IP Library Granted Patent US 9,265,729
Granted Patent B2
US 9,265,729 · App. 12/734,968 · Granted Feb 23, 2016

Nanofunctional silica particles and manufacturing method thereof

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Quick Facts
Patent No.
US 9,265,729
App. No.
12/734,968
Granted
Feb 23, 2016
Kind
B2
Abstract

Provided are nanofunctional silica particles having excellent functionality and quality, and capable of being mass-produced at low costs. According to the present invention, there are provided nanofunctional silica particles including a coating layer containing one or more silica compounds selected from the group consisting of mercaptopropyl trimethoxysilane (MPS), mercaptopropyl triethoxysilane (MPES), mercaptopropyl methyldimethoxysilane (MPDMS), trimethoxy[2-(7-oxabicyclo[4.1.0]-hept-3-yl)ethyl]silane (EpoPS), thiocyanatopropyl triethoxysilane (TCPS), acryloxypropyl trimethoxysilane (ACPS), and aminopropyl trimethoxysilane (APS); and functional particles in the coating layer, and being used in imaging, assay, diagnosis, treatment or the like, medicine or bioresearch.

Claims (23)

1. Nanofunctional non-porous silica particles, comprising a shell made mainly of silica obtained from one or more organosilica compounds selected from the group consisting of mercaptopropyl trimethoxysilane (MPS), mercaptopropyl triethoxysilane (MPES), mercaptopropyl methyldimethoxysilane (MPDMS), trimethoxy[2-(7-oxabicyclo[4.1.0]-hept-3-yl)ethyl]silane (EpoPS), thiocyanatopropyl triethoxysilane (TCPS), acryloxypropyl trimethoxysilane (ACPS), aminopropyl trimethoxysilane (APS), and aminopropyl triethoxysilane (APES); and a core, in the shell, having a diameter of 2 to 200 nm and containing one or more species selected from the group consisting of a magnetic material, gold colloid, a quantum dot, gadolinium-containing particles, and an imaging functional material-containing liquid, wherein a thickness of the shell is more than 5 nm and less than 100 nm and wherein a functional compound chosen from fluorescent material or an imaging agent is held in the shell and in the core.

2. The nanofunctional non-porous silica particles according to claim 1 , wherein the shell is made of two or more organosilica compounds selected from the group consisting of mercaptopropyl trimethoxysilane (MPS), mercaptopropyl triethoxysilane (MPES), mercaptopropyl methyldimethoxysilane (MPDMS), trimethoxy[2-(7-oxabicyclo[4.1.0]-hept-3-yl)ethyl]silane (EpoPS), thiocyanatopropyl triethoxysilane (TCPS), acryloxypropyl trimethoxysilane (ACPS), aminopropyl trimethoxysilane (APS), and aminopropyl triethoxysilane (APES).

3. The nanofunctional non-porous silica particles according to claim 1 , wherein the thickness of the shell is more than 5 nm and less than 30 nm.

4. The nanofunctional non-porous silica particles according to claim 1 , wherein a difference in surface potential between the shell and the functional compound itself is 3 mV or more.

5. The nanofunctional non-porous silica particles according to claim 1 , wherein each of the nanofunctional non-porous silica particles have a particle diameter of 3 to 500 nm.

6. The nanofunctional non-porous silica particles according to claim 1 , wherein a material having a cell damage activating function is held in the surface of the shell, and/or in the shell, and/or in the core.

7. The nanofunctional non-porous silica particles according to claim 6 , wherein the material is irradiated with light to exhibit the cell damage activating function.

8. A method for manufacturing nanofunctional non-porous silica particles as recited in claim 1 , comprising steps for:

(a) preparing a mixed liquid of an organosilica compound, a functional material, and an aqueous ammonia solution; or preparing a mixed liquid of an organosilica compound, a functional material, a functional compound, and an aqueous ammonia solution, and

(b) allowing the organosilica compound and the aqueous ammonia solution to react with one another at a predetermined temperature, wherein

the organosilica compound is one or more selected from the group consisting of mercaptopropyl trimethoxysilane (MPS), mercaptopropyl triethoxysilane (MPES), mercaptopropyl methyldimethoxysilane (MPDMS), trimethoxy[2-(7-oxabicyclo[4.1.0]-hept-3-yl)ethyl]silane (EpoPS), thiocyanatopropyl triethoxysilane (TcPS), acryloxypropyl trimethoxysilane (ACPS) and aminopropyl trimethoxysilane (APS),

the functional material is one or more species selected from the group consisting of a magnetic material, gold colloid, a quantum dot, gadolinium-containing particles, and an imaging functional material-containing liquid, and wherein

the aqueous ammonia solution and conditions for the temperature in the steps (a) and (b) are adjusted to satisfy the following:

(i) the temperature is high temperature (in the temperature range of 80 to 100° C.), and

(ii) the solution has high ammonia concentration (the solution gives a final concentration of 25% or more).

9. A method for manufacturing nanofunctional non-porous silica particles as recited in claim 1 , comprising steps for:

(a) preparing a mixed liquid of organosilica compounds, a functional material, and an aqueous ammonia solution; or preparing a mixed liquid of organosilica compounds, a functional material, a functional compound, and an aqueous ammonia solution, and

(b) allowing the organosilica compounds and the aqueous ammonia solution to react with each other at a predetermined temperature, wherein

the organosilica compounds are one or more selected from the group consisting of mercaptopropyl trimethoxysilane (MPS), mercaptopropyl triethoxysilane (MPES), mercaptopropyl methyldimethoxysilane (MPDMS), trimethoxy[2-(7-oxabicyclo[4.1.0]-hept-3-yl)ethyl]silane (EpoPS), thiocyanatopropyl triethoxysilane (TcPS), acryloxypropyl trimethoxysilane (ACPS) and aminopropyl trimethoxysilane (APS), and aminopropyl triethoxysilane (APES),

the functional material is one or more species selected from the group consisting of a magnetic material, gold colloid, a quantum dot, gadolinium-containing particles, and an imaging functional material-containing liquid, and wherein

the aqueous ammonia solution and conditions for the temperature in the steps (a) and (b) are adjusted to satisfy the following:

(i) the temperature is high temperature (in the temperature range of 80 to 100° C.), and

(ii) the solution has a high ammonia concentration (the solution gives a final concentration of 25% or more).

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 12, 2016
From: THE UNIVERSITY OF TOKUSHIMA
To: NAKAMURA, MICHIHIRO
Reel/Frame 039705/0133 →
CHANGE OF ENGLISH NAME Recorded Jan 28, 2016
From: THE UNIVERSITY OF TOKUSHIMA
To: TOKUSHIMA UNIVERSITY
Reel/Frame 037630/0710 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 30, 2010
From: NAKAMURA, MICHIHIRO
To: THE UNIVERSITY OF TOKUSHIMA
Reel/Frame 024769/0511 →