Synthesis of polyamic acid resin

A polyamic acid resin and a synthesis method technology, applied in the field of resin synthesis, can solve the problems of uneven surface, uneven color, high resin viscosity, etc., and achieve the effects of simple and feasible process method, reduced thickness deviation, and improved uniformity

Active Publication Date: 2011-04-20
GUILIN ELECTRICAL EQUIP SCI RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, near the end point, the viscosity of the resin is relatively high, and the stirring effect is not good. At this time, the dianhydride material put in from the upper part is difficult to disperse in the whole system, resulting in a large difference between the viscosity of the upper layer resin and the lower layer resin in the reactor. The resin system Not uniform enough, prolonging the stirring time may improve the uniformity of the system, but it also causes the problem of low production efficiency
Uneven viscosity will affect the quality of salivation in the next process, resulting in uneven film thickness and color, uneven surface, and even visible streaks on the film surface.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Embodiment 1 of the polyamic acid resin synthesis method adopts a jacketed reaction kettle, and cooling water is passed into the jacket. From the input of dianhydride, water at 10°C is continuously poured into the jacket of the reaction kettle and stirred, and the viscosity is detected during the feeding process. When the viscosity reaches 70,000 centipoise, the addition of dianhydride is stopped, and the stabilizer triphenyl phosphite is added. Ester, add-on is 0.1% of resin gross weight in the reactor, at this moment in the jacket of reactor, pass into the hot water of 45 ℃, the temperature of resin system rises to 60 ℃ after insulation and continue to stir for 5 hours. Obtaining the resin I that the viscosity is 60,000 centipoises at last is standby for the next operation.

Embodiment 2

[0011] The polyamic acid resin synthesis method embodiment 2 is similar to the method of embodiment 1, but the heating temperature is different. Starting from putting dianhydride into the reactor, water at 15°C is continuously poured into the jacket of the reactor and stirred. Viscosity detection is carried out during the feeding process. When the viscosity reaches 70,000 centipoise, stop adding dianhydride and add a stabilizer. Triphenyl phosphite, the addition amount is 0.3% of the total weight of the resin in the reactor. At this time, water at 50°C is introduced into the jacket of the reactor, and the temperature of the resin system rises to 65°C. Stir for 4 hours. Obtaining the resin II with a viscosity of 50,000 centipoise at last is standby for the next process.

Embodiment 3

[0013] The polyamic acid resin synthesis method embodiment 3 is similar to the method of embodiment 1, but the heating temperature is different. Starting from putting dianhydride into the reactor, water at 20°C is continuously poured into the jacket of the reactor and stirred. Viscosity detection is carried out during the feeding process. When the viscosity reaches 65,000 centipoise, stop adding dianhydride and add a stabilizer. Triphenyl phosphite, the addition is 0.2% of the total weight of the resin in the reactor. At this time, 55°C hot water is introduced into the jacket of the reactor, and the temperature of the resin system rises to 70°C. Stirring was continued for 3 hours. Obtaining the resin III with a viscosity of 45,000 centipoises at last is standby for the next process.

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PUM

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Abstract

The invention discloses a synthesis method of polyamide acid resin. Water is inlet into a jacket of a reaction kettle. As dianhydride is input, the water of 10 DEG C to 30 DEG C is inlet into the jacket continuously and is stirred. After the viscosity of the resin reaches 60,000 centipoises to 70,000 centipoises, the addition of dianhydride is ceased, but hot water of 45 DEG C to 55 DEG C is inlet into the jacket to control the temperature of resin system at 60 DEG C to 70 DEG C, and after a preset temperature is reached, temperature is preserved and stirring is carried out continuously for 2hours to 5 hours. The optimum proposal is that the temperature of the resin system is controlled at 65 DEG C to 70 DEG C and the temperature-preservation stirring time is 3 hours to 4 hours. In orderto prevent from degradation, after the addition of dianhydride is ceased, triphenyl phosphate, a stabilizer, is added, with the addition amount equaling to 0.1 percent to 0.5 percent of the total weight of the resin system. The synthesis method ensures sufficient plasticization of the resin within quite a short time, improves the homogeneity of the system and facilitates the processing of postprocess; and the synthesis method is simple and feasible and increases quite little cost of equipment. Membranes produced by the resin obtained through the synthesis method are unchanged in main performance indexes, even in thickness, consistent in color and smooth in surface.

Description

(1) Technical field [0001] The invention relates to the technical field of resin synthesis, in particular to a synthesis method of polyamic acid resin. (2) Background technology [0002] The traditional method of synthesizing polyamic acid resin is to use a jacketed reaction kettle, and the heat exchange medium water at 10°C to 30°C is passed into the jacket to cool the reaction kettle. This is because the reaction of forming polyamic acid is an exothermic reaction. , lowering the temperature of the reactor during the synthesis process can make the polyamic acid produced reach a high molecular weight and ensure that the final polyamic acid meets a certain viscosity requirement. When various raw materials are added into the reactor and the viscosity is tested to meet the requirements, the synthesis process is generally completed by continuing to stir for 4 to 6 hours. However, near the end point, the viscosity of the resin is relatively high, and the stirring effect is not g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10
Inventor 李耀星张俊丽
Owner GUILIN ELECTRICAL EQUIP SCI RES INST
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