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A kind of production method of low-cost polyimide molding powder

A polyimide and production method technology, which is applied in the direction of organic chemistry, condensation between hydrocarbons and non-hydrocarbons to produce hydrocarbons, etc. The effect of reducing the cost of post-processing procedures, improving thermal stability, and widening market space

Active Publication Date: 2020-06-09
潍坊弘润新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The wastewater contains a large amount of ethanol or methanol or acetone, unreacted raw materials in the reaction system (such as diamine, dianhydride, entrainer, end-capping agent, etc.) The composition is more complicated
If the detergents such as ethanol, methanol or acetone in the wastewater are recovered, due to the complex composition of the wastewater, it is difficult to separate and obtain pure ethanol, methanol or propanol, and it is difficult to recycle them as detergents
Moreover, the components of wastewater are complex, and it is difficult to separate and recycle each component one by one. Therefore, it will not only consume a lot of manpower, material resources, and financial resources to treat these wastewater, but also inevitably waste energy.
Therefore, the traditional washing method has the problems of difficult wastewater treatment, waste of energy and high treatment cost.
[0005] In addition, the thermal stability of traditional polyimide molding powder is not good. For example, the 5% thermal weight loss temperature is generally below 550°C, and it is difficult to reach 560°C or above, which restricts the use of polyimide in certain high-temperature environments. Applications
[0006] To sum up, polyimide molding powders in the prior art have problems of high cost of use, poor thermal stability, large amount of waste water generated during post-preparation and post-processing costs, and there is still a lack of effective solutions

Method used

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  • A kind of production method of low-cost polyimide molding powder
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Alkylation reaction of 1L methanol and 1L toluene at 400°C in the presence of nanometer ZSM-5 molecular sieve catalysts to obtain xylene, trimethylbenzene, tetramethylbenzene, etc., followed by de-xylene tower and de-trimethylbenzene tower to obtain tetramethylbenzene At the same time, the xylene and trimethylbenzene recycled from the xylene removal tower and the trimethylbenzene tower are re-alkylated to obtain durene.

[0046]500g of durene is reacted with oxygen under catalyst conditions. During the reaction, the recovered waste gas generated during the reaction is mixed with oxygen, and then recycled into the catalytic oxidation reaction device to finally obtain pyromellitic dianhydride.

[0047] 200g of p-phenylenediamine was dissolved in 2000ml of N,N-dimethylformamide organic solvent, nitrogen gas was continuously passed through, and stirred for 2 hours. Add 250g of PMDA to the above solution in batches, the interval between each addition is 1 hour, and react at ...

Embodiment 2

[0051] 1.5L of methanol and 1.2L of toluene are alkylated at 450°C in the presence of nanometer ZSM-5 molecular sieve catalysts to obtain xylene, trimethylbenzene, tetramethylbenzene, etc., and then pass through the de-xylene tower and the de-trimethylbenzene tower, Tetramethylbenzene is obtained, and at the same time, the xylene and trimethylbenzene recycled from the xylene removal tower and the trimethylbenzene tower are re-alkylated to obtain durene.

[0052] 600g of durene reacts with oxygen under catalyst conditions. During the reaction, the waste gas generated is mixed with oxygen and then recycled into the reaction device to finally obtain pyromellitic dianhydride.

[0053] 400g of m-phenylenediamine was dissolved in 4000ml of N,N-dimethylformamide as a solvent, nitrogen gas was continuously passed through, and stirred for 2 hours. Add 300g of PMDA to the above solution in batches, the interval between each addition is 1 hour, and react at room temperature for 3 hours a...

Embodiment 3

[0058] In the presence of a catalyst, 2L of methanol and 2.1L of toluene are alkylated at high temperature to obtain xylene, trimethylbenzene, tetramethylbenzene, etc., which are successively passed through the de-xylene tower and the de-trimethylbenzene tower to obtain tetramethylbenzene. The xylene and trimethylbenzene recycled from the toluene tower and the trimethylbenzene tower are re-alkylated to obtain durene.

[0059] 800g of durene reacts with oxygen under catalyst conditions. During the reaction, the waste gas generated is mixed with oxygen and then recycled into the reaction device to finally obtain pyromellitic dianhydride.

[0060] Dissolve 600g of 4,4'-diaminodiphenylether in 5000ml of N,N-dimethylacetamide solvent, continuously feed nitrogen, and stir for 2 hours. Add 550g of PMDA to the above solution in batches, the interval between each addition is 1 hour, and react at room temperature for 3 hours after adding. Add 80 g of phthalic dianhydride to the above s...

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Abstract

The invention discloses a low-cost polyimide molding powder production chain which includes the steps: 1) performing alkylation reaction on methanol and methylbenzene under the action of a catalyst toobtain dimethylbenzene, trimethylbenzene and tetramethylbenzene, recycling the dimethylbenzene and the trimethylbenzene and performing alkylation reaction on the dimethylbenzene, the trimethylbenzeneand the methanol again; 2) performing reaction on durene and oxygen under the action of the catalyst to prepare pyromellitic acid dianhydride, recycling waste gas generated in the reaction process and then performing catalytic reaction on the waste gas and the oxygen again; 3) dissolving the prepared pyromellitic acid dianhydride and aromatic diamine in an organic solvent to prepare polyimide molding powder suspension liquid under the action of an end-capping reagent and an entrainer, and washing polyimide molding powder filter cakes by the organic solvent during filtration. The methanol serves as the most basic raw material, the raw material cost of polyimide molding powder is greatly reduced, and the production chain has a wide market space.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a low-cost polyimide molding powder production chain. Background technique [0002] Polyimide (PI) is a kind of polymer material formed by dianhydride and diamine, and the main chain contains imide ring. It is a class of high-performance polymer materials with excellent thermal stability, chemical stability, dielectric properties and mechanical properties. It plays a very important role in the aerospace industry, automobiles, microelectronics and other fields. Specific application examples are aircraft engine parts, aircraft wear pads, automatic transmission bearings, seal rings, material processing equipment parts, and shaft seals. [0003] With the rapid development of high technology, the demand for polyimide in various industries is increasing. However, the conversion rate in the production of polyimide raw material dianhydride and diamine is low, which makes the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C07C2/88C07C15/02C07D493/04
CPCC07C2/88C07D493/04C08G73/1014C08G73/1067C08G73/1071C07C15/02
Inventor 曲延涛
Owner 潍坊弘润新材料有限公司