 100 parts by weight of pimaric acid, 17 parts by weight of maleic anhydride, 3.33 parts by weight of p-toluenesulfonic acid (TSA), 55 parts by weight of ice After the acetic acid, pass nitrogen gas for 15 minutes to make the reactants exist in the environment under the protection of nitrogen gas. Slowly heat to 110°C. After the material is basically melted, turn on the stirrer at a stirring speed of 50r / min, and continue to heat up evenly. Adjust the reaction temperature in the bottle by adjusting the amount of acetic acid in the reaction bottle. After the temperature in the reaction bottle rises to After 180° C., keep this temperature for 4 hours, then lower the temperature. When the temperature in the reaction bottle drops to 110° C., add 210 parts by weight of glacial acetic acid and stir evenly. When the material was lowered to room temperature, it was further cooled with ice water, and the white crystalline crud...

Embodiment 1

[0045]Embodiment 1 A kind of synthetic method of rosin-based semialicyclic polyamide-imide PA6I

[0046] Include the following steps:

[0047] (1) Using gum rosin as raw material, prepare maleopimaric acid chloride and dry it in vacuum;

[0048] (2) Add maleopimaric acid chloride and 1,6-hexanediamine in a molar ratio of 1:0.85 (mass ratio: 4.190kg:0.986kg) into the stirred polymerization reactor after vacuum drying, and vacuumize for 1min After passing helium for 30 minutes, this cycle is repeated 20 times, so that the reactant exists in the environment under the protection of helium, and the system pressure in the reactor is controlled to 0.3MPa;

[0049] (3) Seal the polymerization reactor and heat it to 130°C, control the system pressure in the reactor to 1.1MPa, and keep the reactant under pressure for 24 hours, then slowly release the gas to normal pressure;

[0050] (4) Under normal pressure, continue to heat the polymerization reactor to 320°C, keep vacuuming for 1 h...

Embodiment 2

[0051] Embodiment 2 A kind of synthetic method of rosin-based semialicyclic polyamide-imide PA6I

[0052] Include the following steps:

[0053] (1) Using gum rosin as raw material, prepare maleopimaric acid chloride and dry it in vacuum;

[0054] (2) Add maleopimaric acid chloride and 1,6-hexanediamine in a molar ratio of 1:0.95 (mass ratio: 4.190kg:1.102kg) into the stirred polymerization reactor after vacuum drying, and vacuumize for 30 minutes Then pass nitrogen gas for 1 min, and cycle like this once, so that the reactant exists in the environment under the protection of nitrogen gas, and the system pressure in the reactor is controlled to 0.1MPa;

[0055] (3) Seal the polymerization reactor and heat it to 170°C, adjust the stirring speed to 500r / min, control the system pressure in the reactor to 1.3MPa, and keep the reactant under pressure for 0.5h, then slowly release the gas to normal pressure;

[0056] (4) Under normal pressure, continue to heat the polymerization re...

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Abstract

The invention discloses a synthesizing method for rosin-based semi-alicyclic polyamide-imide PA6I. Maleopimaric acid acyl chloride is prepared by using gum rosin as raw materials, and the maleopimaric acid acyl chloride is dried through vacuumization; the dried maleopimaric acid acyl chloride and 1,6-hexanediamine are put into a stirring-type polymerization reaction container, and inert gases are fed after the stirring-type polymerization reaction container is vacuumized; the polymerization reaction container is heated hermetically; after the stirring speed is adjusted, the polymerization reaction container is thermally insulated and pressurized, and the gases are discharged so as to obtain ordinary pressure; and under ordinary pressure, the polymerization reaction container continues to be heated, the stirring speed is adjusted, and the polymerization reaction container is continually vacuumized after constant temperature is obtained; and the rosin-based semi-alicyclic polyamide-imidePA6I is obtained after the reaction is over. The rosin-based semi-alicyclic polyamide-imide produced by the invention is environment-friendly material, and has the advantages of good heat resistance, high-temperature rigidity, dimensional stability, and low water absorption; the preparation technique is simple, and the polymerization process is convenient, so that control and industrialization are easily achieved; and the synthesizing process is melt polycondensation with no organic solvent and no danger to people and the environment.

Description

technical field [0001] The invention relates to a rosin-based semi-alicyclic polyamide-imide PA6I and a synthesis method thereof. Background technique [0002] Gum rosin is a renewable natural chemical raw material, which contains about 90% resin acid, about 10% ester and unsaponifiable substances. The main component of resin acid is abietic acid with conjugated double bonds. 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 at high temperature Butabietic 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] Polyamide-imide (PAI) is an industrial polymer...

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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