JPS62279837A - Manufacture of fine grain type inorganic filler dispersion - Google Patents
Manufacture of fine grain type inorganic filler dispersionInfo
- Publication number
- JPS62279837A JPS62279837A JP61122907A JP12290786A JPS62279837A JP S62279837 A JPS62279837 A JP S62279837A JP 61122907 A JP61122907 A JP 61122907A JP 12290786 A JP12290786 A JP 12290786A JP S62279837 A JPS62279837 A JP S62279837A
- Authority
- JP
- Japan
- Prior art keywords
- dispersion
- inorganic filler
- particulate inorganic
- solvent
- fine grain
- 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.)
- Granted
Links
- 239000006185 dispersion Substances 0.000 title claims abstract description 94
- 239000011256 inorganic filler Substances 0.000 title claims abstract description 48
- 229910003475 inorganic filler Inorganic materials 0.000 title claims abstract description 48
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 239000002904 solvent Substances 0.000 claims abstract description 38
- 150000001408 amides Chemical class 0.000 claims abstract description 28
- 125000003118 aryl group Chemical group 0.000 claims abstract description 19
- 239000002270 dispersing agent Substances 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 38
- 239000000843 powder Substances 0.000 claims description 23
- 239000004408 titanium dioxide Substances 0.000 claims description 19
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000945 filler Substances 0.000 claims description 7
- 239000011164 primary particle Substances 0.000 claims description 7
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 3
- 159000000000 sodium salts Chemical group 0.000 claims description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims 1
- -1 alkyl naphthalenesulfonate Chemical compound 0.000 abstract description 11
- 239000004576 sand Substances 0.000 abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 2
- 150000003871 sulfonates Chemical class 0.000 abstract 3
- 150000004996 alkyl benzenes Chemical class 0.000 abstract 1
- 229940077388 benzenesulfonate Drugs 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 21
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 20
- 239000007864 aqueous solution Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 239000003960 organic solvent Substances 0.000 description 7
- 229920005575 poly(amic acid) Polymers 0.000 description 6
- 238000001132 ultrasonic dispersion Methods 0.000 description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 229920001721 polyimide Polymers 0.000 description 4
- 239000011163 secondary particle Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 238000010494 dissociation reaction Methods 0.000 description 2
- 230000005593 dissociations Effects 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 125000001165 hydrophobic group Chemical group 0.000 description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000005456 alcohol based solvent Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000008055 alkyl aryl sulfonates Chemical class 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 150000004984 aromatic diamines Chemical class 0.000 description 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 125000006267 biphenyl group Chemical group 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000003759 ester based solvent Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 150000000000 tetracarboxylic acids Chemical class 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Landscapes
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Colloid Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
Description
【発明の詳細な説明】
３、発明の詳細な説明
［発明の分野］
本発明は、アミド系溶媒を分散媒とする微粒子状無機フ
ィラー分散液の製造法に関する。さらに詳しくは本発明
は、アミド系溶媒と該溶媒に対して２０重量％以下の一
次粒子径が１．０ｇｍ以下の凝集塊状の微粒子状無機フ
ィラーとを混合して得られた混合物からフィラーの凝集
状態が低下した微粒子状無機フィラー分散液を製造する
方法に関する。Detailed Description of the Invention 3. Detailed Description of the Invention [Field of the Invention] The present invention relates to a method for producing a fine particulate inorganic filler dispersion using an amide solvent as a dispersion medium. More specifically, the present invention is directed to the aggregation of filler from a mixture obtained by mixing an amide solvent and an agglomerated fine particulate inorganic filler having a primary particle size of 1.0 gm or less and 20% by weight or less based on the solvent. The present invention relates to a method for producing a finely divided inorganic filler dispersion.
［発明の背景］
微粒子状の二酸化チタン、シリカなどの微粒子状無機フ
ィラーを易滑剤として含む芳香族ポリイミドフィルムは
、たとえばポリイミドの前駆体であるポリアミック酸（
ポリアミド酸）を溶解状態で、そして微粒子状無機フィ
ラーを分散状態でそれぞれ含むアミド系溶媒からなる組
成物を金属面の上に流延塗布し、得られた塗布膜を加熱
して溶媒の除去と重合・イミド化を行なうような方法に
より得られている。[Background of the Invention] An aromatic polyimide film containing a particulate inorganic filler such as particulate titanium dioxide or silica as a lubricant is made of a polyamic acid (polyamic acid) which is a precursor of polyimide, for example.
A composition consisting of an amide solvent containing poly(amic acid) in a dissolved state and a fine particulate inorganic filler in a dispersed state is cast onto a metal surface, and the resulting coating film is heated to remove the solvent. It is obtained by methods such as polymerization and imidization.
上記のポリアミック酸、微粒子状無機フィラーモしてア
ミド系溶媒を含む組成物は、微粒子状無機フィラーを分
散状態で含むアミド系溶媒分散袋（フィラー分散液）に
ポリアミック酸もしくはポリアミック酸の製造原料（芳
香族テトラカルボン酸成分と芳香族ジアミン成分）を溶
解させて得ることができる。The above-mentioned composition containing polyamic acid, particulate inorganic filler, and amide solvent is prepared by dispersing polyamic acid or a raw material for producing polyamic acid (aromatic It can be obtained by dissolving a group tetracarboxylic acid component and an aromatic diamine component).
上記のフィラー分散液は、微粒子状無機フィラーをアミ
ド系溶媒中に分散させることにより得ることができるが
、その分散操作には従来ではボールミル、サンドミルな
どの機械式分散装置が用いられてきた。すなわち、微粒
子状無機フィラーとアミド系溶媒との混合物を上記のよ
うな機械式分散装置に導入し、これにより分散液を得る
方法が一般的に利用されてきている。The filler dispersion described above can be obtained by dispersing particulate inorganic filler in an amide solvent, and conventionally, mechanical dispersion devices such as ball mills and sand mills have been used for the dispersion operation. That is, a method has generally been used in which a mixture of a particulate inorganic filler and an amide solvent is introduced into a mechanical dispersion device such as the one described above, thereby obtaining a dispersion liquid.
通常の粉末の分散は上記のような機械式分散装置を用い
、所望の均一度になるまで分散操作を行なうことにより
容易に実現できる。しかしながら、本発明者の検討によ
ると、−次粒子径が極度に小さい微粒子状のフィラー粉
末をアミド系溶媒に分散する場合には、上記のような機
械式分散装置による通常の分散操作では、充分な分散が
困難であることがわかった。Ordinary powder dispersion can be easily achieved by using a mechanical dispersion device such as that described above and performing a dispersion operation until a desired degree of uniformity is achieved. However, according to the inventor's study, when dispersing fine particle filler powder with an extremely small secondary particle size in an amide solvent, the normal dispersion operation using the mechanical dispersion device as described above is sufficient. It was found that accurate dispersion was difficult.
すなわち、たとえば−次粒子径が１．ＯＢｍ程度以下の
二酸化チタン、シリカなどの微粒子状無機フィラーは、
通常の粉末状態では二次粒子、三次粒子などの凝集塊と
して存在しており、この微粒子状無機フィラーの凝集塊
は通常の分散操作によっては殆ど凝集がほどけることな
く、はぼそのままの凝集塊として分散液に導入される。That is, for example, if the -order particle diameter is 1. Fine particulate inorganic fillers such as titanium dioxide and silica with an OBm level or below,
In a normal powder state, it exists as an agglomerate of secondary particles, tertiary particles, etc., and the agglomerate of this fine particulate inorganic filler is hardly loosened by normal dispersion operations, and remains as an agglomerate as it is. is introduced into the dispersion as
このため、そのような凝集体を単に分散した分散液の調
製については従来の分散方法は充分に有効であるが、凝
集体の凝集状態が明らかに低下した分散液を得るために
は従来の分散方法は有効とはいえない。勿論、従来の機
械式分散装置を用いる分散方法であっても、その分散条
件（たとえば、付与するせん断心力、分散時間）などを
通常の程度より過酷にすることによって１分散の程度を
向上させることは可能であるが、その分散の向上は僅か
であって、充分とはいえない、またそのような過酷な条
件下にて機械式分散操作を行なった場合、分散装置から
の摩耗粉末の混入が無視できない量となるとの問題もあ
る。For this reason, conventional dispersion methods are sufficiently effective for preparing dispersions in which such aggregates are simply dispersed, but in order to obtain dispersions in which the state of agglomeration of aggregates is clearly reduced, The method cannot be said to be effective. Of course, even in a dispersion method using a conventional mechanical dispersion device, it is possible to improve the degree of dispersion by making the dispersion conditions (for example, applied shear core force, dispersion time) more severe than usual. Although it is possible to improve the dispersion, the improvement in dispersion is small and not sufficient, and when mechanical dispersion is performed under such harsh conditions, there is a risk of contamination by wear particles from the dispersion equipment. There are also problems when the amount becomes too large to ignore.
上記の微粒子状無機フィラーの分散操作における凝集体
の解離の不充分さは、特に無機フィラーの量が少ない場
合に顕著になる。すなわち、たとえば無機フィラーの量
が分散媒体に対して２０重量％程度以下、特に１０重量
％以下のように少ない場合には、機械式分散操作によっ
て無機フィラー凝集体に付与されるせん断心力が低いレ
ベルにとどまるため、凝集体の解離はますます困難にな
る。The insufficient dissociation of aggregates in the dispersion operation of the fine particulate inorganic filler becomes particularly noticeable when the amount of the inorganic filler is small. That is, when the amount of inorganic filler is small, for example, about 20% by weight or less, especially 10% by weight or less, based on the dispersion medium, the shear center force applied to the inorganic filler aggregate by the mechanical dispersion operation is at a low level. dissociation of aggregates becomes increasingly difficult.
前記芳香族ポリイミドフィルム中の微粒子状無機フィラ
ーは易滑剤としてフィルム表面を適度な状態の粗面とす
る（換言すれば、フィルムの表面に適度な大きさの凹凸
を形成する）ために利用される。この場合において、無
機フィラーとして一次粒子径の非常に小さな微粒子状無
機フィラーを用いても、その凝集状態がほどけることな
くフィルム製造用組成物に導入された場合には、そのフ
ィラーは、得られるフィルム内にも同等な凝集状態で導
入されるため、フィルムの表面に形成される凹凸が大き
なものとなり、その充填目的に適合しなくなる。The particulate inorganic filler in the aromatic polyimide film is used as a lubricant to make the film surface appropriately rough (in other words, to form irregularities of an appropriate size on the film surface). . In this case, even if a fine particulate inorganic filler with a very small primary particle size is used as the inorganic filler, if it is introduced into the film manufacturing composition without unraveling its agglomerated state, the filler can be obtained. Since it is introduced into the film in the same agglomerated state, the unevenness formed on the surface of the film becomes large, making it unsuitable for the filling purpose.
［発明の構成］
本発明は、少なくとも一部が凝集状態にある微粒子状無
機フィラーを、その凝集状態をほどきなからアミド系溶
媒に分散して高い分散性を有する分散液を製造するため
の方法を提供することを目的とする。[Structure of the Invention] The present invention provides a method for producing a dispersion liquid having high dispersibility by dispersing fine particulate inorganic filler, at least a part of which is in an agglomerated state, in an amide solvent without undoing the agglomerated state. The purpose is to provide a method.
本発明は特に、少なくとも一部が凝集状態にある微粒子
状無機フィラーを用いて低い濃度の微粒子状無機フィラ
ーのアミド系溶媒分散液を製造する方法であって、その
凝集状態をほどきながらアミド系溶媒に分散して高い分
散性を有する分散液を製造する方法を提供することを目
的とする。In particular, the present invention is a method for producing an amide-based solvent dispersion of a particulate inorganic filler at a low concentration using a particulate inorganic filler in which at least a part of the particulate inorganic filler is in an agglomerated state. It is an object of the present invention to provide a method for producing a dispersion liquid having high dispersibility by dispersing it in a solvent.
本発明は、アミド系溶媒と該溶媒に対して２０重量％以
下の一次粒子径が１．０ルｍ以下の凝集塊状の微粒子状
無機フィラーとを混合して得られた混合物を分散操作に
かけてフィラー分散液を調製するに際して、該混合物中
に芳香族スルホン酸塩系分散剤を（１０５〜５重量％そ
して水を０．０５〜５重量％、それぞれ存在させた状態
で分散操作を施すことを特徴とする微粒子状無機フィラ
ー分散液の製造法からなる。The present invention involves dispersing a mixture obtained by mixing an amide solvent and an agglomerated fine particulate inorganic filler having a primary particle size of 1.0 lm or less by 20% by weight or less based on the solvent. When preparing a dispersion liquid, a dispersion operation is carried out in the presence of an aromatic sulfonate dispersant (105 to 5% by weight and 0.05 to 5% by weight of water, respectively) in the mixture. This method consists of a method for producing a fine particulate inorganic filler dispersion.
上記の微粒子状無機フィラー分散液の製造法は微粒子状
無機フィラーをアミド系溶媒中に０．１〜ＩＯ重量％の
範囲の濃度で含まれる分散液を製造する際に特に有利で
ある。The above-described method for producing a finely divided inorganic filler dispersion is particularly advantageous when producing a dispersion in which a finely divided inorganic filler is contained in an amide solvent at a concentration ranging from 0.1 to IO% by weight.
次に、本発明について詳しく説明する。Next, the present invention will be explained in detail.
本発明において分散対象とされる微粒子状無機フィラー
は、−次粒子径が１．０ＪＬｍ以下の凝集塊状の微粒子
状無機フィラーであり、その例としては、微粒子状の銅
粉末、亜鉛粉末、アルミニウム粉末、鉄粉末、コバルト
粉末、ニッケル粉末などの金属粉末、微粒子状の二酸化
チタン粉末、二酸化ケイ素（シリカ）粉末、酸化マグネ
シウム粉末、酸化アルミニウム（アルミナ）粉末、酸化
亜鉛粉末などの無機酸化物粉末、微粒子状の窒化ケイ素
粉末、窒化チタン粉末などの無機窒化物粉末、炭化ケイ
素粉末、炭化チタン粉末、炭化タングステン粉末などの
無機酸化物粉末、および微粒子状の炭酸カルシウム粉末
、硫酸カルシウム粉末、硫酸バリウム粉末のなど無機塩
粉末を挙げることができる。これらの微粒子状無機フィ
ラーは二種以上組合せて使用されてもよい、本発明で用
いられるアミド系溶媒は芳香族ポリイミドの製造用とし
て用いられるものであり１その代表例としては、ジメチ
ルアセトアミド、ジメチルホルムアミド、Ｎ−メチルピ
ロリドンなどを挙げることができるが１分子内にアミド
結合を有する有機溶媒である限り特に限定はない、また
、アミド系溶媒は、たとえばアルコール系溶媒、ケトン
系溶媒、エーブル系溶媒、エステル系溶媒、炭化水素系
溶媒、ハロゲン化炭化水素系溶媒などの各種の公知の有
機溶媒を含んでいてもよい、ただし、これらの有機溶媒
がアミド系溶媒と混合される場合には、該有機溶媒は全
体量の５０重量％以下であることが好ましく、特に２０
重量％以下であることが好ましい、なお、本発明におい
て用いる芳香族スルホン酸塩系分散剤は水に対して高い
溶解性を示すため、アミド系溶媒中に少量の水（全体量
の０．０５〜２重量％、特に好ましくは０．１５〜１．
５重量％）が存在していることが、本発明の目的である
高い分散効果をもたらすために必要である。The particulate inorganic filler to be dispersed in the present invention is an agglomerated particulate inorganic filler with a secondary particle size of 1.0 JLm or less, and examples thereof include particulate copper powder, zinc powder, and aluminum powder. , metal powders such as iron powder, cobalt powder, and nickel powder, inorganic oxide powders such as finely divided titanium dioxide powder, silicon dioxide (silica) powder, magnesium oxide powder, aluminum oxide (alumina) powder, zinc oxide powder, and fine particles. Inorganic nitride powder such as silicon nitride powder, titanium nitride powder, inorganic oxide powder such as silicon carbide powder, titanium carbide powder, tungsten carbide powder, and fine particulate calcium carbonate powder, calcium sulfate powder, barium sulfate powder. Examples include inorganic salt powder. These particulate inorganic fillers may be used in combination of two or more kinds.The amide solvent used in the present invention is used for producing aromatic polyimide.1 Typical examples thereof include dimethylacetamide, dimethyl Examples include formamide, N-methylpyrrolidone, etc., but there is no particular limitation as long as it is an organic solvent that has an amide bond in one molecule.Amide solvents include, for example, alcohol solvents, ketone solvents, and able solvents. may contain various known organic solvents such as ester solvents, hydrocarbon solvents, and halogenated hydrocarbon solvents; however, when these organic solvents are mixed with amide solvents, The organic solvent is preferably 50% by weight or less of the total amount, particularly 20% by weight or less.
It is preferable that the amount is less than % by weight. Since the aromatic sulfonate dispersant used in the present invention exhibits high solubility in water, a small amount of water (0.05% of the total amount) is added to the amide solvent. ~2% by weight, particularly preferably 0.15-1.
5% by weight) is necessary to provide the high dispersion effect which is the aim of the present invention.
本発明においては、アミド系溶媒への微粒子状無機フィ
ラーの分散補助剤として芳香族スルホン酸塩系分散剤が
用いられる。In the present invention, an aromatic sulfonate-based dispersant is used as a dispersion aid for a particulate inorganic filler in an amide-based solvent.
芳香族スルホン酸塩系分散剤は、ベンゼン、ナフタリン
、アントラセン、ジフェニルなどのような芳香環あるい
はこれを水素添加した炭素環を少なくとも一個有し、通
常はこれにアルキル基などの鎖状の疎水基が結合してな
る大きな疎水基単位と親水性のスルホン酸塩が結合して
なるものである。上記のアルキル基は通常は分岐鎖もし
くは直鎖の炭素数１〜１８のアルキル基である。Aromatic sulfonate dispersants have at least one aromatic ring such as benzene, naphthalene, anthracene, diphenyl, or a hydrogenated carbon ring, and usually have a chain hydrophobic group such as an alkyl group attached thereto. It is made up of a large hydrophobic group unit formed by bonding to a hydrophilic sulfonate. The alkyl group mentioned above is usually a branched or straight chain alkyl group having 1 to 18 carbon atoms.
芳香族スルホン酸塩系分散剤の例としては、アルキルベ
ンゼンスルホン酸塩、アルキルナフタリンスルホン酸塩
、アルキルナフタリンスルホン酸塩のホルマリン縮合物
、アルキルテトラヒドロナフタリンスルホン酸塩、アル
キルジフェニルスル。Examples of aromatic sulfonate-based dispersants include alkylbenzenesulfonates, alkylnaphthalenesulfonates, formalin condensates of alkylnaphthalenesulfonates, alkyltetrahydronaphthalenesulfonates, and alkyldiphenylsulfonates.
ホン酸塩、アルキルアリールスルホン酸塩のケトン化合
物を挙げることができる。Examples include ketone compounds such as phonates and alkylarylsulfonates.
芳香族スルホン酸塩系分散剤としては、芳香族スルホン
酸塩のアルカリ金属塩（ナトリウム塩、カリウム塩など
）、芳香族スルホン酸のアンモニウム塩、あるいは芳香
族スルホン酸と有機アミン化合物との塩を用いることが
好ましい。As aromatic sulfonate dispersants, alkali metal salts of aromatic sulfonates (sodium salts, potassium salts, etc.), ammonium salts of aromatic sulfonic acids, or salts of aromatic sulfonic acids and organic amine compounds are used. It is preferable to use
本発明において用いる芳香族スルホン酸塩系分散剤とし
て特に好ましいのは、アルキルナフタリンスルホン醜ナ
トリウム塩のホルマリン縮合物である。Particularly preferred as the aromatic sulfonate dispersant used in the present invention is a formalin condensate of an alkylnaphthalene sulfone ugly sodium salt.
アミド系溶媒と該溶媒に対して２０重量％以下の−次粒
子径が１．０ｇｍ以下の凝集塊状の微粒子状無機フィラ
ーとを混合して得られた混合物を分散操作にかけてフィ
ラー分散液を調製するに際して、有機溶媒に溶解しやす
い公知のポリカルボン酸系分散剤などの通常の有機溶媒
系用分散剤を用いた場合には、その分散効果は充分でな
く、このような一般的な有機溶媒系用分散剤は通常の分
散操作を利用する限り１本発明の目的である微粒子状無
機フィラーの高度な分散を達成することができない、ま
た、通常の有機溶媒系用分散剤を用いた場合には、高度
に分散された分散液が一旦生成しても、短時間のうちに
再凝集が発生する傾向がある。A filler dispersion liquid is prepared by dispersing the mixture obtained by mixing an amide solvent and an agglomerated fine particulate inorganic filler having a secondary particle size of 1.0 gm or less, which is 20% by weight or less based on the solvent. When using conventional dispersants for organic solvent systems, such as known polycarboxylic acid dispersants that are easily soluble in organic solvents, the dispersion effect is not sufficient; Dispersants for organic solvents cannot achieve the high degree of dispersion of particulate inorganic fillers, which is the objective of the present invention, unless ordinary dispersion operations are used. , even once a highly dispersed dispersion is formed, reaggregation tends to occur within a short time.
本発明の分散液の製造法は、まず、アミド系溶媒と該ア
ミド系溶媒に対して２０重量％以下の微粒子状無機フィ
ラーと芳香族スルホン酸塩系分散剤（通常は１０〜５０
重量％濃度の水溶液として導入）とを混合して混合物を
得たのち、これに分散操作を施すことにより実施する。The method for producing the dispersion of the present invention involves firstly including an amide solvent, a particulate inorganic filler of 20% by weight or less based on the amide solvent, and an aromatic sulfonate dispersant (usually 10 to 50% by weight).
(introduced as an aqueous solution at a concentration of % by weight) to obtain a mixture, which is then subjected to a dispersion operation.
なお、本発明の分散液の製造法は特に、アミド系溶媒と
該アミド系溶媒に対して０．１〜１０ｉ量％の微粒子状
無機フィラーとを混合した混合物から所望の分散液を調
製する場合に特に有効である。Note that the method for producing a dispersion liquid of the present invention is particularly applicable when a desired dispersion liquid is prepared from a mixture of an amide solvent and a particulate inorganic filler in an amount of 0.1 to 10i% based on the amide solvent. It is particularly effective for
アミド系溶媒と微粒子状無機フィラーとの混合物は通常
の添加操作により得ることができる。なお、この混合物
には所望により公知の分散剤を併用してもよい。A mixture of an amide solvent and a particulate inorganic filler can be obtained by a conventional addition operation. Note that a known dispersant may be used in combination with this mixture if desired.
上記のようにして得られたアミド系溶媒と微粒子状無機
フィラーとの混合物には１次に分散操作が施される０分
散操作は機械式分散装置あるいは超音波分散装置を単独
で、あるいは組合せて用いることにより行なうことがで
きる。特に、機械式分散操作と超音波分散操作とをこの
順に組合せた分散操作によることが好ましい。The mixture of the amide solvent and the particulate inorganic filler obtained as described above is subjected to a primary dispersion operation. This can be done by using In particular, it is preferable to use a dispersion operation that combines a mechanical dispersion operation and an ultrasonic dispersion operation in this order.
上記の機械式分散操作は公知の機械式分散装置を利用し
て行なわれる。利用することのできる機械式分散装置の
例としては、ボールミル、サンドミル、自動乳鉢、ロー
ルミル、インペラーミル、ホモジナイザーなどを挙げる
ことができる。このような機械式分散装置は、一般に回
転数７００〜１２０００ｒμｍの条件にて回転して固体
粒子の分散を行なう装置である。The above mechanical dispersion operation is carried out using a known mechanical dispersion device. Examples of mechanical dispersion devices that can be utilized include ball mills, sand mills, automatic mortars, roll mills, impeller mills, homogenizers, and the like. Such a mechanical dispersion device is generally a device that rotates at a rotational speed of 700 to 12,000 rpm to disperse solid particles.
本発明にｔおける機械式分散操作はは２０分間〜２時間
程度で実施することが望ましい、この分散操作を長時間
実施すると１分散装置の摩耗粉末が少なからぬ量で分散
液に混入することがある。The mechanical dispersion operation in the present invention is preferably carried out for about 20 minutes to 2 hours. If this dispersion operation is carried out for a long time, a considerable amount of worn powder from one dispersion device may be mixed into the dispersion liquid. be.
本発明にて利用することのできる超音波分散操作は、超
音波洗浄やエマルジョンの調製などの目的にて、既に利
用されている操作である。このような操作は公知の超音
波振動子を用いて行なわれる１本発明における超音波分
散操作は、強い分散箋力を達成するために１５〜３０Ｋ
Ｈｚ程度の低い周波数にて行なうことが望ましい、また
、超音波分散操作は約１５分間〜１０時間の範囲の操作
時間にて行なうことが望ましい、なお、超音波分散操作
によって分散液の液温か上昇する傾向があるため、超音
波分散操作が施される装置は冷却下に置くことが望まし
い。The ultrasonic dispersion operation that can be used in the present invention is an operation that has already been used for purposes such as ultrasonic cleaning and emulsion preparation. Such an operation is performed using a known ultrasonic transducer.1 The ultrasonic dispersion operation in the present invention is carried out at 15 to 30K in order to achieve a strong dispersion force.
It is desirable to perform the ultrasonic dispersion operation at a low frequency of about Hz, and it is desirable to carry out the ultrasonic dispersion operation for an operation time in the range of about 15 minutes to 10 hours. Therefore, it is desirable to keep the equipment where ultrasonic dispersion operations are performed under cooling.
［発明の効果］
アミド系溶媒と微粒子状無機フィラーとを混合して得ら
れた混合物からフィラー分散液を調製するに際して、本
発明に従って芳香族スルホン酸塩系分散剤を特定量そし
て水を特定量、それぞれ存在させた状態で分散操作を施
すことによって、均一な分散と凝集体の低減とが達成さ
れた分散液を容易に得ることができる。[Effect of the invention] When preparing a filler dispersion from a mixture obtained by mixing an amide solvent and a particulate inorganic filler, according to the present invention, a specific amount of an aromatic sulfonate dispersant and a specific amount of water are added. By carrying out a dispersion operation in the presence of each of them, it is possible to easily obtain a dispersion liquid in which uniform dispersion and reduction of aggregates are achieved.
また、本発明に従って得られた分散液は再凝集が発生し
にくく、長期にわたって安定な分散液として存在すると
の利点もある。Further, the dispersion obtained according to the present invention has the advantage that re-agglomeration is difficult to occur and it exists as a stable dispersion for a long period of time.
［実施例と比較例］
［実施例１］
ジメチルアセトアミド４９４ｇとアルキルナフタリンス
ルホン酸ナトリウム塩のホルマリン縮合物の４０重量％
水溶液３．５ｇとを容量１文のビーカーに入れ、ホモミ
キサーを用いａｏｏ。[Examples and Comparative Examples] [Example 1] 40% by weight of formalin condensate of 494 g of dimethylacetamide and sodium alkylnaphthalene sulfonate
Place 3.5 g of the aqueous solution in a 1-liter beaker and mix using a homo mixer.
ｒμｍの回転速度で３分間、攪拌混合した０次に一次粒
子径０．０３ｇｍの二酸化チタン２．５ｇを加えてホモ
ミキサーを用いて８０００ｒμｍの回転速度で１時間攪
拌して分散を行なった。2.5 g of titanium dioxide having a primary particle size of 0.03 gm, which had been stirred and mixed at a rotational speed of 8000rpm for 3 minutes using a homomixer, was added and dispersed by stirring for 1 hour at a rotational speed of 8000rpm.
得られた分散液中の二酸化チタンの平均粒子径は０．７
５ｇｍ（堀場製作所■製遠心沈降弐粒径分布測定装置Ｃ
ＡＰＡ−５００による測定値、以下同じ）であった。The average particle size of titanium dioxide in the obtained dispersion was 0.7
5gm (Centrifugal sedimentation 2 particle size distribution measuring device C manufactured by Horiba, Ltd.)
The value measured by APA-500 (the same applies hereinafter).
［比較例１］
アルキルナフタリンスルホン酸ナトリウム塩のホルマリ
ン縮合物の水溶液を添加しなかった以外は実施例１と同
様にして、二酸化チタンの分散操作を行なった。[Comparative Example 1] Titanium dioxide was dispersed in the same manner as in Example 1 except that an aqueous solution of a formalin condensate of alkylnaphthalene sulfonic acid sodium salt was not added.
得られた分散液中の二酸化チタンの平均粒子径は１．６
ルｍであった。The average particle size of titanium dioxide in the obtained dispersion was 1.6.
It was Lem.
［比較例２］
アルキルナフタリンスルホン酸ナトリウム塩のホルマリ
ン縮合物の水溶液の代りに有機溶媒溶解性アクリル系カ
ルボン酸分散剤を１．５ｇ添加した以外は実施例１と同
様にして、二酸化チタンの分散操作を行なった。 得ら
れた分散液中の二酸化チタンの平均粒子径は１．０ｇｍ
であった。[Comparative Example 2] Dispersion of titanium dioxide was carried out in the same manner as in Example 1, except that 1.5 g of an organic solvent-soluble acrylic carboxylic acid dispersant was added instead of the aqueous solution of the formalin condensate of sodium alkylnaphthalene sulfonate. performed the operation. The average particle size of titanium dioxide in the obtained dispersion was 1.0 gm.
Met.
［実施例２］
ジメチルアセトアミド９７．３ｇとアルキルナフタリン
スルホン酸ナトリウム塩のホルマリン縮合物の４０重量
％水溶液０．７ｇとを容量２００ｍ１のビーカーに入れ
、スターラチップを用いて５分間、攪拌混合した０次に
一次粒子径０．４４１７−ｍの二酸化チタン（表面にア
ルミナ処理が施されたもの）２．０ｇを加え、超音波洗
浄器（ＢＲＡＮＳＯＮ社製、ウルトラクリーナ）で２時
間分散を行なった。[Example 2] 97.3 g of dimethylacetamide and 0.7 g of a 40% by weight aqueous solution of a formalin condensate of sodium alkylnaphthalene sulfonate were placed in a beaker with a capacity of 200 ml, and mixed with stirring for 5 minutes using a stirrer tip. Next, 2.0 g of titanium dioxide (surface treated with alumina) having a primary particle size of 0.4417-m was added and dispersed for 2 hours using an ultrasonic cleaner (Ultra Cleaner, manufactured by BRANSON).
得られた分散液中の二酸化チタンの平均粒子径は０．５
５１Ｌｍであった。The average particle size of titanium dioxide in the obtained dispersion was 0.5
It was 51 Lm.
［比較例３］
アルキルナフタリンスルホン酸ナトリウム塩のホルマリ
ン縮合物の水溶液を添加しなかった以外は実施例２と同
様にして、二酸化チタンの分散操作を行なった。[Comparative Example 3] Titanium dioxide was dispersed in the same manner as in Example 2, except that an aqueous solution of a formalin condensate of alkylnaphthalene sulfonic acid sodium salt was not added.
得られた分散液中の二酸化チタンの平均粒子径は１．９
ルｍであった。The average particle size of titanium dioxide in the obtained dispersion was 1.9.
It was Lem.
［実施例３］
ジメチルアセトアミド４７５０ｇ、アルキルナフタリン
スルホン酸ナトリウム塩のホルマリン縮合物の４０重量
％水溶液５０ｇ、そして−次粒子径０．０４涛ｍの酸化
ケイ素を回転型攪拌機を用い５分間、攪拌混合した。次
に超音波ホモジナイザー（日本精機製作所輛製、ＲＵＳ
６００）で４．５時間の分散を行なった。[Example 3] 4750 g of dimethylacetamide, 50 g of a 40% by weight aqueous solution of a formalin condensate of sodium alkylnaphthalene sulfonate, and silicon oxide with a particle diameter of 0.04 m were mixed by stirring for 5 minutes using a rotary stirrer. did. Next, use an ultrasonic homogenizer (manufactured by Nippon Seiki Seisakusho, RUS).
600) for 4.5 hours.
得られた分散液中の酸化ケイ素の平均粒子径は０．０９
１Ｌｍであった。The average particle diameter of silicon oxide in the obtained dispersion was 0.09
It was 1 Lm.
［実施例４］
ジメチルアセトアミド９７．８ｇとアルキルナフタリン
スルホン酸ナトリウム塩のホルマリン縮合物の４０重量
％水溶液０．７ｇとを容量２００ｍｆＬのビーカーに入
れ、スターラチ７プを用いて５分間、Ｗｌ、拌混合した
０次に、−次粒子径０゜０３ｇｍの二酸化チタン２．０
ｇを加え、超音波洗浄器（ウルトラクリーナ）で２時間
の分散を行なった。[Example 4] 97.8 g of dimethylacetamide and 0.7 g of a 40% by weight aqueous solution of a formalin condensate of sodium alkylnaphthalene sulfonate were placed in a beaker with a capacity of 200 mfL, and stirred for 5 minutes using a stirrer tip. Mixed 0-order and -order particle size 0゜03gm titanium dioxide 2.0
g was added thereto, and dispersion was carried out for 2 hours using an ultrasonic cleaner (Ultra Cleaner).
得られた分散液中の二酸化チタンの平均粒子径は０．２
６μｍであった。この分散液を１日間そして９日間静置
したのち、再度平均粒子径の測定を行なったところ平均
粒子径はそれぞれ０．２８１１ ｍシ０ り７ ｕ ｍ
で訊４１ 木質的か介什り士坊められす、この分散液
が長期にわたって安定であることがわかった。The average particle size of titanium dioxide in the obtained dispersion was 0.2
It was 6 μm. After this dispersion was allowed to stand for 1 day and then for 9 days, the average particle size was measured again, and the average particle size was 0.2811 m and 7 μm, respectively.
This dispersion was found to be stable over a long period of time.
［比較例４］
アルキルナフタリンスルホン酸ナトリウム塩のホルマリ
ン縮合物の水溶液の代りに有機溶媒溶解性ポリカルボン
酸分散剤を０．３ｇ添加した以外は実施例４と同様にし
て、二酸化チタンの分散操作を行なった。 得られた分
散液中の二酸化チタンの平均粒子径は０．１２．４ｍで
あった。この分散液を１日間と９日間静置したのち、再
度平均粒子径の測定を行なったところ平均粒子径はそれ
ぞれ０．９５ルｍと１．７５ルｍであり、明らかな再凝
集が認められた。[Comparative Example 4] Dispersion of titanium dioxide was performed in the same manner as in Example 4, except that 0.3 g of an organic solvent-soluble polycarboxylic acid dispersant was added instead of the aqueous solution of formalin condensate of alkylnaphthalene sulfonate sodium salt. I did it. The average particle diameter of titanium dioxide in the obtained dispersion was 0.12.4 m. After this dispersion was allowed to stand for 1 day and 9 days, the average particle diameter was measured again. Ta.
［実施例５］
二酸化チタンの代りに一次粒子径が０．０１６４ｍの酸
化マグネシウムを用いた以外は実施例４と同様にして、
酸化マグネシウムの分散操作を行なった。[Example 5] Same as Example 4 except that magnesium oxide with a primary particle size of 0.0164 m was used instead of titanium dioxide,
A dispersion operation of magnesium oxide was performed.
得られた分散液中の酸化マグネシウムの平均粒子径は０
．４０ｇｍであった。この分散液を１日間と９日間静置
したのち、再度平均粒子径の測定を行なったところ平均
粒子径はそれぞれ０．４０ＪＬｍと０．３フルｍであり
、実質的な変化は認められず、この分散液が長期にわた
って安定であることがわかった。The average particle size of magnesium oxide in the obtained dispersion was 0.
．． It was 40gm. After this dispersion was allowed to stand for 1 day and 9 days, the average particle diameter was measured again, and the average particle diameter was 0.40 JLm and 0.3 full m, respectively, and no substantial change was observed. This dispersion was found to be stable over long periods of time.
Claims (1)
次粒子径が１．０μｍ以下の凝集塊状の微粒子状無機フ
ィラーとを混合して得られた混合物を分散操作にかけて
フィラー分散液を調製するに際して、該混合物中に芳香
族スルホン酸塩系分散剤を０．０５〜５重量％そして水
を０．０５〜５重量％、それぞれ存在させた状態で分散
操作を施すことを特徴とする微粒子状無機フィラー分散
液の製造法。 ２、芳香族スルホン酸塩系分散剤がアルキルナフタリン
スルホン酸のナトリウム塩であることを特徴とする特許
請求の範囲第１項記載の微粒子状無機フィラー分散液の
製造法。 ３、凝集塊状の微粒子状無機フィラーの混合量がアミド
系溶媒に対して０．１〜１０重量％の範囲にあることを
特徴とする特許請求の範囲第１項記載の微粒子状無機フ
ィラー分散液の製造法。 ４、微粒子状無機フィラーが微粒子状二酸化チタン粉末
、酸化ケイ素粉末、アルミナ粉末あるいは酸化マグネシ
ウム粉末であることを特徴とする特許請求の範囲第１項
記載の微粒子状無機フィラー分散液の製造法。[Claims] 1. Dispersion operation of a mixture obtained by mixing an amide solvent and an agglomerated fine particulate inorganic filler having a primary particle size of 1.0 μm or less at 20% by weight or less based on the solvent When preparing a filler dispersion liquid, a dispersion operation is performed in a state in which 0.05 to 5% by weight of an aromatic sulfonate dispersant and 0.05 to 5% by weight of water are present in the mixture. A method for producing a fine particulate inorganic filler dispersion, characterized by: 2. The method for producing a particulate inorganic filler dispersion according to claim 1, wherein the aromatic sulfonate-based dispersant is a sodium salt of alkylnaphthalene sulfonic acid. 3. The fine particulate inorganic filler dispersion according to claim 1, wherein the amount of the particulate inorganic filler in the form of aggregates is in the range of 0.1 to 10% by weight based on the amide solvent. manufacturing method. 4. The method for producing a fine particulate inorganic filler dispersion according to claim 1, wherein the fine particulate inorganic filler is a fine particulate titanium dioxide powder, silicon oxide powder, alumina powder, or magnesium oxide powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61122907A JPH0615032B2 (en) | 1986-05-27 | 1986-05-27 | Method for producing fine particle inorganic filler-dispersion liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61122907A JPH0615032B2 (en) | 1986-05-27 | 1986-05-27 | Method for producing fine particle inorganic filler-dispersion liquid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62279837A true JPS62279837A (en) | 1987-12-04 |
| JPH0615032B2 JPH0615032B2 (en) | 1994-03-02 |
Family
ID=14847562
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61122907A Expired - Lifetime JPH0615032B2 (en) | 1986-05-27 | 1986-05-27 | Method for producing fine particle inorganic filler-dispersion liquid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0615032B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100807165B1 (en) | 2005-09-30 | 2008-02-27 | 에어 프로덕츠 앤드 케미칼스, 인코오포레이티드 | Use of 2,3-dihydroxynaphthalene-6-sulfonic acid salts as dispersants |
| JP2017074556A (en) * | 2015-10-14 | 2017-04-20 | 永嶋 良一 | Decomposition method of aggregation structure, and manufacturing method of primary particles or/and fine aggregates constituted of primary particles including the decomposition method as process |
| CN115806747A (en) * | 2022-11-19 | 2023-03-17 | 中信钛业股份有限公司 | Preparation method of titanium dioxide pigment for photovoltaic back panel film |
-
1986
- 1986-05-27 JP JP61122907A patent/JPH0615032B2/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100807165B1 (en) | 2005-09-30 | 2008-02-27 | 에어 프로덕츠 앤드 케미칼스, 인코오포레이티드 | Use of 2,3-dihydroxynaphthalene-6-sulfonic acid salts as dispersants |
| JP2017074556A (en) * | 2015-10-14 | 2017-04-20 | 永嶋 良一 | Decomposition method of aggregation structure, and manufacturing method of primary particles or/and fine aggregates constituted of primary particles including the decomposition method as process |
| CN115806747A (en) * | 2022-11-19 | 2023-03-17 | 中信钛业股份有限公司 | Preparation method of titanium dioxide pigment for photovoltaic back panel film |
| CN115806747B (en) * | 2022-11-19 | 2024-03-29 | 中信钛业股份有限公司 | Preparation method of titanium dioxide pigment for photovoltaic backboard film |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0615032B2 (en) | 1994-03-02 |
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