CN103013114A

CN103013114A - Method for preparing waterproof polyimide thin film

Info

Publication number: CN103013114A
Application number: CN2012105280160A
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: 2013-04-03
Anticipated expiration: 2032-12-05
Also published as: CN103013114B

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 water tolerance Kapton

Technical field

The present invention relates to a kind of preparation method of water tolerance Kapton.

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 characteristics of petroleum industry itself are large flux, continuous operation at full capacity, to the reliability and stability of oil-immersed pump motor device require high.What the oil-immersed pump motor material adopted at present is common Kapton, because its water-absorbent is high, causes decreasing insulating, the situation that oil-immersed pump is burnt in operational process often occurs, so that 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, the urgent need exploitation is a kind of can to reduce water-absorbent, has simultaneously good thermotolerance and the Kapton of processing characteristics, makes motor can be adapted at moist abominable the grade under the environment and uses.

Summary of the invention

The objective of the invention is to provide a kind of in order to solve above-mentioned the deficiencies in the prior art and can in relative high humidity and water under the environment, play the preparation method of the water tolerance Kapton of insulation, waterproof action.

To achieve these goals, the preparation method of a kind of water tolerance Kapton 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 4 of reaction environment is provided, synthetic resulting polyamic acid in the reactor of 4 '-N,N-DIMETHYLACETAMIDE, press the weighing scale of polyamic acid, 4, the weight ratio that 4 '-N,N-DIMETHYLACETAMIDE accounts in the polyamic acid is 70%-90%, described nano level polytetrafluoroethylpowder powder is to select the Zongyl Mp of Du Pont, Zongyl 1200, the mixture of 1,500 three kinds of models of Zongyl, the weight part of nano level polytetrafluoroethylpowder powder mixture consists of: the Zongyl Mp:10 of Du Pont part-40 part, the Zongyl 1200:20 of Du Pont part-50 part, the Zongyl 1500:20 of Du Pont part-60 part, nano level polytetrafluoroethylpowder powder mixture accounts for the 3%-10% of polyamic acid gross weight; When synthetic, at first to pyromellitic acid anhydride and 4,4 '-diaminodiphenyl oxide calculates required separately reacting weight by equimolar ratio, and the synthetic polyamic acid that obtains, in its building-up process, will calculate first requiredly 4,4 '-diaminodiphenyl oxide places reactor, and then the 90%-95% that add to calculate required pyromellitic acid anhydride total amount joins in the reactor with 4, and 4 '-diaminodiphenyl oxide carries out building-up reactions; After mixing, nano level polytetrafluoroethylpowder powder mixture needs to grind, and make diameter of particle reach D90＜3um, in reacted polyamic acid, add according to the above ratio the nano level polytetrafluoroethylpowder powder mixture after grinding, and then not yet add the pyromellitic acid anhydride of remaining 5%-10% when adding building-up reactions, viscosity with control final reaction resultant reaches 90000 ± 5000CP, and then deaeration salivation film forming gets final product.

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

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.

A kind of water tolerance Kapton that obtains by preparation method of the present invention, its advantage is: water-intake rate is lower, reach≤0.1%, prolongation is the electrical machine insulation working life in wet environment, can be applicable in relative high humidity or the water in the environment, play the effects such as insulation, waterproof, in the fields such as water pump, oil pump.And have easy processing, can have the good characteristic of the polyimide of maintenance itself simultaneously.

Embodiment

The present invention is further described below by embodiment.

Embodiment 1:

The preparation method of a kind of water tolerance Kapton that the present embodiment is described, 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 4 of reaction environment is provided, synthetic resulting polyamic acid in the reactor of 4 '-N,N-DIMETHYLACETAMIDE, press the weighing scale of polyamic acid, 4, the weight ratio that 4 '-N,N-DIMETHYLACETAMIDE accounts in the polyamic acid is 70%-90%, described nano level polytetrafluoroethylpowder powder is to select the Zongyl Mp of Du Pont, Zongyl 1200, the mixture of 1,500 three kinds of models of Zongyl, the weight part of nano level polytetrafluoroethylpowder powder mixture consists of: the Zongyl Mp:30 of Du Pont part, the Zongyl 1200:35 of Du Pont part, the Zongyl 1500:40 of Du Pont part, nano level polytetrafluoroethylpowder powder mixture accounts for 3% of polyamic acid gross weight; When synthetic, at first to pyromellitic acid anhydride and 4,4 '-diaminodiphenyl oxide calculates required separately reacting weight by equimolar ratio, and the synthetic polyamic acid that obtains, in its building-up process, will calculate first requiredly 4,4 '-diaminodiphenyl oxide places reactor, and then add to calculate 90% of required pyromellitic acid anhydride total amount and join in the reactor with 4,4 '-diaminodiphenyl oxide carries out building-up reactions; After mixing, nano level polytetrafluoroethylpowder powder mixture needs to grind, and make diameter of particle reach D90＜3um, in reacted polyamic acid, add according to the above ratio the nano level polytetrafluoroethylpowder powder mixture after grinding, and then not yet add remaining pyromellitic acid anhydride when adding building-up reactions, viscosity with control final reaction resultant reaches 90000 ± 5000CP, and then deaeration salivation film forming gets final product.

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

Table 1:

By the water tolerance Kapton that the present embodiment method obtains, its advantage is: water-intake rate is lower, reach≤0.1%, prolonging electrical machine insulation working life in wet environment, easily processing can have the good characteristic of the polyimide of maintenance itself simultaneously.Can be applicable in relative high humidity or the water in the environment, play the effects such as insulation, waterproof, in the fields such as water pump, oil pump.

Embodiment 2:

The preparation method of a kind of water tolerance Kapton that the present embodiment provides, the weight part of nano level polytetrafluoroethylpowder powder mixture consists of: the Zongyl Mp:40 of Du Pont part, the Zongyl 1200:50 of Du Pont part, the Zongyl 1500:60 of Du Pont 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 for calculating 95% of total amount.After tested, can reach performance index as shown in table 2 below:

Table 2:

Embodiment 3:

The preparation method of a kind of water tolerance Kapton that the present embodiment provides, the weight part of nano level polytetrafluoroethylpowder powder mixture consists of: the Zongyl Mp:10 of Du Pont part, the Zongyl 1200:20 of Du Pont part, the Zongyl 1500:20 of Du Pont 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, can reach performance index as shown in table 3 below.

Table 3:

Claims

1. the preparation method of a water tolerance Kapton, 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 4 of reaction environment is provided, synthetic resulting polyamic acid in the reactor of 4 '-N,N-DIMETHYLACETAMIDE, press the weighing scale of polyamic acid, 4, the weight ratio that 4 '-N,N-DIMETHYLACETAMIDE accounts in the polyamic acid is 70%-90%, described nano level polytetrafluoroethylpowder powder is to select the Zongyl Mp of Du Pont, Zongyl 1200, the mixture of 1,500 three kinds of models of Zongyl, the weight part of nano level polytetrafluoroethylpowder powder mixture consists of: the Zongyl Mp:10 of Du Pont part-40 part, the Zongyl1200:20 of Du Pont part-50 part, the Zongyl 1500:20 of Du Pont part-60 part, nano level polytetrafluoroethylpowder powder mixture accounts for the 3%-10% of polyamic acid gross weight; When synthetic, at first to pyromellitic acid anhydride and 4,4 '-diaminodiphenyl oxide calculates required separately reacting weight by equimolar ratio, and the synthetic polyamic acid that obtains, in its building-up process, will calculate first requiredly 4,4 '-diaminodiphenyl oxide places reactor, and then the 90%-95% that add to calculate required pyromellitic acid anhydride total amount joins in the reactor with 4, and 4 '-diaminodiphenyl oxide carries out building-up reactions; After mixing, nano level polytetrafluoroethylpowder powder mixture needs to grind, and make diameter of particle reach D90＜3um, in reacted polyamic acid, add according to the above ratio the nano level polytetrafluoroethylpowder powder mixture after grinding, and then not yet add the pyromellitic acid anhydride of remaining 5%-10% when adding building-up reactions, viscosity with control final reaction resultant reaches 90000 ± 5000CP, and then deaeration salivation film forming gets final product.

2. the preparation method of a kind of water tolerance Kapton according to claim 1, the weight proportioning components that it is characterized in that described nano level polytetrafluoroethylpowder powder mixture is the Zongyl Mp:30 of Du Pont part, 1200: 40 parts of the Zongyl of Du Pont, 1500: 30 parts of the Zongyl of Du Pont.