Method for removing low molecular polymers in polythioetherimide resin

A polysulfide imide resin and polymer technology, which is applied in the field of preparation of polysulfide imide resin, can solve the problem that the impact strength of the material is greatly affected, the physical and mechanical properties of the material are greatly affected, and there is no low-molecular polymerization. material and other problems to achieve the effect of improving physical and mechanical properties

Inactive Publication Date: 2019-02-01
宏威高新材料有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The applicant found that there are at least the following technical problems in the prior art: the method for synthesizing polythioetherimide by the above-mentioned nucleophilic substitution etherification reaction has the following disadvantages: that is, the molecular weight of polythioetherimide often exists during the synthesis process. In the case of a wide distribution, the molecular weight distribution width is greater than 4 in many cases. Such a wide molecular weight distribution has a greater impact on the physical and mechanical properties of the material, especially the impact strength of the material.
However, due to the different methods used in the prior art for removing low-molecular polymers from different polymer materials, polythioetherimide resins are still in the stage of technical development, and there is no method that can remove polysulfideimide resins. The method for low-molecular polymers in amine resins, based on this, the present invention proposes a method for effectively removing low-molecular polymers in polythioetherimide resins

Method used

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  • Method for removing low molecular polymers in polythioetherimide resin
  • Method for removing low molecular polymers in polythioetherimide resin
  • Method for removing low molecular polymers in polythioetherimide resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Add 200g of polythioetherimide resin A with an intrinsic viscosity of 0.35dl / g into 2000ml of reaction flask replaced with nitrogen three times, add 800ml of DMAC, start stirring and heat to 60°C until the resin is completely dissolved into a transparent solution , stop heating and keep stirring. When the temperature drops below 40°C, add toluene slowly under rapid stirring. After adding a certain amount, resin will slowly precipitate. At this time, the precipitated resin is a resin with a relatively high molecular weight. Stop adding when nearly 400ml of toluene is added. Blowing, and suction filtration. The filter cake was washed 4 times with ethanol to remove toluene and residual DMAC, washed 2 times with distilled water to remove residual ethanol, and then dried in a hot air circulation oven at 180°C for 4 hours. The intrinsic viscosity of resin A after testing was 0.38dl / g. It shows that the method of the present invention can effectively improve the molecular we...

Embodiment 2

[0056] Add 200 g of the polythioetherimide resin A with an intrinsic viscosity of 0.35 dl / g in Example 1 into a 2000 ml reaction flask replaced with nitrogen three times, then add 800 ml of DMAC, start stirring and add to 60°C until the resin is completely dissolved After forming a transparent solution, stop heating and keep stirring. When the temperature drops below 40°C, add toluene slowly under rapid stirring. After adding a certain amount, resin will slowly precipitate. The resin precipitated at this time is a resin with a relatively high molecular weight. Stop adding when 500ml of toluene is added. Blowing, and suction filtration under nitrogen protection. The filter cake was washed 4 times with ethanol to remove toluene and residual DMAC, then washed 2 times with distilled water to remove residual ethanol, and then dried in a hot air oven at 180°C. The intrinsic viscosity of the tested resin after drying was 0.36dl / g.

[0057] From the test results of Example 1 and Exa...

Embodiment 3

[0059] Add 200 g of polythioetherimide resin A with an intrinsic viscosity of 0.35 dl / g in Example 1 into a 2000 ml reaction flask replaced with nitrogen three times, add 800 ml of DMSO, start stirring and heat to 60°C until the resin is completely dissolved into After a clear solution, stop heating and keep stirring. When the temperature drops below 40°C, add toluene slowly under rapid stirring. After adding a certain amount, the resin will slowly precipitate out. At this time, the precipitated resin is a resin with a relatively high molecular weight. Stop adding when 500ml of pro-xylene is added. Blowing, and suction filtration under nitrogen protection. The filter cake was washed 4 times with ethanol to remove o-xylene and residual DMSO, then washed 2 times with distilled water to remove ethanol, and then dried in a hot air oven at 180°C. The intrinsic viscosity of the tested resin after drying was 0.39dl / g. It shows that the method of the present invention can effectivel...

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Abstract

The invention provides a method for removing low molecular polymers in polythioetherimide resin. The method comprises the following steps: adding 15-60 wt% of polythioetherimide resin powder into a reaction kettle; adding 40-95 mass% of an aprotic polar solvent into the reaction kettle subjected to nitrogen displacement; stirring a mixture obtained in the reaction kettle; cooling the mixture afterthe polythioetherimide resin is completely dissolved to form a transparent solution; slowly adding a certain amount of a non-polar solvent or a low-polarity solvent into the mixture when the temperature decreases to 40 DEG C or less, and stopping the addition of the non-polar solvent or the low-polarity solvent after a certain of resin powder is precipitated; and sampling the obtained material, filtering the sampled material, testing the filtered material, discharging the material in the reaction kettle after the molecular weight distribution reaches a target value, and performing centrifugalfiltration under the protection of nitrogen. The method effectively removes the low molecular polymers in the polythioetherimide resin, and improves the physical performances of the polythioetherimide resin.

Description

technical field [0001] The invention relates to the field of preparation methods of polythioetherimide resins, and in particular to a method for removing low-molecular polymers in polythioetherimide resins. Background technique [0002] Polythioetherimide resin is a very promising thermoplastic heat-resistant polymer material. The polythioetherimide synthesized by disubstituted phthalimide and sodium sulfide or sodium hydrosulfide or sulfur is a synthetic method that effectively reduces the manufacturing cost of polyimide, and the synthetic method is widely used in the application of polyimide have an important impetus. [0003] The applicant found that there are at least the following technical problems in the prior art: the method for synthesizing polythioetherimide by the above-mentioned nucleophilic substitution etherification reaction has the following disadvantages: that is, the molecular weight of polythioetherimide often exists during the synthesis process. In the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/0281
CPCC08G75/0281
Inventor 不公告发明人
Owner 宏威高新材料有限公司
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