Process for the surface modification of particles

• US 8,318,120 B2
• Filed: 04/17/2009
• Issued: 11/27/2012
• Est. Priority Date: 04/25/2008
• Status: Active Grant

• Current Assignee: 3M Innovative Properties Company (3M Company)
• Original Assignee: 3M Innovative Properties Company (3M Company)
• Inventors: Nelson, James M., Archibald, Matthew N., Thompson, Wendy L., Tiefenbruck, Grant F.
• Primary Examiner(s): Bos, Steven
• Assistant Examiner(s): Bova, Justin
• Application Number:
  US12/988,092
• Publication Number:
  US 20110048923A1
• Time in Patent Office: 1,320 Days
• Field of Search: 423/335, 423/592.1, 204/157.43, 204/157.5, 204/157.51, 204/157.74, 204/157.73, 204/157.76, 204/157.81, 204/157.75, 556/9, 556/173, 556/466, 219/686, 219/687, 219/756, 977/895, 977/773, 977/775, 977/777, 977/811, 422/186.29, 422/186, 422/186.04, 422/21
• US Class Current: 423/335
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01P 2004/61 Micrometer sized, i.e. from 1-100 micrometer
• CPC Class Codes: C01P 2004/62 Submicrometer sized, i.e. from 0.1-1 micrometer
• CPC Class Codes: C01P 2004/64 Nanometer sized, i.e. from 1-100 nanometer
• CPC Class Codes: C01P 2006/22 Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
• CPC Class Codes: C09C 1/043 Zinc oxide
• CPC Class Codes: C09C 1/3081 Treatment with organo-silicon compounds
• CPC Class Codes: C09C 1/346 Chromium oxides
• CPC Class Codes: C09C 1/3684 Treatment with organo-silicon compounds
• CPC Class Codes: C09C 1/407 Aluminium oxides or hydroxides
• CPC Class Codes: C09C 1/62 Metallic pigments or fillers C09C1/0015 takes precedence
• CPC Class Codes: C09C 3/08 Treatment with low-molecular-weight non-polymer organic compounds C09C3/006, C09C3/048 take precedence
• CPC Class Codes: C09C 3/10 Treatment with macromolecular organic compounds C09C3/006 takes precedence
• CPC Class Codes: C09C 3/12 Treatment with organosilicon compounds C09C3/006 takes precedence

Abstract

A method for the preparation of functionalized particles includes providing a feedstock made of particles, a surface treatment agent reactive with the particles, and solvent. The feedstock is exposed to microwave radiation to heat the feedstock and react the particles with the surface treatment agent to provide the functionalized particles in less than about 60 minutes.

Claims

1. A method for the preparation of functionalized particles, the method comprising:

providing a feedstock at a first temperature, the feedstock comprising particles,

a surface treatment agent reactive with the particles, and a solvent; and

exposing the feedstock to microwave radiation to heat the feedstock and react the particles with the surface treatment agent to provide the functionalized particles in less than about 60 minutes;

wherein exposing the feedstock to microwave radiation occurs;

(i) prior to combining the particles with an organic matrix; and

(ii) in a closed reaction vessel;

wherein the particles in the feedstock comprise silica particles and the surface treatment agent is selected from the group consisting of organosilanes, organotitanates, organozirconates, organoacids, organoamines, organothiols, phosphinic acids and combinations thereof; and

wherein exposing the feedstock to microwave radiation heats the feedstock to a temperature of at least 130°

C.

2. The method according to claim 1 wherein the concentration of particles in the feedstock is between about 20% and about 60% by weight.

3. The method according to claim 1 wherein the particles in the feedstock are substantially symmetric particles and the solvent is water, the feedstock further comprising water-miscible organic solvent.

4. The method according to claim 3 wherein the substantially symmetric particles are substantially spherical particles having an average diameter less than about one micron.

5. The method according to claim 4 wherein the spherical particles comprise a mixture of particles having different diameters.

6. The method according to claim 1, wherein the particles in the feedstock further comprise inorganic oxide selected from the group consisting of zirconia, aluminum oxide, titanium dioxide, iron oxide, zinc oxide, antimony trioxide, boron oxide, boron suboxide, bismuth(III) oxide, copper(I) oxide, copper(II) oxide, chromium(III) oxide, iron(II) oxide, iron (III) oxide, magnesium oxide, manganese(IV) oxide and combinations of two or more of the foregoing.

7. The method according to claim 1, wherein the particles in the feedstock further comprise inorganic sulfide selected from the group consisting of copper(I) sulfide, copper(II) sulfide and zinc sulfide and combinations of two or more of the foregoing.

8. The method according to claim 1 wherein the particles in the feedstock further comprise inorganic materials selected from the group consisting of indium phosphide, aluminum phosphide, brass, metal coated glass, boron carbide, boron nitride, calcium carbide, calcium hydroxide, copper(II) hydroxide, lithium hydroxide, magnesium hydroxide, aluminum, aluminum hydroxide, aluminum sulfate, calcium sulfate, cobalt(II) carbonate, copper(II) carbonate, copper(II) nitrate, copper(II) sulfate, lithium carbonate, lithium nitrate, lithium sulfate, magnesium carbonate, magnesium phosphate, magnesium sulfate, manganese(II) sulfate monohydrate, manganese(II) phosphate, nickel(II) carbonate, nickel(II) hydroxide, nickel(II) nitrate, silicon dioxide, titanium dioxide, zinc carbonate, zinc oxide, zinc sulfate and combinations of two or more of the foregoing.

9. The method according to claim 1 wherein the silica particles in the feedstock are glass beads.

10. The method according to claim 1, wherein the organosilane is selected from the group consisting of [2-(3-cyclohexenyl) ethyl] trimethoxysilane, trimethoxy(7-octen-l-yl) silane, isooctyl trimethoxy-silane, N-(3-triethoxysilylpropyl) methoxyethoxyethoxyethyl carbamate, N-(3-triethoxysilylpropyl) methoxyethoxyethoxyethyl carbamate, 3-(methacryloyloxy)propyltrimethoxysilane, allyl trimethoxysilane, 3-acryloxypropyltrimethoxysilane, 3-(methacryloyloxy)propyltriethoxysilane, 3-(methacryloyloxy) propylmethyldimethoxysilane, 3-acryloyloxypropyl)methyldimethoxysilane, -9-3-(methacryloyloxy)propyldimethylethoxysilane, 3-(methacryloyloxy) propyldimethylethoxysilane, vinyldimethylethoxysilane, phenyltrimethoxysilane, n-octyltrimethoxysilane, dodecyltrimethoxysilane, octadecyltrimethoxysilane, propyltrimethoxysilane, hexyltrimethoxysilane, vinylmethyldiacetoxysilane, vinylmethyldiethoxysilane, vinyltriacetoxysilane, vinyltriethoxysilane, vinyltriisopropoxysilane, vinyltrimethoxysilane, vinyltriphenoxysilane, vinyltri-tbutoxysilane, vinyltris-isobutoxysilane, vinyltriisopropenoxysilane, vinyltris(2-methoxyethoxy)silane, styrylethyltrimethoxysilane, mercaptopropyltrimethoxysilane, 3-glycidoxypropyltrimethoxysilane, acrylic acid, methacrylic acid, oleic acid, stearic acid, dodecanoic acid, 2-[2-(2-methoxyethoxy)ethoxy]acetic acid (MEEAA), betacarboxyethylacrylate, 2-(2-methoxyethoxy)acetic acid, methoxyphenyl acetic acid, and combinations of two or more of the foregoing.

11. The method according to claim 1, wherein exposing the feedstock to microwave radiation provides the functionalized particles in a period of time from about 2 minutes to about 60 minutes, and wherein exposing the feedstock to microwave radiation heats the feedstock to a temperature in the range of 130°

C. to 230°

C., and wherein the feedstock is stirred during the exposing step.