CN108264766A - A kind of preparation method of Kapton - Google Patents
A kind of preparation method of Kapton Download PDFInfo
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- CN108264766A CN108264766A CN201810073351.3A CN201810073351A CN108264766A CN 108264766 A CN108264766 A CN 108264766A CN 201810073351 A CN201810073351 A CN 201810073351A CN 108264766 A CN108264766 A CN 108264766A
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- kapton
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- 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
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- 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
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
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- 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
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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- 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
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- 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
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-containing compounds
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- 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)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The present invention relates to a kind of preparation methods of Kapton, polyamic acid solution is prepared in intensive polar solvent using the dianhydride of diamine mixture and equimolar amounts, then adds in after the nanometer calcium sulfate whisker film forming of polyamic acid solution quality 0.1 5% and Kapton is prepared through imidization.Preparation method of the present invention is simple, step is easily operated, Kapton can be made to have better two-dimentional mechanical property, relatively low shrinking percentage and film without through-hole by adding in nanometer calcium sulfate whisker into raw material, and with preferable covering, water resistance, chemical resistance, high-modulus, lower shrinkage performance, can be extensively using electronic circuit board copper membrane, cover film, insulating film.
Description
Technical field
The present invention relates to a kind of preparation methods of polyimide film, belong to technical field of material.
Background technology
Whisker is the mono-crystlling fibre that draw ratio is more than 10, and atomic structural arrangement high-sequential, internal flaw is few, is a kind of
The strengthening and toughening agent of excellent composite material, earliest industrialization crystal whisker products (silicon carbide) come across 1962, because price is held high
Expensive (3000-5000 members/kilogram) and make its application limited.More cheap potassium titanate crystal whisker comes across the Japan after 1980, brilliant
It must apply and just have breakthrough.The research and development of the inorganic crystal whisker in China start from the initial stage nineties, and emphasis is related to the materials such as silicon carbide, silicon nitride
Material, but because material price costliness can not obtain large-scale commercial Application.
Compared with other crystal whisker materials, calcium sulfate crystal whiskers have the advantages that mechanical strength is good, nontoxic, stable, inexpensive, can make
It is that reinforcing material is used for the fields such as polyurethane, plastics, cement, ceramics, papermaking, film.As CN1598083A, CN1317430C,
Stable nanometer calcium sulfate whisker material is prepared in CN10313337A, CN103139382A etc. using the technique of different synthesis
Material.CN101671848 proposes a kind of synthesis preparation method of the nanometer calcium sulfate whisker of high draw ratio.
Polyimide material can be used as plastics, film, solution etc. are various to apply model as high-performance aromatic polymer
It encloses, has in excellent height temperature stability, show excellent physics, chemical property and electrical property, be aviation boat
My god, the core material in the fields such as microelectronics.
In recent years, with the slimming of smart mobile phone, tablet computer, high operational capability, high storage capacity, for polyamides Asia
The requirement of amine thin-film material is higher and higher, such as, higher modulus, lower contraction, superior three dimensionality, and more
Excellent heat conductivility etc..And the acquisition of these performances relies on inorganic nano material to the compound, modified etc. of organic material.
The one-dimensional size extension of whisker helps polyphosphazene polymer imide membrane two dimensional surface orientation strand regularity stretching, extension row
Row, the two is compound can to assign film superior comprehensive performance.Expire patent for SHANGHAI RESEARCH INSTITUTE OF SYNTHETIC RESINS
CN97106672 is disclosed using potassium titanate crystal whisker reinforced polyimide composite material, and CN104631200B discloses a kind of titanium
The preparation method of sour potassium crystal whisker reinforced polyimide fibrous paper equally exists whisker and manufactures of high cost, fiber blend modification difficulty
It greatly, can not industrial applications.
CN103524767A is disclosed adds in ultra-fine inorganic silica, zinc oxide, tungsten wire array whisker in polyamic acid glue
Whisker and/or nano carbon tube material are ultrasonically treated, and formation micro-nano in situ is compound, and agitated dispersion, filtering and vacuum defoamation are made
Stablize, high-quality can casting film-forming composite glue solution, produce that thickness is 7.5~125 μm, linear expansion coefficient is 5~18ppm/
DEG C electron level Kapton；The of high cost of whisker and carbon nanotube is equally existed, industrial applications can not be obtained.
Invention content
The purpose of the present invention is to solve problem, provide that a kind of preparation method is simple, the easily operated one kind of step
The preparation method of polyimide compositions.
The present invention adopts the following technical scheme that：A kind of preparation method of Kapton, using diamine mixture with etc.
The dianhydride of mole prepares polyamic acid solution for raw material in intensive polar solvent, then adds in receiving for material quality 0.1-5%
Kapton is prepared through imidization after rice calcium sulfate crystal whiskers film forming.
Further, the draw ratio of the nanometer calcium sulfate whisker is 5-50, and length is less than 10 μm, a diameter of 0.2-2 μm.
Further, the diamines in the diamine mixture at least contains a kind of organosilicon structures.
Further, the nanometer calcium sulfate whisker ultrasonic dissolution is in dimethylacetamide solvent.
Further, the thickness of the Kapton is 10-75 μm.
Further, the diamines for p-phenylenediamine, m-phenylene diamine (MPD), benzidine, p dimethylamine, 4,4 '-diamino two
Phenyl ether, 3,4 '-diamino-diphenyl ether, 4,4 '-diaminodiphenyl-methane, 4,4 '-diamino diphenyl sulfone, 3,3 '-two
Methyl -4,4 '-diaminodiphenyl-methane, 1,5 '-diaminonaphthalene, 3,3 '-dimethoxy benzidine, Isosorbide-5-Nitrae '-bis- (3- methyl -5
Aminophenyl) benzene and above-mentioned several substances amide formative derivative
Further, the dianhydride for pyromellitic acid dianhydride, 3,3 ' 4,4 '-bibenzene tetracarboxylic dianhydride, 2,3 ', 3,4 '-connection
Pyromellitic dianhydride, 3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydride, 2,3 ', 6,7 '-naphthalenetetracarbacidic acidic, 2,2- bis- (3,4- dicarboxyls
Base phenyl) ether, pyridine -2,3,5,6- tetracarboxylic acids or above-mentioned several substances amide formed derivative.
Further, the intensive polar solvent is in pyrrolidones series solvent, phenol system solvent, hexamethyl phosphoramide or r- fourth
One or both of ester aprotic polar solvent.
The preparation method of the present invention is simple, and step is easily operated, can by adding in nanometer calcium sulfate whisker into raw material
Kapton is made to have preferably two-dimentional mechanical property, relatively low shrinking percentage and film to hide without through-hole, and with preferable
Gai Xing, water resistance, chemical resistance, high-modulus, lower shrinkage performance, can be extensively using electronic circuit board with covering copper
Film, cover film, insulating film etc..
Description of the drawings
Fig. 1 is the atomic force microscopy diagram of Kapton that the embodiment of the present invention 1 is prepared.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Comparative example 1：
The logical nitrogen protection in the reaction vessel strictly removed water adds in the 4 of 199g (0.995mol), 4 '-diaminodiphenyl ether
(ODA) and the diamino silanes (AS-0) of 1.24g (0.005mol) n=0 solvent N, N- the dimethyl second of 1672g, is then added in
Amide (DMAc) is eventually adding the pyromellitic dianhydride (PMDA) of 218g (1mol).It is stirred at room temperature 12 hours, it is fully anti-
Should, filtering obtains polyamic acid solution.After standing and defoaming, coating baking becomes the film of 25 micron thickness.
Embodiment 1：
The logical nitrogen protection in the reaction vessel strictly removed water adds in the 4 of 199g (0.995mol), 4 '-diaminodiphenyl ether
(ODA) and the diamino silanes (AS-0) of 1.24g (0.005mol) n=0 solvent N, N- the dimethyl second of 1612g, is then added in
Amide is eventually adding the pyromellitic dianhydride (PMDA) of 218g (1mol).It is stirred at room temperature 12 hours, fully reacts, filtering,
Obtain polyamic acid solution.
By 0.5 micron of the commercially available diameters of 0.2g, length is 5 microns of nanometer calcium sulfate whisker (NW-10), is distributed to
In 60gDMAc solvents, ultrasonic disperse 20min, then dispersion liquid is added in above-mentioned polyamic acid solution, strong stirring dispersion,
After standing and defoaming, coating baking becomes the film of 25 micron thickness.
Embodiment 2：
The logical nitrogen protection in the reaction vessel strictly removed water adds in the 4 of 199g (0.995mol), 4 '-diaminodiphenyl ether
(ODA) and the diamino silanes (AS-0) of 1.24g (0.005mol) n=0 solvent N, N- the dimethyl second of 1512g, is then added in
Amide is eventually adding the pyromellitic dianhydride (PMDA) of 218g (1mol).It is stirred at room temperature 12 hours, fully reacts, filtering,
Obtain polyamic acid solution.
By 0.2 micron of the commercially available diameters of 0.4g, length is 2 microns of nanometer calcium sulfate whisker (NW-20), is distributed to
In 160gDMAc solvents, ultrasonic disperse 20min, then dispersion liquid is added in above-mentioned polyamic acid solution, strong stirring dispersion,
After standing and defoaming, coating baking becomes the film of 25 micron thickness.
Embodiment 3：
The logical nitrogen protection in the reaction vessel strictly removed water adds in the 4 of 199g (0.995mol), 4 '-diaminodiphenyl ether
(ODA) and the diamino silanes (AS-0) of 1.24g (0.005mol) n=0 solvent N, N- the dimethyl second of 1500g, is then added in
Amide is eventually adding the pyromellitic dianhydride (PMDA) of 218g (1mol).It is stirred at room temperature 12 hours, fully reacts, filtering,
Obtain polyamic acid solution.
By 0.5 micron of the commercially available diameters of 1.0g, length is 5 microns of nanometer calcium sulfate whisker (NW-10), is distributed to
In 172gDMAc solvents, ultrasonic disperse 20min, then dispersion liquid is added in above-mentioned polyamic acid solution, strong stirring dispersion,
After standing and defoaming, coating baking becomes the film of 25 micron thickness.
Embodiment 4：
The logical nitrogen protection in the reaction vessel strictly removed water adds in the 4 of 199g (0.995mol), 4 '-diaminodiphenyl ether
(ODA) and the diamino silanes (AS-0) of 1.24g (0.005mol) n=0 solvent N, N- the dimethyl second of 1372g, is then added in
Amide is eventually adding the pyromellitic dianhydride (PMDA) of 218g (1mol).It is stirred at room temperature 12 hours, fully reacts, filtering,
Obtain polyamic acid solution.
By 0.2 micron of the commercially available diameters of 2.5g, length is 2 microns of nanometer calcium sulfate whisker (NW-20), is distributed to
In 300gDMAc solvents, ultrasonic disperse 20min, then dispersion liquid is added in above-mentioned polyamic acid solution, strong stirring dispersion,
After standing and defoaming, coating baking becomes the film of 25 micron thickness.
Embodiment 5：
The logical nitrogen protection in the reaction vessel strictly removed water adds in the 4 of 199g (0.995mol), 4 '-diaminodiphenyl ether
(ODA) and the diamino silanes (AS-0) of 1.24g (0.005mol) n=0 solvent N, N- the dimethyl second of 1372g, is then added in
Amide is eventually adding the pyromellitic dianhydride (PMDA) of 218g (1mol).It is stirred at room temperature 12 hours, fully reacts, filtering,
Obtain polyamic acid solution.
By 0.5 micron of the commercially available diameters of 2.5g, length is 5 microns of nanometer calcium sulfate whisker (NW-10), is distributed to
In 300gDMAc solvents, ultrasonic disperse 20min, then dispersion liquid is added in above-mentioned polyamic acid solution, strong stirring dispersion,
After standing and defoaming, coating baking becomes the film of 25 micron thickness.
Embodiment 6：
The logical nitrogen protection in the reaction vessel strictly removed water adds in the 4 of 199g (0.995mol), 4 '-diaminodiphenyl ether
(ODA) and the diamino silanes (AS-0) of 1.24g (0.005mol) n=0 solvent N, N- the dimethyl second of 1072g, is then added in
Amide is eventually adding the pyromellitic dianhydride (PMDA) of 218g (1mol).It is stirred at room temperature 12 hours, fully reacts, filtering,
Obtain polyamic acid solution.
By 0.2 micron of the commercially available diameters of 3.5g, length is 2 microns of nanometer calcium sulfate whisker (NW-20), is distributed to
In 600gDMAc solvents, ultrasonic disperse 20min, then dispersion liquid is added in above-mentioned polyamic acid solution, strong stirring dispersion,
After standing and defoaming, coating baking becomes the film of 25 micron thickness.
Comparative example 1 and embodiment 1-6 polyamide solutions are prepared into 25 uniform micrometer polyamide films by coating,
And hot imidization is completed, performance evaluation is carried out to it, is shown in Table 2.
Table 1
| Composition | Comparative example 1 | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| ODA | 0.995mol | 0.995mol | 0.995mol | 0.995mol | 0.995mol | 0.995mol | 0.995mol |
| PMDA | 1.000mol | 1.000mol | 1.000mol | 1.000mol | 1.000mol | 1.000mol | 1.000mol |
| AS-0 | 0.005mol | 0.005mol | 0.005mol | 0.005mol | 0.005mol | 0.005mol | 0.005mol |
| DMac | 1672g | 1672g | 1672g | 1672g | 1672g | 1672g | 1672g |
| NW-10 | / | 0.2g | / | 1.0g | / | 2.5g | / |
| NW-20 | / | / | 0.4g | / | 2.5g | / | 3.5g |
Table 2
As seen from the results in Table 2, the shrinking percentage of Kapton being prepared using the present invention is relatively low, coefficient of thermal expansion
Low and with higher initial modulus, the tensile strength of film is larger.
The Kapton that Example 1 is prepared carries out atomic force microscope observation, as a result as Fig. 1 results can
Know, Kapton pattern has the coarse structure of 50nm or so, while visible nanometer calcium sulfate whisker is in polyimides tree
It is uniformly dispersed in fat, therefore the mechanical property of film can be substantially improved.
Claims (8)
1. a kind of preparation method of Kapton, it is characterised in that：Use the dianhydride of diamine mixture and equimolar amounts for
Raw material prepares polyamic acid solution in intensive polar solvent, then adds in the nanometer calcium sulfate whisker film forming of material quality 0.1-5%
Kapton is prepared by imidization.
2. the preparation method of Kapton as described in claim 1, it is characterised in that：The nanometer calcium sulfate whisker
Draw ratio is 5-50, and length is less than 10 μm, a diameter of 0.2-2 μm.
3. the preparation method of Kapton as described in claim 1, it is characterised in that：Two in the diamine mixture
Amine at least contains a kind of organosilicon structures.
4. the preparation method of Kapton as described in claim 1, it is characterised in that：The nanometer calcium sulfate whisker surpasses
Sound is dissolved in dimethylacetamide solvent.
5. the preparation method of Kapton as described in claim 1, it is characterised in that：The thickness of the Kapton
Spend is 10-75 μm.
6. the preparation method of Kapton as described in claim 1, it is characterised in that：The diamines for p-phenylenediamine,
M-phenylene diamine (MPD), benzidine, p dimethylamine, 4,4 '-diamino-diphenyl ether, 3,4 '-diamino-diphenyl ether, 4,4 '-diamino
Base diphenyl methane, 4,4 '-diamino diphenyl sulfone, 3,3 '-dimethyl -4,4 '-diaminodiphenyl-methane, 1,5 '-diamino
Base naphthalene, 3,3 '-dimethoxy benzidine, Isosorbide-5-Nitrae '-bis-（- 5 aminophenyl of 3- methyl）The amide shape of benzene and above-mentioned several substances
Become second nature derivative.
7. the preparation method of Kapton as described in claim 1, it is characterised in that：The dianhydride is pyromellitic acid two
Acid anhydride, 3,3 ' 4,4 '-bibenzene tetracarboxylic dianhydride, 2,3 ', 3,4 '-bibenzene tetracarboxylic dianhydride, 3,3 ', 4,4 '-benzophenone tetracarboxylic
Dianhydride, 2,3 ', 6,7 '-naphthalenetetracarbacidic acidic, 2,2- is bis-（3,4- dicarboxyphenyis）Ether, pyridine -2,3,5,6- tetracarboxylic acids or above-mentioned several
The derivative that the amide of kind substance is formed.
8. the preparation method of Kapton as described in claim 1, it is characterised in that：The intensive polar solvent is pyrroles
One or both of alkanone series solvent, phenol system solvent, hexamethyl phosphoramide or r- butyrolactone aprotic polar solvents.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112251022A (en) * | 2020-08-21 | 2021-01-22 | 湖南国柔科技有限公司 | High-order repeated bending CPI film and preparation method thereof |
| CN113745761A (en) * | 2021-08-19 | 2021-12-03 | 中国科学院上海硅酸盐研究所 | Polyimide/silicon nitride whisker composite lithium ion battery diaphragm and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112251022A (en) * | 2020-08-21 | 2021-01-22 | 湖南国柔科技有限公司 | High-order repeated bending CPI film and preparation method thereof |
| CN113745761A (en) * | 2021-08-19 | 2021-12-03 | 中国科学院上海硅酸盐研究所 | Polyimide/silicon nitride whisker composite lithium ion battery diaphragm and preparation method thereof |
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