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INORGANIC-PARTICLE COMPOSITE, PRODUCTION METHOD THEREFOR, AND INORGANIC-PARTICLE COMPOSITE DISPERSION

Foreign code F190009858
File No. (S2017-0863-N0)
Posted date Jul 26, 2019
Country WIPO
International application number 2018JP038171
International publication number WO 2019074109
Date of international filing Oct 12, 2018
Date of international publication Apr 18, 2019
Priority data
  • P2017-198450 (Oct 12, 2017) JP
  • P2018-033385 (Feb 27, 2018) JP
Title INORGANIC-PARTICLE COMPOSITE, PRODUCTION METHOD THEREFOR, AND INORGANIC-PARTICLE COMPOSITE DISPERSION
Abstract Provided are an inorganic-particle composite exhibiting excellent dispersion stability in a polar solvent, a production method therefor, and an inorganic-particle composite dispersion. This method for producing an inorganic-particle composite includes a step (A) in which a water-soluble salt is added to an inorganic powder and dry mixed or mixed as a paste, and a step (B) in which the same is washed after step (A) to obtain an inorganic-particle composite that contains a component derived from the water-soluble salt, wherein the water-soluble salt is a water-soluble salt for which the acid dissociation constant pKa (H2O) of the acid of the counter anion of the water-soluble salt is greater than zero.
Outline of related art and contending technology BACKGROUND ART
Represented by graphene layered nano-plate, high thermal conductivity and having the conductive adhesive and the like, the functional coating film, including the functionality of the functional material printable ink, a material that is expected to be applied to.
Graphite such as sulfuric acid and nitric acid oxidized violently to synthesize a graphene oxide, and then hydrothermal synthesis, the cleavage of epoxy chain to the size of the graphene is disclosed a method (Non-Patent Document 1). Also, 9,9-bis (substituted aryl) and a water-soluble compound having a fluorene skeleton and a graphene oxide aqueous dispersion using a graphene oxide, graphene sheets to obtain the organic dispersion, an aqueous dispersion of a graphene sheet after mixing with an organic solvent, and recovered by a centrifugal sedimentation graphene sheets through the graphene sheet and a step to obtain a dispersion method of the organic has been disclosed (Patent Document 1). In addition, the graphite was added and the particular ionic liquid, such as microwave irradiation of a method of producing graphene dispersion has been proposed (Patent Document 2).
Also, NMP, DMF or DMSO in the salt was added, high shear, ultrasonic treatment is a method of manufacturing graphene (non-patent document 2), is inserted into the interlayer of graphite salt, an interlayer compound thereof and an ultrasonic wave irradiation in pyridine, a method of manufacturing graphene (non-patent document 3) has been proposed. Further, the active methylene compound and derivatives thereof and the basic compound in a liquid containing a graphene has a laminated structure is immersed in a carbon material, graphite flakes by stirring a method (Patent Document 3), a poly-aromatic hydrocarbon compound and graphite are dispersed in a dispersion of graphene flakes are used (Patent Document 4) a method has been proposed also. In addition, graphite lithium borate, lithium salt and a solvent (Patent Document 5) a method of forming a graphene sheet, a permanganic acid salt in a solvent comprising the steps of dipping the graphite crystal, a method of manufacturing the thin-film graphite or graphene (Patent Document 6) and, fine carbon dispersion liquid containing a polyimide precursor obtained by using fine carbon dispersion composition (Patent Document 7) has been proposed. In addition, the clay mineral is not, as a method to improve the dispersibility of the carbon nanotubes, a method of using a salt with an organic solvent has been proposed (Patent Document 8).
Such as the above-described other manufacturing method using a liquid phase, the production of the nanoparticles by dry grinding method has been proposed. To facilitate grinding of the natural graphite as a method, a vacuum environment or in a nitrogen atmosphere is effective to dry grinding method has been reported (Non-Patent Document 4). In addition, a sulfur-containing environment or an environment containing hydrogen and graphite by dry grinding, the edge portion of the hydrogen atom is bonded to sulfur and graphite nano plate can be obtained and reported (Non-Patent Document 5, Patent Document 9). In addition, NaCl was added during the crushing method for producing a graphite nanosheets (non-patent document 6), nano-diamond by grinding together with NaCl, effective in preventing the aggregation of the nano diamond has been reported (Non-Patent Document 7).
Scope of claims (In Japanese)[請求項1]
 無機粉体に、水溶性塩を加えて乾式またはペースト状で混合する工程(A)と、
 前記工程(A)の後に水洗して、前記水溶性塩由来の成分を含む無機粒子複合体を得る工程(B)とを含み、
 前記水溶性塩は、当該水溶性塩の対アニオンの酸の酸解離定数pKa(H 2O)が0より大きい水溶性塩である無機粒子複合体の製造方法。

[請求項2]
 前記無機粒子複合体は、前記水溶性塩の対カチオン由来の成分を1~100,000ppm含む請求項1に記載の無機粒子複合体の製造方法。

[請求項3]
 前記無機粉体は、層状鉱物粉体、sp 2型炭素材料、金属粉体、セラミックスおよびこれらの酸化物粉体の少なくともいずれかである請求項1又は2に記載の無機粒子複合体の製造方法。

[請求項4]
 前記水溶性塩の対カチオンは、カリウムイオン、ナトリウムイオン、リチウムイオン、バリウムイオン、カルシウムイオン、マグネシウムイオン、ルビジウムイオンおよびアンモニウムイオンのいずれかである請求項1~3のいずれかに記載の無機粒子複合体の製造方法。

[請求項5]
 前記無機粒子複合体を極性溶媒に分散したときの当該無機粒子複合体の平均粒子径が、1000nm以下である請求項1~4のいずれかに記載の無機粒子複合体の製造方法。

[請求項6]
 無機粉体に、水溶性塩を加えて乾式またはペースト状で混合した後に水洗することにより得られ、
 前記水溶性塩は、当該水溶性塩の対アニオンの酸の酸解離定数pKa(H 2O)が0より大きい水溶性塩であり、
 前記水溶性塩由来の成分を含む無機粒子複合体。

[請求項7]
 前記水溶性塩の対カチオン由来の成分を1~100,000ppm含む請求項6に記載の無機粒子複合体。

[請求項8]
 前記無機粉体は、層状鉱物粉体、sp 2型炭素材料、金属粉体、セラミックスおよびこれらの酸化物粉体の少なくともいずれかである、請求項6又は7に記載の無機粒子複合体。

[請求項9]
 前記水溶性塩の対カチオンは、カリウムイオン、ナトリウムイオン、リチウムイオン、バリウムイオン、カルシウムイオン、マグネシウムイオン、ルビジウムイオンおよびアンモニウムイオンのいずれかである請求項6~8のいずれかに記載の無機粒子複合体。

[請求項10]
 極性溶媒に分散したときの平均粒子径が1000nm以下である請求項6~9のいずれかに記載の無機粒子複合体。

[請求項11]
 請求項6~10のいずれかに記載の無機粒子複合体を溶媒に分散した無機粒子複合体分散液。

  • Applicant
  • ※All designated countries except for US in the data before July 2012
  • TOKYO INSTITUTE OF TECHNOLOGY
  • Inventor
  • ARAO Yoshihiko
  • KUBOUCHI Masatoshi
IPC(International Patent Classification)
Specified countries National States: AE AG AL AM AO AT AU AZ BA BB BG BH BN BR BW BY BZ CA CH CL CN CO CR CU CZ DE DJ DK DM DO DZ EC EE EG ES FI GB GD GE GH GM GT HN HR HU ID IL IN IR IS JO KE KG KH KN KP KR KW KZ LA LC LK LR LS LU LY MA MD ME MG MK MN MW MX MY MZ NA NG NI NO NZ OM PA PE PG PH PL PT QA RO RS RU RW SA SC SD SE SG SK SL SM ST SV SY TH TJ TM TN TR TT TZ UA UG US UZ VC VN ZA ZM ZW
ARIPO: BW GH GM KE LR LS MW MZ NA RW SD SL SZ TZ UG ZM ZW
EAPO: AM AZ BY KG KZ RU TJ TM
EPO: AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR
OAPI: BF BJ CF CG CI CM GA GN GQ GW KM ML MR NE SN ST TD TG
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