CN108822319A - Inverter fed motor porous aluminas/Kapton and preparation method thereof - Google Patents
Inverter fed motor porous aluminas/Kapton and preparation method thereof Download PDFInfo
- Publication number
- CN108822319A CN108822319A CN201810704456.4A CN201810704456A CN108822319A CN 108822319 A CN108822319 A CN 108822319A CN 201810704456 A CN201810704456 A CN 201810704456A CN 108822319 A CN108822319 A CN 108822319A
- Authority
- CN
- China
- Prior art keywords
- kapton
- film
- fed motor
- inverter fed
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1046—Polyimides containing oxygen in the form of ether bonds in the main chain
- C08G73/105—Polyimides containing oxygen in the form of ether bonds in the main chain with oxygen only in the diamino moiety
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
- C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Laminated Bodies (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to a kind of Inverter fed motor porous aluminas/Kaptons and preparation method thereof, and it includes following steps：Alumina precursor is prepared using triethanolamine, aluminium isopropoxide prehydrolysis, the alumina precursor is added in KH550 silane coupler solution, forms aluminum oxide precursor precursor emulsion；(3) pyromellitic acid anhydride is added by lotion and containing amine aqueous solution, is fabricated to polyamic acid resin, obtained polyamic acid resin forms film by casting technique, and heating obtains Inverter fed motor porous aluminas/Kapton.The dielectric properties and corona-resistance property for the film that the present invention obtains are greatly improved, and improve to the service life for extending film and are also greatly improved.
Description
Technical field
The present invention relates to inorganic and organic composite material synthesis fields, more particularly to a kind of system of Kapton
Preparation Method, more particularly, to a kind of preparation method of porous aluminas/Kapton.
Background technique
Polyimides (PI) film has good heat resistance, mechanical performance, electric property and radiation resistance, in electricity
The fields such as sub- industrial circle and aerospace play highly important effect.However the corona-resistance property of common PI film compared with
Difference is no longer satisfied the requirement on the special electrical equipment such as high-voltage generator, high-pressure engine, variable-frequency motor.
In order to solve the deficiency in terms of PI film corona-resistance property, DuPont Corporation released one after another at 1994 or so by
Inverter fed motor PI series thin film Kapton CR and the kapton FCR of nano aluminium oxide filling.Kapton CR 50Hz alternating current,
Under the electric field strength of 20MV/m, the service life can be more than 100,000 hours, and the service life of traditional Kapton 100HN film only has
200h or so.But due to expensive, and for the strategic concerns of high-end devices.It is necessary to grasp mature Inverter fed motor for the country
PI film preparing technology.
In recent decades, China expands detailed research to Inverter fed motor PI film, has obtained certain achievement, studies work
Author thinks to influence many because being known as of material property for polyimides Inverter fed motor nanocomposite.Preparation process, nanometer
The type of filler, content, surface chemical modification are to influence the key factor of composite property.Polyimides corona-resistant film
Preparation process mainly has In-situ reaction and sol-gel method, both techniques respectively have advantage and disadvantage.In-situ reaction generally requires pair
Nanofiller carries out surface chemical modification, but the surface chemical modification effect of inorganic nano-filler is poor, it is difficult to improve nanometer and fill out
Expect the dispersibility in polyimide matrix.However, its process is simple, technical maturity is very suitable to industrial production.Colloidal sol-is solidifying
Glue method can allow nanoparticle it is evenly dispersed with matrix among, but there is also many disadvantages.Such as need to be added a certain amount of water and
Catalyst, this can have a significant impact the performance of polymer；Followed by during gel drying, solvent, small molecule, water are waved
Hair may cause material internal and generate shrinkage stress, influence the mechanics and mechanical performance of material；In addition, this method cannot achieve pair
The control of inorganic particle crystal form.There is also problems in industrialization production for sol-gel method craft.Related nanofiller
Type, the nanometer Al used in addition to E.I.Du Pont Company2O3In addition, Nano-meter SiO_22, nano-TiO2, nano-ZnO, nano-aluminum nitride, montmorillonite
(MMT) corona-resistance property of Kapton can be improved in various degree.Different nanofiller collaboration additions, can also be into one
Step improves corona-resistance property (the Applied Surface Science 2012,263 of film：30).
Chinese patent CN107652680A discloses a kind of nanometer alumina modified hybrid film of polyimide and its preparation
Method, the component including following volumes proportion：98-108 parts of bibenzene tetracarboxylic dianhydride, 67-77 parts of 4.4- diaminodiphenyl ether, N,
600-620 parts of N- dimethyl acetamide, 15-25 parts of the nano aluminium oxide of drying process, then special process is made nano oxidized
Aluminium modified polyimide hybrid film, this method can further increase blending effect, and the thermal stability of modified resin has
It is obviously improved.But the obtained composite polyimide material containing inorganic nanometer powder often reduces the mechanical property of film
Can, it is more significant for the reduction of film performance especially when nano-powder dispersion is uneven.
Chinese patent CN107501549A discloses a kind of preparation method of nano aluminium oxide doped polyimide film, should
Specific step is as follows for method:1) suitable pyromellitic acid anhydride (PMDA), 4,4'- diaminodiphenyl ethers (ODA), are chosen；
2), the material of selection is mixed, weighs the nano-oxide dispersion liquid of a certain amount of aluminium well prepared in advance, is added by certain
The dilution of solvent needed for solid content, is added in the there-necked flask equipped with ODA after high-speed stirred, and stirring is to being completely dissolved；This is received
Nano alumina particles solution is added in the preparation method of the alumina doped Kapton of rice in solution mixed process, can be with
For Kapton strengthening and toughening, and the wear-resisting property of Kapton can also be significantly improved.
However, the Kapton that above-mentioned addition inorganic particulate is compound, in the limitation for improving corona-resistance property, and
And the deficiencies of uneven there are inorganic particulate dispersion.Therefore needing to develop a kind of can be obviously improved Kapton Inverter fed motor
The preparation method of performance, and the requirement of industrialization can be reached.
Summary of the invention
Present inventor has found in the process of Study on Polyimide film Inverter fed motor to inorganic particulate compound in film
Microstructure be changed, can to improve Kapton corona resistance generate positive improvement.
Inorganic particulate microscopic appearance in film is modified and is regulated and controled in technical scheme, proposes a kind of porous oxygen
Change aluminium/Kapton preparation method, it is intended to solve one or more shortcomings, especially polyamides in the prior art
The insufficient defect of imines film corona-resistance property.
Concrete scheme provided by the present application is as follows：
A kind of preparation method of Inverter fed motor porous aluminas/Kapton, it includes following steps：
(1) alumina precursor is prepared：Triethanolamine is dissolved in deionized water, stirring adds isopropanol to dissolving
Aluminium, stirring form uniform, stable mixed liquor, and it is anti-that above-mentioned mixed liquor is placed in progress prehydrolysis reaction, prehydrolysis in reaction kettle
After answering, filtering is dried to obtain alumina precursor；
(2) aluminum oxide precursor precursor emulsion is prepared：The alumina precursor is added in KH550 silane coupler solution,
High-pressure emulsification machine high speed disperses to form aluminum oxide precursor precursor emulsion；
(3) polyamide is prepared：4,4'- diaminodiphenyl ether and dimethyl acetamide are dissolved into amine-containing molten
The lotion of step (2) and step (3) containing amine aqueous solution are about 1 according to mass ratio by liquid：1.1~20 are added in reaction kettle simultaneously
It is stirred, then according to pyromellitic acid anhydride and 4, the mass ratio of 4'- diaminodiphenyl ether is about 1：1~1.2 ratio
Pyromellitic acid anhydride is added to described step by step and is passed through in mixed solution to obtain polyamic acid resin；
(4) casting film-forming：The polyamic acid resin that step (3) obtains is formed into film by casting technique；
(5) film imidization：The film that step (4) obtains is heated, it is sub- to obtain Inverter fed motor porous aluminas/polyamides
Amine film.
Preferably, in the step (1), triethanolamine, deionized water, aluminium isopropoxide mass ratio are about：0.1-0.2：2~
5:1。
Preferably, in the step (1), the prehydrolysis reaction temperature is about 80-100 DEG C.
Preferably, in the step (2), the alumina precursor and KH550 silane coupled quality are about 1：0.01-
0.1。
Preferably, in the step (2), during the high speed dispersion, about 1.5%-2.5% mass fraction can be added
Emulsifier.
Preferably, the emulsifier is alkyl phenol polyoxyethylene ether.
Preferably, in the step (3), amine-containing solution ratio be mass ratio be 4,4'- diaminodiphenyl ether 20-25% and
Dimethyl acetamide 75-80% mixing.
Preferably, the casting technique in the step (4) is to heat polyamic acid resin on slobbering machine to carry out salivation shape
At film, the film by salivation is stretched on longitudinal stretching machine according to required size.
Preferably, the heating temperature in the step (5) is about 350-450 DEG C.
Another technical solution provided by the invention is：
Inverter fed motor porous aluminas/the Kapton obtained according to any of the above-described preparation method, which is characterized in that
Porous nano aluminium oxide particles are evenly dispersed in Kapton.
The present invention reacts to obtain alumina precursor using prehydrolysis, what realization regulated and controled the pattern of aluminium oxide particles
The evenly dispersed polyimide composite film of porous aluminas can be obtained in the process of later period film heating imidization in purpose.By
In the distribution of the porous aluminas of laminated film, so that the dielectric properties of film are greatly improved, thus thin to polyimides
The corona-resistance property of film has significant raising, improves to the service life for extending film and is also greatly improved.
The technical solution described for the present invention, it should be understood that the feature of various aspects disclosed in specification can be partly
Or be integrally bonded to each other or be combined with each other, and can with it is different from each other it is multinomial between be combined with each other.The present embodiment it is each
Aspect can execute independently of one another, or can also be executed together with complementary relationship.
Using " comprising " described in this specification, " having " and "comprising", unless using " only ", otherwise
Expression can add another part.The component and component that the present invention mentions, can be can also individually indicate a plurality of quantity.
In addition, term " at least " is understood to include any and all combinations of one or more related institute lists.
The preparation method of porous aluminas polyimide composite film of the invention, has the following advantages that：
1. being realized big to the pore size distribution of aluminium oxide particles, aperture by structure directing agent of the triethanolamine as aluminium oxide
It is small regulated and controled；
2. reacting by prehydrolysis, the interface performance of structure directing agent and aluminium oxide can be improved, before obtained aluminium oxide
Driving body also has more stable structure and surface property；
3. forming the lotion of uniform alumina precursor by high speed emulsification, mix, has higher with containing amine aqueous solution
The aluminium oxide particles of compatibility, formation also more disperse in laminated film.
Detailed description of the invention
Fig. 1 a is the SEM photograph on Inverter fed motor porous aluminas/Kapton surface of the present invention；
Fig. 1 b is the SEM photograph of Inverter fed motor porous aluminas/Kapton cross section of the present invention；
Specific embodiment
The technical solution of the application is described combined with specific embodiments below：
Embodiment one
A kind of preparation method of Inverter fed motor porous aluminas/Kapton, it includes following steps：
10g triethanolamine is dissolved in deionized water, stirring adds 100g aluminium isopropoxide to dissolving, and stirring forms equal
One, above-mentioned mixed liquor is placed in reaction kettle in 100 DEG C of progress prehydrolysis reactions by stable mixed liquor, and prehydrolysis reaction terminates
Afterwards, it filters, is dried to obtain alumina precursor；The alumina precursor is added in KH550 silane coupler solution, is added
Emulsifier disperses to form aluminum oxide precursor precursor emulsion in high-pressure emulsification machine high speed；By 4,4'- diaminodiphenyl ether 25% and two
Methylacetamide 75% (being mass ratio) is dissolved into containing amine aqueous solution, according to mass ratio is 1 by lotion and containing amine aqueous solution：
15 are added in reaction kettle are stirred simultaneously, then according to pyromellitic acid anhydride and 4, the mass ratio of 4'- diaminodiphenyl ether
It is 1：1 ratio pyromellitic acid anhydride is added step by step to described passes through in mixed solution to be fabricated to polyamic acid tree
Rouge；Obtained polyamic acid resin forms film by casting technique；Film is heated at 400 DEG C, obtains Inverter fed motor porous oxidation
Aluminium/Kapton.
It wherein obtains embodiment 1 and obtains the SEM figure on porous aluminas/polyimide composite film surface layer such as Fig. 1 a institute
Show, the SEM figure of cross section is as shown in Figure 1 b.Can be seen that laminated film surface from Fig. 1 a can be clearly seen that porous oxidation
Aluminium surface forms uniform hole；And from the point of view of sectional view, it can be seen that porous aluminas and polyimide polymer are uniform
Ground is combined with each other.In addition, from SEM figure it can also be seen that in compound polyimide film uniformly, monodisperse be distributed with it is more
Porous aluminum oxide particle, porous structure are able to ascend the dielectric properties and corona-resistance property of film.
Embodiment two
A kind of preparation method of Inverter fed motor porous aluminas/Kapton, it includes following steps：
15g triethanolamine is dissolved in deionized water, stirring adds 100g aluminium isopropoxide to dissolving, and stirring forms equal
One, above-mentioned mixed liquor is placed in 80 DEG C of progress prehydrolysis reactions in reaction kettle by stable mixed liquor, prehydrolysis after reaction,
Filtering, is dried to obtain alumina precursor；The alumina precursor is added in KH550 silane coupler solution, in high pressure
Mulser high speed disperses to form aluminum oxide precursor precursor emulsion；By 4,4'- diaminodiphenyl ether 20% and dimethyl acetamide
80% is dissolved into containing amine aqueous solution, according to mass ratio is 1 by lotion and containing amine aqueous solution：5 are added stirring in reaction kettle simultaneously mixes
It closes, then according to pyromellitic acid anhydride and 4, the mass ratio of 4'- diaminodiphenyl ether is 1：1.2 ratio is by Pyromellitic Acid
Dianhydride, which is added step by step to described, to be passed through in mixed solution to be fabricated to polyamic acid resin；Obtained polyamic acid resin is logical
It crosses casting technique and forms film；Film is heated at 400 DEG C, obtains Inverter fed motor porous aluminas/Kapton.
Embodiment three
A kind of preparation method of Inverter fed motor porous aluminas/Kapton, it includes following steps：
15g triethanolamine is dissolved in deionized water, stirring adds 100g aluminium isopropoxide to dissolving, and stirring forms equal
One, above-mentioned mixed liquor is placed in 80 DEG C of progress prehydrolysis reactions in reaction kettle by stable mixed liquor, prehydrolysis after reaction,
Filtering, is dried to obtain alumina precursor；The alumina precursor is added in KH550 silane coupler solution, in high pressure
Mulser high speed disperses to form aluminum oxide precursor precursor emulsion；By 4,4'- diaminodiphenyl ether 23% and dimethyl acetamide
77% is dissolved into containing amine aqueous solution, according to mass ratio is 1 by lotion and containing amine aqueous solution：10 are added stirring in reaction kettle simultaneously mixes
It closes, then according to pyromellitic acid anhydride and 4, the mass ratio of 4'- diaminodiphenyl ether is 1：1 ratio is by Pyromellitic Acid two
Acid anhydride, which is added step by step to described, to be passed through in mixed solution to be fabricated to polyamic acid resin；Obtained polyamic acid resin passes through
Casting technique forms film；Film is heated at 350 DEG C, obtains Inverter fed motor porous aluminas/Kapton.
Example IV
A kind of preparation method of Inverter fed motor porous aluminas/Kapton, it includes following steps：
20g triethanolamine is dissolved in deionized water, stirring adds 100g aluminium isopropoxide to dissolving, and stirring forms equal
One, above-mentioned mixed liquor is placed in 90 DEG C of progress prehydrolysis reactions in reaction kettle by stable mixed liquor, prehydrolysis after reaction,
Filtering, is dried to obtain alumina precursor；The alumina precursor is added in KH550 silane coupler solution, cream is added
Agent disperses to form aluminum oxide precursor precursor emulsion in high-pressure emulsification machine high speed；By 4,4'- diaminodiphenyl ether 20% and diformazan
Yl acetamide 80% is dissolved into containing amine aqueous solution, according to mass ratio is 1 by lotion and containing amine aqueous solution：1.1 are added reaction simultaneously
It is stirred in kettle, then according to pyromellitic acid anhydride and 4, the mass ratio of 4'- diaminodiphenyl ether is 1：1 ratio will be equal
Pyromellitic dianhydride, which is added step by step to described, passes through in mixed solution to be fabricated to polyamic acid resin；Obtained polyamide
Acid resin forms film by casting technique；Film is heated at 370 DEG C, obtains Inverter fed motor porous aluminas/Kapton.
Embodiment five
A kind of preparation method of Inverter fed motor porous aluminas/Kapton, it includes following steps：
18g triethanolamine is dissolved in deionized water, stirring adds 100g aluminium isopropoxide to dissolving, and stirring forms equal
One, above-mentioned mixed liquor is placed in 100 DEG C of progress prehydrolysis reactions in reaction kettle by stable mixed liquor, prehydrolysis after reaction,
Filtering, is dried to obtain alumina precursor；The alumina precursor is added in KH550 silane coupler solution, in high pressure
Mulser high speed disperses to form aluminum oxide precursor precursor emulsion；By 4,4'- diaminodiphenyl ether 22% and dimethyl acetamide
78% is dissolved into containing amine aqueous solution, according to mass ratio is 1 by lotion and containing amine aqueous solution：4 are added stirring in reaction kettle simultaneously mixes
It closes, then according to pyromellitic acid anhydride and 4, the mass ratio of 4'- diaminodiphenyl ether is 1：1 ratio is by Pyromellitic Acid two
Acid anhydride, which is added step by step to described, to be passed through in mixed solution to be fabricated to polyamic acid resin；Obtained polyamic acid resin passes through
Casting technique forms film；Film is heated at 400 DEG C, obtains Inverter fed motor porous aluminas/Kapton.
Embodiment six
A kind of preparation method of Inverter fed motor porous aluminas/Kapton, it includes following steps：
20g triethanolamine is dissolved in deionized water, stirring adds 100g aluminium isopropoxide to dissolving, and stirring forms equal
One, above-mentioned mixed liquor is placed in 100 DEG C of progress prehydrolysis reactions in reaction kettle by stable mixed liquor, prehydrolysis after reaction,
Filtering, is dried to obtain alumina precursor；The alumina precursor is added in KH550 silane coupler solution, in high pressure
Mulser high speed disperses to form aluminum oxide precursor precursor emulsion；By 4,4'- diaminodiphenyl ether 20% and dimethyl acetamide
80% is dissolved into containing amine aqueous solution, according to mass ratio is 1 by lotion and containing amine aqueous solution：5 are added stirring in reaction kettle simultaneously mixes
It closes, then according to pyromellitic acid anhydride and 4, the mass ratio of 4'- diaminodiphenyl ether is 1：1.2 ratio is by Pyromellitic Acid
Dianhydride, which is added step by step to described, to be passed through in mixed solution to be fabricated to polyamic acid resin；Obtained polyamic acid resin is logical
It crosses casting technique and forms film；Film is heated at 400 DEG C, obtains Inverter fed motor porous aluminas/Kapton.
Porous aluminas/polyester-imide laminated film is obtained to embodiment 1-6 to perform the following performance tests, test method and
Device therefor is as follows：
(1), corona-resistance property is tested
The film of composite material is prepared using the technique of this specification, wherein obtaining thickness is about that 10 μm of polyimides are compound
Film.Laminated film is cut into the sample of several 50mm × 50mm, and carries out Inverter fed motor test.Inverter fed motor test uses IEC-
60343 standards, i.e. corona bar electrode diameter 6mm (electrode end surface diameter 4mm, radius of corner R1mm), plate electrode diameter 50mm are surveyed
Strip part is room temperature, 40% or less ambient humidity, frequency 50Hz, field strength 20kV/mm.
(2), relative dielectric constant is tested
It is designed according to international standard ASTMD150 method, using parallel-plate electrode principle, tests electrode by upper/lower electrode+guarantor
Protect electrode composition.In order to ensure the accuracy of measurement result, sample preparation is at the following size：1, sample size：Diameter 5-40mm,
Thickness is less than 1mm；2, sample shape is prepared as circular membrane sample, and top electrode is plated on two sides；3, sample surfaces are flat and smooth, guarantee
It is contacted with parallel pole well.
(3), volume resistivity is tested
Laminated film is cut into the sample of several 50mm × 50mm, and carries out resistivity measurement.Using national standard
The method of GBT1410-2006 tests film volumetric resistivity.Instrument is the test of Air China's epoch ZST-121 volume resistance
Instrument.
Then the correlated performance of embodiment sample is tested.As a result such as table 1：
Table 1
Al2O3 compared to the prior art compound corona-resistant polyimide film, the application is in terms of corona-resistance property
There is significant raising.
The above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be to the present invention
Embodiment restriction.For those of ordinary skill in the art, it can also make on the basis of the above description
Other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all of the invention
Made any modifications, equivalent replacements, and improvements etc., should be included in the protection of the claims in the present invention within spirit and principle
Within the scope of.
The present invention at least provides following scheme：
A kind of preparation method of the Inverter fed motor porous aluminas/Kapton of scheme 1., it includes following steps：
Prepare alumina precursor：Triethanolamine is dissolved in deionized water, stirring adds aluminium isopropoxide to dissolving,
Stirring forms uniform, stable mixed liquor, and above-mentioned mixed liquor is placed in progress prehydrolysis reaction in reaction kettle, prehydrolysis reaction knot
Shu Hou is filtered, and is dried to obtain alumina precursor；
Prepare aluminum oxide precursor precursor emulsion：The alumina precursor is added into KH550 silane coupler solution,
High-pressure emulsification machine high speed disperses to form aluminum oxide precursor precursor emulsion；
Prepare polyamide：4,4'- diaminodiphenyl ether and dimethyl acetamide are dissolved into containing amine aqueous solution, it will
The lotion of step (2) and step (3) according to mass ratio are about 1 containing amine aqueous solution：1.1~20 are added stirring in reaction kettle simultaneously mixes
It closes, then according to pyromellitic acid anhydride and 4, the mass ratio of 4'- diaminodiphenyl ether is about 1：1~1.2 ratio is by equal benzene
Tetracarboxylic acid dianhydride, which is added step by step to described, to be passed through in mixed solution to obtain polyamic acid resin；
Casting film-forming：The polyamic acid resin that step (3) obtains is formed into film by casting technique；
Film imidization：The film that step (4) obtains is heated, Inverter fed motor porous aluminas/polyimides is obtained
Film.
A kind of preparation method of Inverter fed motor porous aluminas/Kapton as described in scheme 1 of scheme 2., feature
It is, in the step (1), triethanolamine, deionized water, aluminium isopropoxide mass ratio are about：0.1-0.2：2~5:1.
A kind of preparation method of Inverter fed motor porous aluminas/Kapton of the scheme 3. as described in scheme 1 or 2,
It is characterized in that, in the step (1), the prehydrolysis reaction temperature is 80-100 DEG C.
A kind of preparation of Inverter fed motor porous aluminas/Kapton of the scheme 4. as described in any one of scheme 1 to 3
Method, which is characterized in that in the step (2), the alumina precursor and KH550 silane coupled quality are 1：0.01-
0.1。
A kind of preparation of Inverter fed motor porous aluminas/Kapton of the scheme 5. as described in any one of scheme 1 to 4
Method, which is characterized in that in the step (2), during the high speed dispersion, 1.5%-2.5% mass fraction can be added
Emulsifier.
A kind of preparation method of Inverter fed motor porous aluminas/Kapton as described in scheme 5 of scheme 6., feature
It is, the emulsifier is alkyl phenol polyoxyethylene ether.
A kind of preparation of Inverter fed motor porous aluminas/Kapton of the scheme 7. as described in any one of scheme 1 to 6
Method, which is characterized in that in the step (3), amine-containing solution ratio is that mass ratio is 4,4'- diaminodiphenyl ether 20-25%
It is mixed with dimethyl acetamide 75-80%.
The Inverter fed motor porous aluminas that preparation method of the scheme 8. as described in any one of scheme 1 to 7 obtains/polyamides is sub-
Amine film, which is characterized in that porous nano aluminium oxide particles are evenly dispersed in Kapton.
Scheme 9. is according to method described in any of the above embodiments or product, the wherein average pore size of porous nano aluminium oxide particles
Between 50-100 nanometers.
Claims (9)
1. a kind of preparation method of Inverter fed motor porous aluminas/Kapton, it includes following steps：
(1) alumina precursor is prepared：Triethanolamine is dissolved in deionized water, stirring adds aluminium isopropoxide, stir to dissolving
It mixes to form uniform, stable mixed liquor, above-mentioned mixed liquor is placed in progress prehydrolysis reaction in reaction kettle, prehydrolysis reaction terminates
Afterwards, it is filtered, is dried to obtain alumina precursor；
(2) aluminum oxide precursor precursor emulsion is prepared：The alumina precursor is added into KH550 silane coupler solution,
High-pressure emulsification machine high speed disperses to form aluminum oxide precursor precursor emulsion；
(3) polyamide is prepared：4,4'- diaminodiphenyl ether and dimethyl acetamide are dissolved into containing amine aqueous solution, it will
The lotion of step (2) and step (3) according to mass ratio are about 1 containing amine aqueous solution：1.1~20 are added stirring in reaction kettle simultaneously mixes
It closes, then according to pyromellitic acid anhydride and 4, the mass ratio of 4'- diaminodiphenyl ether is about 1：1~1.2 ratio is by equal benzene
Tetracarboxylic acid dianhydride, which is added step by step to described, to be passed through in mixed solution to obtain polyamic acid resin；
(4) casting film-forming：The polyamic acid resin that step (3) obtains is formed into film by casting technique；
(5) film imidization：The film that step (4) obtains is heated, it is thin to obtain Inverter fed motor porous aluminas/polyimides
Film.
2. a kind of preparation method of Inverter fed motor porous aluminas/Kapton as described in claim 1, feature exist
In in the step (1), triethanolamine, deionized water, aluminium isopropoxide mass ratio are about：0.1-0.2：2~5：1.
3. a kind of preparation method of Inverter fed motor porous aluminas/Kapton as claimed in claim 1 or 2, feature
It is, in the step (1), the prehydrolysis reaction temperature is 80-100 DEG C.
4. a kind of preparation side of Inverter fed motor porous aluminas/Kapton as claimed any one in claims 1 to 3
Method, which is characterized in that in the step (2), the alumina precursor and KH550 silane coupled quality are about 1：0.01-
0.1。
5. a kind of preparation side of Inverter fed motor porous aluminas/Kapton according to any one of claims 1 to 4
Method, which is characterized in that in the step (2), during the high speed dispersion, the cream of 1.5%-2.5% mass fraction can be added
Agent.
6. a kind of preparation method of Inverter fed motor porous aluminas/Kapton as claimed in claim 5, feature exist
In the emulsifier is alkyl phenol polyoxyethylene ether.
7. such as a kind of preparation side of Inverter fed motor porous aluminas/Kapton described in any one of claims 1 to 6
Method, which is characterized in that in the step (3), amine-containing solution ratio be mass ratio be 4,4'- diaminodiphenyl ether 20-25% and
Dimethyl acetamide 75-80% mixes.
8. wherein the average pore size of porous nano aluminium oxide particles is in 50-100 nanometer according to method described in any of the above embodiments
Between.
9. Inverter fed motor porous aluminas/polyimides that preparation method as claimed in any of claims 1 to 7 in one of claims obtains is thin
Film, which is characterized in that porous nano aluminium oxide particles are evenly dispersed in Kapton.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810704456.4A CN108822319A (en) | 2018-07-02 | 2018-07-02 | Inverter fed motor porous aluminas/Kapton and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810704456.4A CN108822319A (en) | 2018-07-02 | 2018-07-02 | Inverter fed motor porous aluminas/Kapton and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108822319A true CN108822319A (en) | 2018-11-16 |
Family
ID=64134568
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810704456.4A Pending CN108822319A (en) | 2018-07-02 | 2018-07-02 | Inverter fed motor porous aluminas/Kapton and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108822319A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110698682A (en) * | 2019-09-27 | 2020-01-17 | 武汉华星光电半导体显示技术有限公司 | Polyimide composite material, preparation method and application thereof |
| CN112280036A (en) * | 2020-11-17 | 2021-01-29 | 潍坊弘润新材料有限公司 | Processing technology of polyimide film |
| CN115109442A (en) * | 2022-07-20 | 2022-09-27 | 常州嘉尔电子科技有限公司 | Atomic oxygen resistant coating liquid and preparation coating method thereof |
| CN115725101A (en) * | 2022-11-21 | 2023-03-03 | 乌镇实验室 | Preparation method of nano alumina/polyimide high-temperature dielectric composite film |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105818504A (en) * | 2016-03-23 | 2016-08-03 | 中国空间技术研究院 | Single-sided corona-resistant polyimide composite thin film and preparation method thereof |
| CN107501549A (en) * | 2017-06-22 | 2017-12-22 | 莱芜中天绝缘材料有限公司 | A kind of preparation method of nano aluminium oxide doped polyimide film |
-
2018
- 2018-07-02 CN CN201810704456.4A patent/CN108822319A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105818504A (en) * | 2016-03-23 | 2016-08-03 | 中国空间技术研究院 | Single-sided corona-resistant polyimide composite thin film and preparation method thereof |
| CN107501549A (en) * | 2017-06-22 | 2017-12-22 | 莱芜中天绝缘材料有限公司 | A kind of preparation method of nano aluminium oxide doped polyimide film |
Non-Patent Citations (2)
| Title |
|---|
| CABRERA等: "Surfactant-assisted synthesis of mesoporous alumina showing continuously adjustable pore sizes", 《ADVANCED MATERIALS》 * |
| LIZHU LIU等: "Effect of imidization process on the performance of PI/nano-Al2O3 three layer composite film", 《PIGMENT & RESIN TECHNOLOGY》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110698682A (en) * | 2019-09-27 | 2020-01-17 | 武汉华星光电半导体显示技术有限公司 | Polyimide composite material, preparation method and application thereof |
| CN112280036A (en) * | 2020-11-17 | 2021-01-29 | 潍坊弘润新材料有限公司 | Processing technology of polyimide film |
| CN115109442A (en) * | 2022-07-20 | 2022-09-27 | 常州嘉尔电子科技有限公司 | Atomic oxygen resistant coating liquid and preparation coating method thereof |
| CN115725101A (en) * | 2022-11-21 | 2023-03-03 | 乌镇实验室 | Preparation method of nano alumina/polyimide high-temperature dielectric composite film |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108822319A (en) | Inverter fed motor porous aluminas/Kapton and preparation method thereof | |
| CN102993749B (en) | A kind of nanometer Al 2o 3the corona-resistant polyimide film of compound | |
| CN106589374B (en) | A kind of preparation method of Kapton and the Kapton being prepared by this method | |
| CN109438703B (en) | Black polyimide microsphere, preparation method thereof and preparation method of film containing black polyimide microsphere | |
| CN105818504B (en) | A kind of polyimide composite film of one side Inverter fed motor and preparation method thereof | |
| Byun et al. | Effect of solvent and crystal size on the selectivity of ZSM-5/Nafion composite membranes fabricated by solution-casting method | |
| CN106397769B (en) | A kind of polyimides titanium dioxide nanoplate laminated film and preparation method thereof | |
| US20040053060A1 (en) | Hybrid material, use of said hybrid material and method for making same | |
| CN109135554A (en) | polyimide varnish and its preparation method and application | |
| CN108586780A (en) | A kind of porosity Kapton and preparation method thereof | |
| CN108822317A (en) | A kind of preparation method of graphene polyimide heating film | |
| CN111116221A (en) | Preparation method of high-temperature-resistant mullite nanofiber aerogel | |
| CN109082119A (en) | A kind of cellulose modified polyimides corona-resistant film and preparation method thereof | |
| Ren et al. | Synthesis of cement shell microcapsules via W/O Pickering emulsions | |
| CN106898802B (en) | A kind of high-performing car hydrogen fuel cell composite nano-powder material and preparation method thereof | |
| TW201634119A (en) | Ion exchange membrane bearing preferential oriented morphological texture | |
| Qiu et al. | Polyimide/kaolinite composite films: Synthesis and characterization of mechanical, thermal and waterproof properties | |
| CN108499374A (en) | PVDF composite graphites alkene filter core film and its production technology | |
| CN110951115B (en) | Surface grafting modified alumina for epoxy composite insulating material and epoxy composite insulating material | |
| CN110669257B (en) | Coated modified alumina, preparation method thereof and epoxy composite insulating material | |
| Li et al. | Secondary dialkylammonium salt/crown ether [2] pseudorotaxanes as nanostructured platforms for proton transport | |
| CN116742082A (en) | Preparation method of magnetic nanoparticle supported phosphotungstic acid-sulfonated polyether-ether-ketone composite proton exchange membrane | |
| CN107570021A (en) | A kind of hydrophilic polysulfones/silica blend hollow fiber membrane and preparation method thereof | |
| Huang et al. | Composite proton exchange membranes produced using chitosan and kaolin solvent-free fluid | |
| CN109897199A (en) | The polyimide precursor gel and its preparation method and application for inhaling wave and heat resistant poly acid imide lightweight labyrinth can be prepared |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181116 |
|
| RJ01 | Rejection of invention patent application after publication |