CN109134930A - A kind of dispersing method of inorganic filler - Google Patents
A kind of dispersing method of inorganic filler Download PDFInfo
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- CN109134930A CN109134930A CN201810971327.1A CN201810971327A CN109134930A CN 109134930 A CN109134930 A CN 109134930A CN 201810971327 A CN201810971327 A CN 201810971327A CN 109134930 A CN109134930 A CN 109134930A
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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
- C08K9/00—Use of pretreated ingredients
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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
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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
- C08G73/1046—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
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- 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
- C08K3/02—Elements
- C08K3/04—Carbon
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
Abstract
The invention discloses a kind of dispersing method of inorganic filler, specifically: inorganic filler is first placed in ultrasound infiltration in aprotic polar solvent, obtained by gained mixed liquor is placed in the sand mill containing different-grain diameter zirconium pearl again and is dispersed with specific rotation speeds.Inorganic filler is dispersed using the method for the invention, dispersion effect is good；It will disperse resulting inorganic filler dispersed paste and be used to prepare black matt polyimide film, gained film mechanical performance and electrical strength are high, and shading rate is low, and matt is good；The frequency that filter core is replaced in the preparation process of film reduces.
Description
Technical field
The present invention relates to Kaptons, and in particular to the nothing used in black matt polyimide film preparation process
The dispersing method of machine filler.
Background technique
Black matt polyimide (polyimides abbreviation PI) film is a kind of high insulation, high-intensitive insulation film, phase
Than in common PI film, black matt PI film is opaque, light transmission and reflection coefficient are low, has good light-proofness, thermal conductivity
Deng being widely used in mobile device, computer, automobile and Military Electronic Equipment etc..
The prior art is individually added into black material in polyamic acid (PAA) resin or flatting silica prepare PI film document it is more,
But both be added simultaneously prepare black matt polyimide film document it is less.The invention of Publication No. CN101579904A is special
Benefit prepares black paste using grinding 4-8h technique, and black paste and matt agent are first mixed with reactant aromatic diamine in proportion
Uniformly, then with aromatic dianhydride it reacts and directly prepares black matt polyamic acid resin solution.The hair of Publication No. 102529262A
Black matt ink layer is coated on Kapton base upper and lower surface by bright patent, and wherein black matt ink is through being sanded
Machine mixed grinding 1h, then high speed dispersion 1h prepare, group become water base high temperature resistant acrylic ink resin, copper oxide, iron oxide,
Chromium oxide, high temperature resistant auxiliary agent, dispersing agent, advection agent etc..The patent of invention of Publication No. CN105733001A is using ball milling high speed
By the black material of addition, high pressure spray, infiltration ball milling prepare black paste to shearing homogeneous in a solvent with delustering agent；Then black slurry
Expect and is reacted respectively with equal benzene dianhydride and biphenyl dianhydride after diamine reactant.The patent of invention of Publication No. CN105385159A is to two
Silane coupling agent is added in methylacetamide, is stirring evenly and then adding into black pigment, through high-pressure homogeneous processing, obtains black slurry
Material；Delustering agent and talcum powder are added in organic solvent, after mixing evenly, clipped dispersion and ultrasonic disperse processing preparation disappear
Then light slurry material mixes PAA resin obtained, black paste and flatting silica slurry, film.Publication No.
The patent of invention of CN106432724A is mixed polyacrylonitrile powder and highly polar aprotic organic solvent using situ aggregation method,
Heating stirring cools down after completely dissolution, and aromatic dicarboxylic primary amine is added, aromatic dicarboxylic anhydride is added after being completely dissolved, and heats
Under stirring, prepares polyacrylonitrile and polyamic acid forms the blend solution of Molecule interpenetration network.The above invention is not directed to black
Material and the specific dispersing method of flatting silica.
And in production application, since carbon black is Nano grade, the relationship that the blackness of carbon black and its partial size are inversely proportional, charcoal
Black partial size is smaller, and blackness is higher, and the black film light-proofness of preparation is better；Carbon black dispersion is better, and the matt black film of preparation is electrically strong
It is also better to spend, because when carbon black dispersion is good, distance energy stability maintenance between each carbon black particle reduces carbon black and nearly forms conductive path
Possibility.Flatting silica is micron level, and flatting silica partial size acts on directly proportional relationship to the matt of black film, and flatting silica partial size is got over
Greatly, black film matt effect is better, but the excessive flatting silica of partial size easily blocks strainer and reduces the mechanical performance of black film.As it can be seen that charcoal
The partial size difference of black and flatting silica is larger, and the two also differs quite big on surface texture, pattern, at the same to the two dispersed compared with
Individually a kind of filler dispersion, difficulty are in the increase of geometry grade.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of dispersing methods of inorganic filler, using the method for the invention
Disperse inorganic filler, dispersion effect is good；It will disperse resulting inorganic filler dispersed paste and be used to prepare black matt polyimide
Film, gained film mechanical performance and electrical strength are high, and shading rate is low, and matt is good；Filter is replaced in the preparation process of film
The frequency of core reduces.
The dispersing method of inorganic filler of the present invention, the inorganic filler include flatting silica and/or carbon black, specifically
To obtain inorganic filler dispersed paste using one of following methods a)-c):
Method a): when inorganic filler is flatting silica, dispersing method are as follows: flatting silica is taken to be placed in aprotic polar solvent
In, it is infiltrated under ultrasound condition, gained mixed liquor is placed in sand mill, is added or is added without dispersing agent, is then added partial size and is
The zirconium pearl of 1-5mm, is dispersed with the revolving speed of 3000-6000r/min, obtains flatting silica slurry；
Method b): when inorganic filler is carbon black, dispersing method are as follows: take carbon black to be placed in aprotic polar solvent, surpass
It is infiltrated under the conditions of sound, gained mixed liquor is placed in another sand mill, is added or is added without dispersing agent, is then added partial size and is
The zirconium pearl of 0.05-0.45mm, is dispersed with the revolving speed of 1000-2000r/min, and obtaining carbon black slurry is described inorganic fill out
Expect dispersed paste；
Method c): when inorganic filler includes simultaneously flatting silica and carbon black, flatting silica slurry first is obtained with method a), then
Carbon black slurry is obtained with method b), flatting silica slurry is added to later in the sand mill where carbon black slurry and is continued with 1000-
The revolving speed of 2000r/min is dispersed, and resulting material is the inorganic filler dispersed paste.
In the dispersing method of above-mentioned inorganic filler, the flatting silica is conventional selection in the prior art, is preferably selected
A kind of or any two or more combination from silica, titanium dioxide and calcium monohydrogen phosphate.The granularity of the flatting silica is micro-
Meter level.And carbon black is nanoscale, primary partial size is usually 10-40nm (actuals is linked together with grapevine),
Preferably 15-25nm.
In the dispersing method of above-mentioned inorganic filler, the sand mill is conventional selection in the prior art, preferably sleeping
Formula sand mill.
In the dispersing method of above-mentioned inorganic filler, the aprotic polar solvent is molten to can be used for preparing polyamic acid resin
The solvent of liquid, selection is same as the prior art, specifically can be selected from n,N-dimethylacetamide (DMAC), N, N- dimethyl
Formamide (DMF), n-methyl-2-pyrrolidone (NMP), N, one of N- diethyl acetamide and N, N- diethylformamide
Or any two or more combination；When the combination of aprotic polar solvent being selected as more than above two, between them
Proportion can be any proportion.In the above scheme, the dosage of aprotic polar solvent can determine as needed, specifically,
In method a), the dosage of aprotic polar solvent is usually to make concentration 10-20wt% of the flatting silica in gained mixed liquor,
More preferably 11-13wt%；In method b), the dosage of aprotic polar solvent is usually to make carbon black in gained mixed liquor
Concentration is 3-10wt%, more preferably 4-8wt%.
In the dispersing method of above-mentioned inorganic filler, the dispersing agent can be conventional selection in the prior art, usually
For the dispersing agent with pigment affinity groups, specifically can be the copolymer solution dispersing agent containing acidic-group, (such as moist type disperses
Agent KMT-3003), modified high-molecular type interfacial agent (such as KP100), efficient polyurethane-modified acrylic acid dispersing agent (such as oversubscription
Powder SUP1400) either unsaturated carboxylic acid polyamine amides solution (such as wetting dispersing agent BYK-130).When in dispersion
When in the process needing that dispersing agent is added, the dosage of the dispersing agent is preferably the 10-40wt% of flatting silica or carbon black loading, more excellent
It is selected as 15-20wt%.
In the method a) of the dispersing method of above-mentioned inorganic filler, infiltration is carried out under conditions of not heating, infiltration when
Between be usually 1-5h；In ultrasound infiltration, preferably the temperature of control system is at 10-30 DEG C, to prevent flatting silica in the item of overheat
Reunite under part.When dispersing in sand mill, dispersion 0.5-1h first preferably is carried out in the revolving speed of 500-1000r/min, is then mentioned again
The revolving speed of speed to 3000-6000r/min are dispersed, and the jitter time in the first sand mill amounts to 2-3h.
In the method b) of the dispersing method of above-mentioned inorganic filler, infiltration is carried out under conditions of not heating, infiltration when
Between be usually 1-11h；In ultrasound infiltration, preferably the temperature of control system is at 10-30 DEG C, to prevent the black item in overheat of blocking
Reunite under part.When dispersing in sand mill, dispersion 0.2-0.5h first preferably is carried out in the revolving speed of 500-1500r/min, then again
The revolving speed to raise speed to 1000-2000r/min is dispersed, and the jitter time in sand mill amounts to 1-2h.
In the method c) of the dispersing method of above-mentioned inorganic filler, the sand milling that flatting silica slurry is added to where carbon black slurry
Continue to amount to 1-2h with the time that the revolving speed of 1000-2000r/min is dispersed in machine.
Compared with prior art, present invention is characterized in that
1, carbon black, flatting silica are first mixed into ultrasound with solvent respectively, the part generated by the cavitation of ultrasonic wave is high
Pressure, impact force and microjet by carbon black, flatting silica surface and gap air and moisture exclude, reduce the interface of filler surface
Tension improves the interfacial bonding property (improving the wetability of filler) of subsequent dispersing agent and resin and filler.
2, carbon black, flatting silica are dispersed with two sand mills respectively, is put in the sand mill for dispersing flatting silica
The zirconium bead diameter set is larger, and flatting silica is prevented to be broken into smaller particle, reduces the extinction of PI film；Using in sand mill
The zirconium pearl compared with small particle is placed, the carbon black of dispersion Nano grade is used it to, by adjusting rate of dispersion and time, carbon black is attached
It is avoided that carbon blacksurface oxide group is detached from while aggressiveness is broken up, to reduce the dispersibility of carbon black.
3, flatting silica is easier to settle, it is found by the applicant that the addition of Nano grade carbon black can reduce flatting silica sinking speed,
Thus by flatting silica be then added to after sand mill is dispersed into appropriate particle size containing in the sand mill where carbon black slurry with charcoal
The black dispersion of low speed together, since the zirconium bead diameter in this sand mill is smaller, continues to break up flatting silica particle without enough energy,
So that the sinking speed of flatting silica can also be reduced while guaranteeing that film matt is spent.
4, the method for the invention can well disperse carbon black and/or flatting silica in solution, inorganic fill out resulting
Expect that dispersed paste is applied in the preparation of black matt PI film, due to solving the dispersibility of filler in black matt PI film
Problem, so that gained black matt PI film be made to have good mechanical performance and electrical strength, shading rate is low and matt degree is good.
By taking the black matt polyimide film with a thickness of 12.5 μm as an example, tensile strength 190-220MPa, elongation at break is
40-52%, electrical strength 116-130kv/mm, light transmittance 0.1-0.2%, (60 °) of glossiness are 26-35.
5, on the other hand, due to the good dispersion of inorganic filler, so that it is not easy to plug filter core in the preparation process of film,
To reduce the replacement frequency of filter core.
Specific embodiment
The present invention is described in further detail combined with specific embodiments below, content to better understand the invention, but
The present invention is not limited to following embodiments.
Embodiment 1: the preparation of inorganic filler dispersed paste
1) 0.54kg flatting silica (silica, average grain diameter are 5 μm) is taken to be placed in 2.55kg aprotic polar solvent
(DMAC) in, ultrasonic (10kHz) infiltrates 1h at room temperature, and ultrasonic device water temperature is controlled at 20-30 DEG C, and gained mixed liquor is placed in first
It in sand mill, is added 0.1kg dispersing agent (hyper-dispersant SUP1400), adds the zirconium pearl that partial size is 1mm, then with 500r/
The revolving speed of min disperses 0.5h, disperses 2h later with the revolving speed of 300+0r/min, obtains flatting silica slurry；
2) 0.54kg carbon black (primary partial size is 20nm) is taken to be placed in 10.26kg aprotic polar solvent (DMAC), room temperature
Lower ultrasound (10kHz) infiltrates 1h, and ultrasonic device water temperature is controlled at 20-30 DEG C, and gained mixed liquor is placed in the second sand mill, is added
0.1kg dispersing agent (hyper-dispersant SUP1400) adds the zirconium pearl that partial size is 0.05mm, then with the revolving speed of 1000r/min point
0.5h is dissipated, 1h is dispersed with the revolving speed of 3000r/min later, obtains carbon black slurry；
3) flatting silica slurry is added in the sand mill where carbon black slurry, 1h is dispersed with the revolving speed of 1000r/min, is obtained
To inorganic filler dispersed paste.
It is tested using partial size of the laser particle size analyzer to inorganic filler dispersed paste obtained by the present embodiment, is as a result shown
Show, 32.67-320nm particle accounts for the 50% of sum, meso-position radius 201nm in slurry；0.85-8.24 μm of particle accounts for total number of particles
50%, meso-position radius is 4.3 μm.Since the additive amount of flatting silica and carbon black is 1:1, by analyzing above substantially, it can be said that in slurry
Carbon black particle partial size be 32.67-320nm, 0.85-8.24 μm.
Comparative example 1: the preparation of inorganic filler dispersed paste
Embodiment 1 is repeated, unlike:
In step 1), addition be partial size be 0.8mm zirconium pearl；
In step 2), addition be partial size be 0.03mm zirconium pearl.
It is tested using partial size of the laser particle size analyzer to inorganic filler dispersed paste obtained by the present embodiment, is as a result shown
Show, 0.101.17 μm of particle accounts for the 50% of sum in slurry, and meso-position radius is 0.67 μm；1.17-26.16 a μm particle accounts for total number of particles
50%, meso-position radius be 16.14 μm.It since the additive amount of flatting silica and carbon black is 1:1, can substantially be obtained, be starched by analyzing above
Carbon black particle partial size is 0.10-1.17 μm in material, and flatting silica partial size is 1.17-26.16 μm.
Comparative example 2: the preparation of inorganic filler dispersed paste
Embodiment 1 is repeated, unlike:
In step 1), addition be partial size be 5.5.mm zirconium pearl；
In step 2), addition be partial size be 0.5mm zirconium pearl.
It is tested using partial size of the laser particle size analyzer to inorganic filler dispersed paste obtained by the present embodiment, is as a result shown
Show: 0.10-0.89 μm of particle accounts for the 50% of sum in slurry, and meso-position radius is 0.46 μm；0.89-7.1 μm of particle accounts for total number of particles
50%, meso-position radius be 3.0 μm.Since the additive amount of flatting silica and carbon black is 1:1, by analyzing above substantially, it can be said that slurry
Middle carbon black particle partial size is 0.10-1.17 μm, and flatting silica partial size is 0.89-7.1 μm.
Embodiment 2: the preparation of inorganic filler dispersed paste
1) 0.54kg flatting silica (silica, average grain diameter are 3 μm) is taken to be placed in 2.55kg aprotic polar solvent
(DMAC) in, ultrasonic (10kHz) infiltrates 3h at room temperature, and ultrasonic device water temperature is controlled at 20-30 DEG C, and gained mixed liquor is placed in first
It in sand mill, is added 0.1kg dispersing agent (hyper-dispersant SUP1400), adds the zirconium pearl that partial size is 3mm, then with 500r/
The revolving speed of min disperses 0.5h, disperses 2h later with the revolving speed of 4500r/min, obtains flatting silica slurry；
2) 0.54kg carbon black (primary partial size is 15nm) is taken to be placed in 10.26kg aprotic polar solvent (DMAC), room temperature
Lower ultrasound (10kHz) infiltrates 6h, and ultrasonic device water temperature is controlled at 20-30 DEG C, and gained mixed liquor is placed in the second sand mill, is added
0.1kg dispersing agent (hyper-dispersant SUP1400) adds the zirconium pearl that partial size is 0.25mm, then with the revolving speed of 1500r/min point
0.5h is dissipated, 1h is dispersed with the revolving speed of 3000r/min later, obtains carbon black slurry；
3) flatting silica slurry is added in the sand mill where carbon black slurry, 1h is dispersed with the revolving speed of 1000r/min, is obtained
To inorganic filler dispersed paste.
It is tested using partial size of the laser particle size analyzer to inorganic filler dispersed paste obtained by the present embodiment, is as a result shown
Show, 32.67-255nm particle accounts for the 50% of sum, meso-position radius 127nm in slurry；1.08-8.37 μm of particle accounts for total number of particles
50%, meso-position radius is 4.3 μm.Since the additive amount of flatting silica and carbon black is 1:1, by analyzing above substantially, it can be said that in slurry
Carbon black particle partial size is 32.67-255nm, and flatting silica partial size is 1.08-8.37 μm.
Embodiment 3: the preparation of inorganic filler dispersed paste
1) 0.54kg flatting silica (titanium dioxide, average grain diameter are 7 μm) is taken to be placed in 2.55kg aprotic polar solvent
(DMAC) in, ultrasonic (10kHz) infiltrates 5h at room temperature, and ultrasonic device water temperature is controlled at 20-30 DEG C, and gained mixed liquor is placed in first
It in sand mill, is added 0.1kg dispersing agent (hyper-dispersant SUP1400), adds the zirconium pearl that partial size is 5mm, then with 500r/
The revolving speed of min disperses 0.5h, disperses 2h later with the revolving speed of 6000r/min, obtains flatting silica slurry；
2) 0.54kg carbon black (primary partial size is 25nm) is taken to be placed in 10.26kg aprotic polar solvent (DMAC), room temperature
Lower ultrasound (10kHz) infiltrates 5h, and ultrasonic device water temperature is controlled at 20-30 DEG C, and gained mixed liquor is placed in the second sand mill, is added
0.1kg dispersing agent (hyper-dispersant SUP1400) adds the zirconium pearl that partial size is 0.45mm, then with the revolving speed of 3000r/min point
0.5h is dissipated, 2h is dispersed with the revolving speed of 6000r/min later, obtains carbon black slurry；
3) flatting silica slurry is added in the sand mill where carbon black slurry, 2h is dispersed with the revolving speed of 3000r/min, is obtained
To inorganic filler dispersed paste.
It is tested using partial size of the laser particle size analyzer to inorganic filler dispersed paste obtained by the present embodiment, is as a result shown
Show, 43.86-295nm particle accounts for the 50% of sum, meso-position radius 198nm in slurry；0.91-9.27 μm of particle accounts for total number of particles
50%, meso-position radius is 4.7 μm.Since the additive amount of flatting silica and carbon black is 1:1, by analyzing above substantially, it can be said that in slurry
Carbon black particle partial size is 43.86-295nm, and flatting silica partial size is 0.91-9.27 μm.
Embodiment 4: preparation inorganic filler dispersed paste
0.54kg carbon black (primary partial size is 20nm) is taken to be placed in 10.26kg aprotic polar solvent (DMAC), at room temperature
Ultrasonic (10kHz) infiltrates 2h, and ultrasonic device water temperature is controlled at 10-20 DEG C, and gained mixed liquor is placed in sand mill, and 0.1kg is added
Dispersing agent (wetting dispersing agent BYK-130) is then added the zirconium pearl that partial size is 0.1mm, is dispersed with the revolving speed of 1200r/min
0.2h disperses 1.5h later with the revolving speed of 2000r/min, and gained carbon black slurry is inorganic filler dispersed paste.
It is tested using partial size of the laser particle size analyzer to inorganic filler dispersed paste obtained by the present embodiment, is as a result shown
Show, particle size carbon black distribution is 51-190nm, meso-position radius 106nm.
Embodiment 5: preparation inorganic filler dispersed paste
0.54kg flatting silica (silica, average grain diameter are 5 μm) is taken to be placed in 2.55kg aprotic polar solvent (DMAC)
In, ultrasonic (10kHz) infiltrates 3h at room temperature, and ultrasonic device water temperature is controlled at 10-15 DEG C, and gained mixed liquor is placed in the first sand mill
In, it is added 0.1kg dispersing agent (hyper-dispersant SUP1400), then adds the zirconium pearl that partial size is 4mm, with turning for 100r/min
Speed dispersion 1h, disperses 1h later with the revolving speed of 3000r/min, obtains flatting silica slurry.
It is tested using partial size of the laser particle size analyzer to inorganic filler dispersed paste obtained by the present embodiment, is as a result shown
Show, flatting silica particle size distribution range is 0.76-7.24 μm, and meso-position radius is 4.01 μm.
For the basic parameter of inorganic filler dispersed paste will be prepared in above-described embodiment 1-5 and comparative example 1-2 convenient for comparison
It arranges in following table 1.
Table 1:
Embodiment 6: the preparation of black matt polyimide film
1) inorganic filler dispersed paste is prepared:
It is prepared by 1 the method for embodiment；
2) it takes 4.308kg diamines (ODA) and 28.19kg aprotic polar solvent (DMF) to be placed in reaction kettle, is added
1.80kg dianhydride (PMDA) opens cooling system, adjusts acid anhydride obtained for step 1) is added when 10,000 centipoises (room temperature) to material viscosity
Inorganic filler dispersed paste continuously adds dianhydride after being stirred to react 3h, until material viscosity is 100,000 centipoises (room temperature), stirring is anti-
3h is answered, polyamic acid resin solution is obtained；
3) gained polyamic acid resin solution is prepared by existing common process through defoaming, salivation, stretching, hot imidization
To the black matt polyimide film with a thickness of 10 μm.
Comparative example 3: the preparation of black matt polyimide film
1) inorganic filler dispersed paste is prepared:
It is prepared by 1 the method for comparative example；
Step 2) and operation 3) are same as Example 6.
Comparative example 4: the preparation of black matt polyimide film
1) inorganic filler dispersed paste is prepared:
It is prepared by 2 the method for comparative example；
Step 2) and operation 3) are same as Example 6.
Comparative example 5: the preparation of black matt polyimide film
1) the zirconium pearl that partial size is 4mm is added in sand mill, by 0.54kg carbon black, 0.54kg flatting silica, 7.41kgDMAC
It is mixed to join in sand mill with 0.2kg dispersing agent (hyper-dispersant SUP1400), 3h is dispersed with the revolving speed of 3000rpm/min, is obtained
To black paste；
2) 4.308kg ODA is dissolved in 33.59kg DMF, 1.8kg PMDA is added after dissolving completely, opens cooling
System is stirred to react 0.5h；When the additional amount of dianhydride is the 90wt% of total amount, black paste made from step 1) is added, stirs
Reaction 2h is mixed, continues to adjust acid anhydride to 100,000 centipoises, is stirred to react 5h, resulting material is after binder, defoaming, through salivation, biaxial tension
The black matt polyimide film with a thickness of 10 μm is made.
Embodiment 7: the preparation of black matt polyimide film
1) inorganic filler dispersed paste is prepared:
It is prepared by 2 the method for embodiment；
2) it takes 4.308kg diamines (ODA) and 28.19kg aprotic polar solvent (DMF) to be placed in reaction kettle, is added
1.80kg dianhydride (PMDA) opens cooling system, adjusts acid anhydride obtained for step 1) is added when 30,000 centipoises (room temperature) to material viscosity
Inorganic filler dispersed paste continuously adds dianhydride after being stirred to react 3h, until material viscosity is 100,000 centipoises (room temperature), stirring is anti-
3h is answered, polyamic acid resin solution is obtained；
3) gained polyamic acid resin solution is prepared by existing common process through defoaming, salivation, stretching, hot imidization
To the black matt polyimide film with a thickness of 10 μm.
Embodiment 8: the preparation of black matt polyimide film
1) inorganic filler dispersed paste is prepared:
It is prepared by 3 the method for embodiment；
2) it takes 4.308kg diamines (ODA) and 28.19kg aprotic polar solvent (DMF) to be placed in reaction kettle, is added
1.80kg dianhydride (PMDA) opens cooling system, adjusts acid anhydride obtained for step 1) is added when 50,000 centipoises (room temperature) to material viscosity
Inorganic filler dispersed paste continuously adds dianhydride after being stirred to react 3h, until material viscosity is 100,000 centipoises (room temperature), stirring is anti-
3h is answered, polyamic acid resin solution is obtained；
3) gained polyamic acid resin solution is prepared by existing common process through defoaming, salivation, stretching, hot imidization
To the black matt polyimide film with a thickness of 10 μm.
The performance of film made from above-described embodiment 6-8 and each comparative example 3-5 is detected, as a result such as following table 2 institute
Show.
Table 2:
Claims (7)
1. a kind of dispersing method of inorganic filler, the inorganic filler includes flatting silica and/or carbon black, it is characterised in that: is adopted
Inorganic filler dispersed paste is obtained with one of following methods a)-c):
Method a): when inorganic filler is flatting silica, dispersing method are as follows: take flatting silica to be placed in aprotic polar solvent, surpass
It is infiltrated under the conditions of sound, gained mixed liquor is placed in sand mill, is added or is added without dispersing agent, and then adding partial size is 1-5mm
Zirconium pearl, dispersed with the revolving speed of 3000-6000r/min, obtain flatting silica slurry；
Method b): when inorganic filler is carbon black, dispersing method are as follows: take carbon black to be placed in aprotic polar solvent, ultrasonic item
It is infiltrated under part, gained mixed liquor is placed in another sand mill, is added or is added without dispersing agent, and then adding partial size is 0.05-
The zirconium pearl of 0.45mm, is dispersed with the revolving speed of 1000-2000r/min, and gained carbon black slurry is the inorganic filler point
Dissipate slurry；
Method c): when inorganic filler includes simultaneously flatting silica and carbon black, first obtaining flatting silica slurry with method a), then with side
Method b) obtains carbon black slurry, is later added to flatting silica slurry in the sand mill where carbon black slurry and continues with 1000-
The revolving speed of 2000r/min is dispersed, and resulting material is the inorganic filler dispersed paste.
2. the dispersing method of inorganic filler according to claim 1, it is characterised in that: method
A) in, the time of infiltration is 1-5h.
3. the dispersing method of inorganic filler according to claim 1, it is characterised in that: method
A) in, the jitter time in sand mill is 2-3h.
4. the dispersing method of inorganic filler according to claim 1, it is characterised in that: method
B) in, the time of infiltration is 1-11h.
5. the dispersing method of inorganic filler according to claim 1, it is characterised in that: method
B) in, the jitter time in sand mill is 1-2h.
6. the dispersing method of inorganic filler according to claim 1, it is characterised in that: method
C) in, flatting silica slurry is added in the sand mill where carbon black slurry continue with the revolving speed of 1000-2000r/min into
The time of row dispersion is 1-2h.
7. the dispersing method of inorganic filler according to claim 1 to 6, it is characterised in that: the dispersing agent
For the dispersing agent with pigment affinity groups.
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| CN112920431A (en) * | 2021-01-26 | 2021-06-08 | 佛山市三水区康立泰无机合成材料有限公司 | Preparation method and application of inorganic water-based filler slurry |
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| CN103231072A (en) * | 2013-04-09 | 2013-08-07 | 昆明理工大学 | Preparation method of silicon dioxide/silver core-shell composite powder for high temperature electronic paste |
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| CN108047717A (en) * | 2017-12-15 | 2018-05-18 | 桂林电器科学研究院有限公司 | A kind of black low gloss Kapton preparation method |
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| CN103231072A (en) * | 2013-04-09 | 2013-08-07 | 昆明理工大学 | Preparation method of silicon dioxide/silver core-shell composite powder for high temperature electronic paste |
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| CN112920431B (en) * | 2021-01-26 | 2023-04-14 | 佛山市三水区康立泰无机合成材料有限公司 | Preparation method and application of inorganic water-based filler slurry |
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