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Low-temperature stable storage method for polyamide acid glue liquid as well as refrigerating liquid composition

A polyamic acid glue solution and a storage method technology are applied in the field of high molecular weight polyamic acid stable storage method and ethylene glycol type freezing liquid composition, polyamic acid low temperature stable storage method and freezing liquid composition field, which can solve difficult problems. problems such as burning, safety production hidden dangers, equipment safety monitoring and management and maintenance costs increase, etc., to achieve the effects of low foam tendency, long stabilization time, and not easy to degrade and deteriorate.

Active Publication Date: 2013-06-19
HUAWEI POLYIMIDE +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among all kinds of frozen brine and freezing liquid, calcium chloride aqueous solution is widely used in various refrigerators and equipment and occasions that need to lower the freezing point due to its low freezing point, no pollution to the environment, non-flammability, and low price. Industrial calcium chloride aqueous solution is corrosive to reactors and pipelines, so it will pose a certain hidden danger to safe production, which will increase equipment safety monitoring and management and maintenance costs

Method used

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  • Low-temperature stable storage method for polyamide acid glue liquid as well as refrigerating liquid composition
  • Low-temperature stable storage method for polyamide acid glue liquid as well as refrigerating liquid composition
  • Low-temperature stable storage method for polyamide acid glue liquid as well as refrigerating liquid composition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Add 8 kg of isoquinoline or 1.3 kg of octaploid hydrogen-containing siloxane to a storage tank containing 1000 kg of high molecular weight polyamic acid solution with a viscosity of 245,100 centipoise. The temperature of the polyamic acid solution in the storage tank is -15°C. Use a high-speed disperser to disperse and stir at 2200-2500 rpm for 120s, filter and vacuum defoam, and pump it into a heat-insulated hollow jacketed low-temperature storage tank for storage at -20°C. In the jacket, the ethylene glycol refrigerant of formula 1 is used for refrigeration and insulation. The specific weight percentages of each component of the refrigerant are: demineralized water 60.015%, ethylene glycol 34%, 2-ethylhexanoic acid 4%, ethylenediamine Tetramethylene phosphonic acid 0.3%, benzotriazole 0.4%, molybdate 0.3%, sodium benzoate 0.035%, hydroxyethylene diphosphonic acid 0.3%, polyaminopolyether phosphate 0.35%, hydrolyzed maleic acid Anhydride 0.3%.

Embodiment 2

[0057] Add 13 kg of isoquinoline or 0.8 kg of octaploid hydrogen-containing siloxane to a storage tank containing 1000 kg of high-molecular-weight polyamic acid solution with a viscosity of 236,000 centipoise. The temperature of the polyamic acid solution in the storage tank is -20°C. Use a high-speed disperser at 2200-2500 rpm to disperse and stir for 60 seconds, filter and vacuum defoam, and then pump it into a heat-insulated hollow jacketed low-temperature storage tank for storage at -15°C. The jacket is refrigerated and insulated with the ethylene glycol refrigerant of Formula 2. The specific weight percentages of each component of the refrigerant are: demineralized water 66.4%, ethylene glycol 29%, vanillin 0.75%, furfural 0.75%, hexamethylene 0.2% tetramine, 0.25% methyl benzotriazole, 0.55% S-carboxyethyl thiosuccinic acid, 1.1% polyacrylic acid, 0.9% polyepoxy succinic acid, 2-phosphonic acid butane-1, 2,4-Tricarboxylic acid 0.1%.

Embodiment 3

[0059] Add 10 kg of isoquinoline or 1 kg of octaploid hydrogen-containing siloxane to a storage tank containing 1000 kg of high-molecular-weight polyamic acid solution with a viscosity of 218,700 centipoise. The temperature of the polyamic acid solution in the storage tank is -25 ° C. Use Disperse and stir at 2200-2500 rpm for 100 seconds with a high-speed disperser. After filtration and vacuum defoaming, pump it into a heat-insulated hollow jacketed low-temperature storage tank for storage at -25°C. The jacket is refrigerated and insulated with the ethylene glycol refrigerant of Formula 1. The specific weight percentages of each component of the refrigerant are: demineralized water 58.015%, ethylene glycol 36%, 2-ethylhexanoic acid 4%, ethylenediamine Tetramethylene phosphonic acid 0.3%, benzotriazole 0.4%, molybdate 0.3%, sodium benzoate 0.035%, hydroxyethylene diphosphonic acid 0.3%, polyaminopolyether phosphate 0.35%, hydrolyzed maleic acid Anhydride 0.3%.

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Abstract

The invention discloses a low-temperature stable storage method for polyamide acid glue liquid as well as a refrigerating liquid composition. The stable storage method for high-molecular-weight polyamide acid comprises the steps of: adding 0.8-1.3 wt% of isoquinoline and 0.08-0.13 wt% of octaploid hydrogen-containing siloxane into polyamide acid solution, lowering the temperature of the polyamide acid solution to be below 0 DEG C, stirring by utilizing a high-speed dispersion machine in a revolution of 2200-2500 revolutions per minute for 60-120 seconds, pressing the solution into a low-temperature storage tank to be stored after carrying out filtering and vacuum defoamation, and controlling the storage temperature of the storage tank at (-20)-(-5) DEG C by utilizing an ethylene glycol refrigerating liquid composition. According to the preparation method disclosed by the invention, during the storage and the use of the polyamide acid in an industrial production process of polyimide films, the low-temperature storage period is long, the time is controllable, the amidation reaction is avoided in the storage period, and the imidization can be fast carried out under an elevated temperature condition, the performance of the obtained film is relatively improved compared with the performance of the film subjected to thermal amidation, and the cost is lowered.

Description

technical field [0001] The invention relates to a low-temperature stable storage method for polyamic acid and a freezing liquid composition, in particular to a stable storage method for high-molecular-weight polyamic acid and an ethylene glycol-type freezing liquid composition, and belongs to the field of polymer material processing. Background technique [0002] Polyamic acid solution is a prepolymer for industrial production of polyimide, usually synthesized with dianhydride and diamine. The reaction between dianhydride and diamine is an exothermic reaction, and the reaction is reversible, so low temperature is conducive to the positive direction of the reaction. On the other hand, in the industrial production of polyimide films, since the synthesis of polyamic acid is discontinuous, and the industrial film production line must be in continuous operation, how to store polyamic acid glue in a long-term and stable manner has become an urgent problem. The problem. At the sa...

Claims

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Application Information

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IPC IPC(8): C08J3/205C08L79/08C08K5/3437C08K5/5435C09K5/10
Inventor 黄渝鸿袁萍李晓敏邢涛黄樯
Owner HUAWEI POLYIMIDE
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