Search

CN-115124043-B - Silica particles and method for producing same

CN115124043BCN 115124043 BCN115124043 BCN 115124043BCN-115124043-B

Abstract

The invention provides silica particles and a method for producing the same. The silica particles contain a nitrogen-containing element compound, wherein in a 29 Si solid-state Nuclear Magnetic Resonance (NMR) spectrum of the silica particles obtained by a cross-polarization magic angle spinning (CP/MAS) method, a ratio C/D of an integrated value C of a signal observed in a range of-50 ppm to-75 ppm to an integrated value D of a signal observed in a range of-90 ppm to-120 ppm is 0.10 to 0.75, an amount X of the nitrogen-containing element compound extracted from the silica particles by using an ammonia/methanol mixed solution is 0.1 mass% to 0.3, and an extraction amount X of the nitrogen-containing element compound and an extraction amount Y of the nitrogen-containing element compound extracted by water satisfy the formula Y/X <0.3.

Inventors

  • ZENITANI YUKA
  • TAKEUCHI TAKASHI
  • SASAKI KOJI
  • Hui Lixiangshi
  • Mai Mochida

Assignees

  • 富士胶片商业创新有限公司

Dates

Publication Date
20260512
Application Date
20220324
Priority Date
20210325

Claims (10)

  1. 1. A silica particle having: silica master particles, and A structure body which is formed by a reaction product of a 3-functional silane coupling agent and which is formed by adsorbing a nitrogen element compound to at least a part of pores of the reaction product of the 3-functional silane coupling agent, and which is coated with at least a part of the surface of the silica master particle, The nitrogen element compound is a nitrogen element compound with positive charging property, The ratio C/D is from 0.10 to 0.75, The ratio C/D is a ratio of an integrated value C of a signal observed in a range of a chemical shift of-50 ppm to-75 ppm to an integrated value D of a signal observed in a range of a chemical shift of-90 ppm to-120 ppm in 29 Si solid Nuclear Magnetic Resonance (NMR) spectrum of silica particles obtained by a cross-polarization magic angle spinning (CP/MAS) method, The amount X of the nitrogen-containing compound extracted from the silica particles using an ammonia/methanol mixed solution is 0.1 mass% or more, and the extraction amount X of the nitrogen-containing compound and the extraction amount Y of the nitrogen-containing compound extracted with water satisfy the formula Y/X <0.3.
  2. 2. The silica particles according to claim 1, wherein the number average particle diameter is 10nm to 200 nm.
  3. 3. The silica particles according to claim 2, wherein the number average particle diameter is 10nm to 80 nm.
  4. 4. The silica particles according to any one of claims 1 to 3, wherein the average roundness is 0.60 to 0.96.
  5. 5. The silica particles according to claim 4, wherein the average roundness is 0.70 or more and 0.92 or less.
  6. 6. The silica particles according to any one of claims 1 to 3, wherein the volume resistivity is 1.0X10- 7 . OMEGA cm or more and 1.0X10- 11.5 . OMEGA cm or less.
  7. 7. The silica particles according to any one of claims 1 to 3, wherein Ra/Rb is 0.01 to 0.8 when the volume resistivity before and after firing at 350 ℃ is Ra and Rb, respectively.
  8. 8. The silica particles according to claim 1 to 3, wherein when the pore volume of pores having a pore diameter of 1nm to 50nm before and after firing at 350 ℃ is set to A and B, respectively, B/A is 1.2 to 5 and B is 0.2cm 3 /g to 3cm 3 /g, The pore volume of the pore diameter of the silica particles before and after firing at 350 ℃ is 1nm to 50nm, which is obtained from the pore distribution curve of the silica particles obtained by the nitrogen adsorption method.
  9. 9. The silica particles according to any one of claims 1 to 3, wherein the nitrogen-containing compound is at least one selected from the group consisting of quaternary ammonium salts, primary amine compounds, secondary amine compounds, tertiary amine compounds, amide compounds, imine compounds, and nitrile compounds.
  10. 10. A method for producing the silica particles according to any one of claims 1 to 9, comprising the steps of: A first step of forming a structure composed of a reaction product of a 3-functional silane coupling agent on at least a part of the surface of the silica master particle, and And a second step of adsorbing a nitrogen element-containing compound to at least a part of pores of a reaction product of the 3-functional silane coupling agent.

Description

Silica particles and method for producing same Technical Field The present invention relates to silica particles and a method for producing the same. Background Silica particles are used as an additive component or main component of powder coatings, cosmetics, rubbers, abrasives, etc., and have functions of, for example, improving resin strength, improving powder flowability, suppressing build-up, etc. For example, japanese patent application laid-open No. 2019-073418 discloses "a hydrophobic silica powder in which (1) the degree of hydrophobization is 50% or more, (2) the extraction amount X of at least one compound selected from the group consisting of quaternary ammonium ions, monoazo-based complexes and inorganic acid ions extracted with a mixed solvent of methanol and an aqueous methanesulfonic acid solution is 0.1% by mass or more, (3) the extraction amount Y of the above X and the above compound extracted with water satisfies the formula (I) Y/X <0.15". In addition, japanese patent application laid-open No. 2017-039618 discloses "a silica powder comprising a plurality of silica particles in which a quaternary ammonium salt is introduced into a silica structure having a" si—o "bond as a repeating unit. Further, japanese patent application laid-open No. 2011-185998 discloses "an external charge control particle comprising a transfer particle formed of hydrophobic spherical silica particles having an average particle diameter of 20 to 500nm obtained by subjecting the surface of hydrophilic spherical silica particles obtained by a sol-gel method to a hydrophobization treatment", and a charge control agent adhering to the surface of the transfer particle ". In addition, japanese patent application laid-open No. 2001-194825 discloses "a silica fine particle obtained by treating spherical hydrophobic silica fine particles having an average primary particle diameter of 0.01 to 5 μm with a compound selected from the group consisting of a quaternary ammonium salt compound, a fluoroalkyl group-containing betaine compound and a silicone oil". In addition, JP-A-09-166884 discloses "particles obtained by treating fine silica particles having a hydrophobization degree of 80% or more with an amphoteric surfactant and particles obtained by treating fine silica particles having a hydrophobization degree of 80% or more with a quaternary ammonium salt or a polymer having a quaternary ammonium group". Disclosure of Invention The present invention provides silica particles having a narrower charge distribution during charging than in the case where the ratio C/D of the integral value C of a signal observed in the range of from-50 ppm to 75ppm and the integral value D of a signal observed in the range of from-90 ppm to-120 ppm is less than 0.10 or greater than 0.75 in a 29 Si solid Nuclear Magnetic Resonance (NMR) spectrum based on a cross-polarization magic angle spinning (CP/MAS) method in silica particles containing a nitrogen-containing element compound, and the ratio X of the extraction amount X of a nitrogen-containing element compound extracted with an ammonia/methanol mixed solution is less than 0.1 MASs% or the extraction amount Y of a nitrogen-containing element compound extracted with water does not satisfy the formula Y/X <0.3, and a method for producing the same. According to claim 1 of the present invention, there is provided silica particles comprising a nitrogen-containing element compound, wherein in a 29 Si solid-state Nuclear Magnetic Resonance (NMR) spectrum of the silica particles obtained by a cross-polarization magic angle spinning (CP/MAS) method, a ratio C/D of an integrated value C of a signal observed in a range of from-50 ppm to-75 ppm to an integrated value D of a signal observed in a range of from-90 ppm to-120 ppm is 0.10 to 0.75, and an amount X of the nitrogen-containing element compound extracted from the silica particles using an ammonia/methanol mixed solution is 0.1 MASs% or more, and an extraction amount X of the nitrogen-containing element compound and an extraction amount Y of the nitrogen-containing element compound extracted with water satisfy the formula Y/X <0.3. According to the 2 nd aspect of the present invention, the silica particles have a number average particle diameter of 10nm to 200 nm. According to the 3 rd aspect of the present invention, the silica particles have a number average particle diameter of 10nm to 80 nm. According to the 4 th aspect of the present invention, the average roundness of the silica particles is 0.60 to 0.96. According to the 5 th aspect of the present invention, the average roundness of the silica particles is 0.70 to 0.92. According to the invention of claim 6, the volume resistivity of the silica particles is 1.0X10 7. OMEGA cm to 1.0X10. 11.5. OMEGA cm. According to claim 7 of the present invention, in the silica particles, ra/Rb is 0.01 to 0.8 when Ra and Rb are set as the volume resistivity before and after firing at 350 ℃. According to cla