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Method for preparing polyimide and polyimide prepared thereby

一种聚酰亚胺、低聚物的技术，应用在制备聚酰亚胺和由此制备的聚酰亚胺领域，能够解决难以加工、混合物粘稠、没有广泛地实践熔融聚合等问题

Active Publication Date: 2007-01-03
SHPP GLOBAL TECH BV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Another disadvantage of conventional melt polymerization techniques is that the reaction mixture undergoes a so-called "coagulation phase" due to the formation of polyamic acid intermediates
During this reaction stage, the reactant mixture becomes very viscous and thus difficult to process
Because of these disadvantages, melt polymerization is not widely practiced commercially

Method used

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  • Method for preparing polyimide and polyimide prepared thereby
  • Method for preparing polyimide and polyimide prepared thereby
  • Method for preparing polyimide and polyimide prepared thereby

Examples

Experimental program
Comparison scheme
Effect test

preparation Embodiment 1

[0092] This example describes the preparation of a mixture of oligomers. The reaction mixture consisted of 14000 g bisphenol A dianhydride (BPADA), 2490.98 g m-phenylenediamine (mPD), 177.1 g phthalic anhydride (PA) and 30109 g o-dichlorobenzene (o-DCB). The o-DCB, BPADA, and PA were charged into a 50-gallon glass reactor, and the mixture was stirred at room temperature overnight. The mixture was then heated to 160°C under nitrogen, and molten mPD was added to the reaction mixture in increments within about 24 minutes. When water started to form in the reactor, the temperature of the reaction mixture decreased from about 157.1°C at the beginning of the mPD addition to about 146.8°C at the end. Samples of the solution mixture taken from the reactor at different times showed that the molecular weight of the oligomer (M w / M n / PDI) was 18966 / 8767 / 2.163, and 25013 / 11197 / 2.234 after about 45 minutes from the time when all mPD was added to the reactor. This solution containing oligomer...

Embodiment 1-5

[0094] The oligomer solution obtained from Preparation Example 1 and containing about 35 wt% of oligomer in o-DCB was continuously fed into the extruder from a heating tank maintained at about 165-170°C. Extruder structure and above figure 2 The similarity. The extruder is a 25mm diameter, co-rotating, intermeshing twin-screw extruder, and it includes 14 cylinders (total extruder length to diameter ratio L / D is 56) and 6 for removing Orifice for volatile components. Add the oligomer solution to the extruder at cylinder number 4. The solvent o-DCB is removed from the process through the vacuum orifices located at cylinder number 1 (orifice at the rear) and 5, 7, 9, 11 and 13 (orifices at the front). All extruder orifices work under a relatively high degree of vacuum corresponding to a pressure of about 25 mm Hg. The orifice 2 at the cylinder 5 does not have a vacuum gauge. The screw of the extruder is designed to provide a relatively long reaction residence time and frequent surfa...

preparation Embodiment 2

[0101] The reaction mixture consisted of 14050 g BPADA, 2941 g mPD, 177.1 g PA, and 30.1 kg-DCB. The amount of BPADA is 50 g more than that in Preparation Example 1, to balance the amine-rich product in that Example. The o-DCB, BPADA, and PA were charged into a 50-gallon glass reactor, and the mixture was stirred at room temperature overnight. The mixture was then heated to 160°C under nitrogen, and molten mPD was added to the reaction mixture in increments in about 36 minutes. When water started to form in the reactor, the temperature of the reaction mixture dropped from about 155.2°C at the beginning of the mPD addition to about 152.5°C at the end. Samples of the solution mixture taken from the reactor at different times showed that the molecular weight of the oligomer (M w / M n / PDI) was 25873 / 11060 / 2.339, and 28544 / 12225 / 2.335 after about 45 minutes, both of which were taken from the time when all mPD was added to the reactor. This solution containing an oligomer with a weight...

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Abstract

A method for preparing a polyimide includes introducing a mixture of an oligomer and a solvent to an extruder (80), removing solvent via at least one extruder vent (100), and melt kneading the oligomer to form a polyimide. The polyimide has a low residual solvent content. The method is faster than solution polymerization of polyimides, and it avoids the stoichiometric inaccuracies associated with reactive extrusion processes that use monomers as starting materials.

Description

Background of the invention [0001] One well-known method for preparing polyimides is solution polymerization. The method includes a first step in which a diamine compound and a dianhydride compound are reacted in a solution to form a partially polymerized polyimide, and a second step in which the polymerization is completed and the solvent is removed. This second step usually requires a residence time of the order of hours, and also needs to be in the form of a gear pump required to transport the molten polymer and an evaporation device required to remove the solvent and any water formed as a product of the polymerization reaction and imidization reaction Substantial capital investment. This method allows careful control of the ratio of diamine and dianhydride reactants, but its long residence time, high temperature, and exposure of molten polyimide to the atmosphere usually lead to degradation of polyimide and its physical properties. Performance degradation. [0002] Another wel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
CPCC08G73/1032C08G73/1028C08G73/10C08G73/00
Inventor N·西尔维M·H·贾马泰P·E·霍森F·F·扈里
Owner SHPP GLOBAL TECH BV
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