CN103013114B

CN103013114B - Method for preparing waterproof polyimide thin film

Info

Publication number: CN103013114B
Application number: CN201210528016.0A
Authority: CN
Inventors: 岑建军
Original assignee: NINGBO JINSHAN NEW MATERIAL CO Ltd
Current assignee: NINGBO JINSHAN NEW MATERIAL CO Ltd
Priority date: 2012-12-05
Filing date: 2012-12-05
Publication date: 2015-02-18
Anticipated expiration: 2032-12-05
Also published as: CN103013114A

Abstract

The invention discloses a method for preparing a waterproof polyimide thin film. The method comprises the following steps: using nanoscale polytetrafluoroethylene powder and polyamide acid, wherein the mixture of nanoscale polytetrafluoroethylene powder is 3 to 10% of polyamide acid; and during synthesis, synthesizing pyromellitic dianhydride and 4,4'-diaminodiphenyl ether to obtain polyamide acid, wherein in the synthesis process, the calculated 4,4'-diaminodiphenyl ether is placed in a reaction kettle first, and then 90 to 95% of the calculated required total quantity of pyromellitic dianhydride is added in the reaction kettle to synthesize with 4,4'-diaminodiphenyl ether; and utilizing the remaining 5 to 10% of pyromellitic dianhydride to control the viscosity of the final resultant within 90,000 plus/minus 5,000 CP to finish the whole preparation after defoaming, salivation, and film formation. The obtained waterproof polyimide thin film prolongs the service life of a motor in the humid environment and has the functions of isolation and water resistance in a relatively high humidity or water environment.

Description

The preparation method of waterproof polyimide thin film

Technical field

The present invention relates to a kind of preparation method of waterproof polyimide thin film.

Background technology

Petroleum Industry has very few development prospect and wireless business opportunity potentiality as one of key pillars of the national economy.The own feature of petroleum industry itself is large flux, operates continuously at full capacity, high to the requirement of the reliability and stability of oil-immersed pump motor device.What current oil-immersed pump motor material adopted is common Kapton, because its water-absorbent is high, causes decreasing insulating, often occurs oil-immersed pump in operational process by the situation of burning, production process is interrupted, causes a large amount of financial losses.The extensive concern that the technical problem of its isolation protective material is appointed for a long time.

Therefore, being badly in need of exploitation one can reduce water-absorbent, has good thermotolerance and the Kapton of processing characteristics simultaneously, uses under enabling motor be adapted at the environment such as moist severe.

Summary of the invention

The object of the invention is to provide one can in high relative humidity and water under environment to solve above-mentioned the deficiencies in the prior art, playing the preparation method of waterproof polyimide thin film of insulation, waterproof action.

To achieve these goals, the preparation method of a kind of waterproof polyimide thin film provided by the invention, comprise and adopt nano level polytetrafluoroethylpowder powder and polyamic acid, it is characterized in that described polyamic acid is by pyromellitic acid anhydride and 4, 4'-diaminodiphenyl oxide is being equipped with as providing 4 of reaction environment, obtained polyamic acid is synthesized in the reactor of 4 '-N,N-DIMETHYLACETAMIDE, by the weighing scale of polyamic acid, 4, 4 '-N,N-DIMETHYLACETAMIDE weight ratio accounted in polyamic acid is 70%-90%, described nano level polytetrafluoroethylpowder powder selects Du Pont Zonyl Mp, Zonyl 1200, the mixture of Zonyl 1,500 three kinds of models, the weight part of nano level polytetrafluoroethylpowder powder mixture consists of: Du Pont Zonyl Mp:10 part-40 parts, Du Pont Zonyl 1200:20 part-50 parts, Du Pont Zonyl 1500:20 part-60 parts, nano level polytetrafluoroethylpowder powder mixture accounts for the 3%-10% of polyamic acid gross weight, during synthesis, first to pyromellitic acid anhydride and 4,4'-diaminodiphenyl oxide calculates reacting weight required separately by equimolar ratio, and synthesis obtains polyamic acid, in its building-up process, first 4,4'-diaminodiphenyl oxides needed for calculating are placed in reactor, and then add the 90%-95% calculating required pyromellitic acid anhydride total amount and join in reactor and carry out building-up reactions with 4,4'-diaminodiphenyl oxide, grinding is needed after the mixing of nano level polytetrafluoroethylpowder powder mixture, and make diameter of particle reach D90 < 3um, the nano level polytetrafluoroethylpowder powder mixture after grinding is added according to the above ratio in polyamic acid after the reaction, and then when adding building-up reactions, not yet add the pyromellitic acid anhydride of remaining 5%-10%, 90000 ± 5000CP is reached, then deaeration salivation film forming with the viscosity controlling final reaction resultant.

The weight proportioning components of described nano level tetrafluoroethylene (PTFE) powder mixture is Du Pont ZonylMp:30 part, Du Pont Zonyl 1200:40 part, Du Pont Zonyl 1500:30 part.

With pyromellitic acid anhydride (PMDA) and 4, in the building-up process of 4'-diaminodiphenyl oxide (ODA) synthesizing polyamides acid (PAA), adopt 4,4 '-N,N-DIMETHYLACETAMIDE (DMAC) is as the middle envrionment conditions of reaction.

By a kind of waterproof polyimide thin film that preparation method of the present invention obtains, its advantage is: water-intake rate is lower, reach≤0.1%, extend electrical machine insulation working life in wet environment, to can be applicable in high relative humidity or water in environment, play the effects such as insulation, waterproof, as in the field such as water pump, oil pump.And there is easy processing, the characteristic keeping polyimide itself good can be had simultaneously.

Embodiment

Below by embodiment, the present invention is further described.

Embodiment 1:

The preparation method of a kind of waterproof polyimide thin film that the present embodiment describes, comprise and adopt nano level polytetrafluoroethylpowder powder and polyamic acid, described polyamic acid is by pyromellitic acid anhydride and 4, 4'-diaminodiphenyl oxide is being equipped with as providing 4 of reaction environment, obtained polyamic acid is synthesized in the reactor of 4 '-N,N-DIMETHYLACETAMIDE, by the weighing scale of polyamic acid, 4, 4 '-N,N-DIMETHYLACETAMIDE weight ratio accounted in polyamic acid is 70%-90%, described nano level polytetrafluoroethylpowder powder selects Du Pont Zonyl Mp, Zonyl1200, the mixture of Zonyl 1,500 three kinds of models, the weight part of nano level polytetrafluoroethylpowder powder mixture consists of: Du Pont Zonyl Mp:30 part, Du Pont Zonyl 1200:35 part, Du Pont Zonyl 1500:40 part, nano level polytetrafluoroethylpowder powder mixture accounts for 3% of polyamic acid gross weight, during synthesis, first to pyromellitic acid anhydride and 4,4'-diaminodiphenyl oxide calculates reacting weight required separately by equimolar ratio, and synthesis obtains polyamic acid, in its building-up process, first 4,4'-diaminodiphenyl oxides needed for calculating are placed in reactor, and then add and calculate 90% of required pyromellitic acid anhydride total amount and join in reactor and carry out building-up reactions with 4,4'-diaminodiphenyl oxide, grinding is needed after the mixing of nano level polytetrafluoroethylpowder powder mixture, and make diameter of particle reach D90 < 3um, the nano level polytetrafluoroethylpowder powder mixture after grinding is added according to the above ratio in polyamic acid after the reaction, and then when adding building-up reactions, not yet add remaining pyromellitic acid anhydride, 90000 ± 5000CP is reached, then deaeration salivation film forming with the viscosity controlling final reaction resultant.

After tested, performance index as shown in table 1 below are reached.

Table 1:

By the waterproof polyimide thin film that the present embodiment method obtains, its advantage is: water-intake rate is lower, reach≤0.1%, extend electrical machine insulation working life in wet environment, easily process, the characteristic keeping polyimide itself good can be had simultaneously.To can be applicable in high relative humidity or water in environment, play the effects such as insulation, waterproof, as in the field such as water pump, oil pump.

Embodiment 2:

The preparation method of a kind of waterproof polyimide thin film that the present embodiment provides, the weight part of nano level polytetrafluoroethylpowder powder mixture consists of: Du Pont Zonyl Mp:40 part, Du Pont Zonyl 1200:50 part, Du Pont Zonyl 1500:60 part, and nano level polytetrafluoroethylpowder powder mixture accounts for 6% of polyamic acid total amount; In polyamic acid (PAA) building-up process, pyromellitic acid anhydride (PMDA) add-on is calculate total amount 95%.After tested, performance index as shown in table 2 below can be reached:

Table 2:

Embodiment 3:

The preparation method of a kind of waterproof polyimide thin film that the present embodiment provides, the weight part of nano level polytetrafluoroethylpowder powder mixture consists of: Du Pont Zonyl Mp:10 part, Du Pont Zonyl 1200:20 part, Du Pont Zonyl 1500:20 part, and nano level polytetrafluoroethylpowder powder mixture accounts for 10% of polyamic acid total amount; In polyamic acid (PAA) building-up process, pyromellitic acid anhydride (PMDA) add-on reaches 93%.After tested, performance index as shown in table 3 below can be reached.

Table 3:

Claims

1. the preparation method of a waterproof polyimide thin film, comprise and adopt nano level polytetrafluoroethylpowder powder and polyamic acid, it is characterized in that described polyamic acid is by pyromellitic acid anhydride and 4, 4'-diaminodiphenyl oxide is being equipped with as providing 4 of reaction environment, obtained polyamic acid is synthesized in the reactor of 4 '-N,N-DIMETHYLACETAMIDE, by the weighing scale of polyamic acid, 4, 4 '-N,N-DIMETHYLACETAMIDE weight ratio accounted in polyamic acid is 70%-90%, described nano level polytetrafluoroethylpowder powder selects Du Pont Zonyl Mp, Zonyl 1200, the mixture of Zonyl 1,500 three kinds of models, the weight part of nano level polytetrafluoroethylpowder powder mixture consists of: Du Pont Zonyl Mp:10 part-40 parts, Du Pont Zonyl 1200:20 part-50 parts, Du Pont Zonyl 1500:20 part-60 parts, nano level polytetrafluoroethylpowder powder mixture accounts for the 3%-10% of polyamic acid gross weight, during synthesis, first to pyromellitic acid anhydride and 4,4'-diaminodiphenyl oxide calculates reacting weight required separately by equimolar ratio, and synthesis obtains polyamic acid, in its building-up process, first 4,4'-diaminodiphenyl oxides needed for calculating are placed in reactor, and then add the 90%-95% calculating required pyromellitic acid anhydride total amount and join in reactor and carry out building-up reactions with 4,4'-diaminodiphenyl oxide, grinding is needed after the mixing of nano level polytetrafluoroethylpowder powder mixture, and make diameter of particle reach D90 < 3um, the nano level polytetrafluoroethylpowder powder mixture after grinding is added according to the above ratio in polyamic acid after the reaction, and then when adding building-up reactions, not yet add the pyromellitic acid anhydride of remaining 5%-10%, 90000 ± 5000CP is reached, then deaeration salivation film forming with the viscosity controlling final reaction resultant.

2., according to the preparation method of a kind of waterproof polyimide thin film described in claim 1, it is characterized in that the weight proportioning components of described nano level polytetrafluoroethylpowder powder mixture is Du Pont Zonyl Mp:30 part, Du Pont Zonyl 1200:40 part, Du Pont Zonyl 1500:30 part.