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KR-20260066073-A - Method for manufacturing zirconium oxide powder, and zirconium oxide powder

KR20260066073AKR 20260066073 AKR20260066073 AKR 20260066073AKR-20260066073-A

Abstract

The present invention provides a method for producing zirconium oxide powder with excellent dispersibility in organic solvents or resins. The present invention comprises zirconium oxide and the following general formula (1); A method for manufacturing zirconium oxide powder is characterized by comprising a first process of preparing a dispersion by mixing a raw material containing a solvent and a phosphate ester represented by (in Formula (1), R1 represents an alkyl group having 1 to 6 carbon atoms. M represents a hydrogen atom, a metal atom, or an organic base. n is a number from 1 to 8, and k is a number of 1 or 2), and a second process of spray-drying the dispersion obtained in the first process.

Inventors

  • 후지타 유키
  • 오니시 가스미
  • 이에다 다쿠마

Assignees

  • 사카이 가가쿠 고교 가부시키가이샤

Dates

Publication Date
20260512
Application Date
20240910
Priority Date
20230912

Claims (3)

  1. Zirconium oxide and the following general formula (1); [Chemical Formula 1] A first process of preparing a dispersion by mixing a raw material comprising a solvent and a phosphate ester represented by (in Formula (1), R1 represents an alkyl group having 1 to 6 carbon atoms. M represents a hydrogen atom, a metal atom, or an organic base. n is a number from 1 to 8, and k is a number of 1 or 2; and A second process comprising spray-drying the dispersion obtained in the first process A method for manufacturing zirconium oxide powder characterized by the following.
  2. Zirconium oxide and the following general formula (1); [Chemical Formula 2] A first process of preparing a dispersion by mixing a raw material comprising a solvent and a phosphate ester represented by (in Formula (1), R1 represents an alkyl group having 1 to 6 carbon atoms. M represents a hydrogen atom, a metal atom, or an organic base. n is a number from 1 to 8, and k is a number of 1 or 2; and A second process for obtaining zirconium oxide powder by spray-drying the dispersion obtained in the first process, and A third process comprising mixing a composition material including zirconium oxide powder obtained in a second process and a resin. A method for manufacturing a resin composition characterized by the following.
  3. The following general formula (1) ; [Chemical Formula 3] (In formula (1), R1 represents an alkyl group having 1 to 6 carbon atoms. M represents a hydrogen atom, a metal atom, or an organic base. n is a number from 1 to 8, and k is a number of 1 or 2.) comprising zirconium oxide particles surface-treated with a phosphate ester represented by with a bulk density of 1.5 g/cm³ or less Zirconium oxide powder characterized by

Description

Method for manufacturing zirconium oxide powder, and zirconium oxide powder The present invention relates to a method for manufacturing zirconium oxide powder and zirconium oxide powder. More specifically, the invention relates to a method for manufacturing zirconium oxide powder that can be easily dispersed in an organic solvent or resin, and zirconium oxide powder. Zirconium oxide is primarily used as a material to increase the refractive index in optical applications due to its high transparency and refractive index (see Patent Documents 1 to 3). Among these, when used to improve the refractive index of a resin molded body (coating), it is required that the zirconium oxide have good dispersibility in the resin. In conventional technology, an organic solvent dispersion of zirconium oxide is prepared for compatibility purposes, mixed with the resin, and then dispersed in the resin by removing the organic solvent (see Patent Document 4). Hereinafter, preferred embodiments of the present invention will be described in detail, but the present invention is not limited to only those described below, and may be applied with appropriate modifications within the scope of not altering the gist of the present invention. 1. Method for manufacturing zirconium oxide powder The present invention comprises zirconium oxide and the following general formula (1); [Chemical Formula 4] A first process of preparing a dispersion by mixing a raw material comprising a solvent and a phosphate ester represented by (in Formula (1), R1 represents an alkyl group having 1 to 6 carbon atoms. M represents a hydrogen atom, a metal atom, or an organic base. n is a number from 1 to 8, and k is a number of 1 or 2; and This is a method for manufacturing zirconium oxide powder comprising a second process of spray-drying a dispersion obtained in a first process. By manufacturing zirconium oxide powder using this manufacturing method, zirconium oxide powder with excellent dispersibility in organic solvents or resins can be obtained. In the first step of the method for manufacturing zirconium oxide powder according to the present invention, the amount of phosphate ester used is preferably 5 to 40 weight% with respect to 100 weight% of zirconium oxide. By using it in such a ratio, the affinity of the zirconium oxide powder for the resin becomes higher, and thus, when mixed with the resin, the dispersibility becomes better. More preferably, it is 7 to 35 weight% with respect to 100 weight% of zirconium oxide, and even more preferably, 10 to 30 weight%. In the first step of the method for manufacturing zirconium oxide powder according to the present invention, the amount of solvent used is preferably 1 to 3000 weight% with respect to 100 weight% of zirconium oxide. By using it in such a ratio, the affinity of the zirconium oxide powder for the resin becomes higher, and thus, when mixed with the resin, the dispersibility becomes superior. More preferably, it is 50 to 2500 weight% with respect to 100 weight% of zirconium oxide, and even more preferably, 100 to 2000 weight%. The solvent used in the first process above is not particularly limited, but water; Methanol, ethyl alcohol, propyl alcohol, butyl alcohol, pentyl alcohol, hexyl alcohol, heptyl alcohol, octyl alcohol, nonyl alcohol, decyl alcohol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monopropyl ether, propylene glycol monobutyl ether, dipropylene glycol monomethyl ether, ethyl carbitol, butyl carbitol, 2-ethyl-1,3-hexanediol, methyl methoxybutanol, α-terpineol, β-terpineol, hexylene glycol, benzyl alcohol, 2-phenylethyl alcohol, isopalmityl alcohol, isostearyl alcohol, lauryl alcohol, ethylene glycol, Alcohols such as propylene glycol or glycerin; ketone-based solvents such as acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, diacetone alcohol (4-hydroxy-4-methyl-2-pentanone), 2-octanone, isophorone (3,5,5-trimethyl-2-cyclohexen-1-one), or diisobutyl ketone (2,6-dimethyl-4-heptanone); ester-based solvents such as ethyl acetate, butyl acetate, diethyl phthalate, dibutyl phthalate, acetoxyethane, methyl butyrate, methyl hexanoate, methyl octanoate, methyl decanoate, methyl cellosolve acetate, ethylene glycol monobutyl ether acetate, propylene glycol monomethyl ether acetate, ethyl diglycol acetate, 1,2-diacetoxyethane; Ether-based solvents such as tetrahydrofuran, dimethyl ether, diethyl ether, dipropyl ether, ethylene glycol dimethyl ether, ethylene glycol diethyl ether, ethylene glycol dibutyl ether, propylene glycol dimethyl ether, ethoxyethyl ether, 1,2-bis(2-diethoxy)ethane or 1,2-bis(2-methoxyethoxy)ethane; ester ethers such as acetic acid 2-(2-butoxyethoxy)ethane; ether-alcohol-based solvents such as 2-(2-methoxyethoxy)ethanol; hydrocarbon-based solvents such as benzene, toluene, xylene, n-para