# US 8,541,485 B2 · Process for making filled resins

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- Number: US 8,541,485 B2
- Document ID: US8541485B2
- Status: Granted
- Kind: B2
- Application number: 13/263,283
- Filed: 2010-05-24
- Published: 2012-03-08
- Granted: 2013-09-24
- Earliest claimed: 2009-05-26
- Assignees: 3M Innovative Properties Company
- Applicants: James M. Nelson; Matthew N. Archibald; Wendy L. Thompson; Jeremy A. Miller; Randy A. Larson; Terence D. Spawn
- Inventors: James M. Nelson; Matthew N. Archibald; Wendy L. Thompson; Jeremy A. Miller; Randy A. Larson; Terence D. Spawn
- Web page: https://patentgrep.com/patent/US8541485B2

## CPC

- B01J 19/1887: {forming a thin film}
- B01D 1/222: {In rotating vessels; vessels with movable parts}
- B01J 19/1862: {placed in series}
- B01J 19/2415: {Tubular reactors}
- C08J 3/2053: {the additives only being premixed with a liquid phase}
- C08J 3/215: at least one additive being also premixed with a liquid phase
- B01J 2219/0004: Processes in series
- B01J 2219/00094: Jackets
- B01J 2219/00765: Baffles attached to the reactor wall
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)

## Abstract

A method of making a filled resin includes the steps of: Providing a wiped film evaporator with an internal evaporator chamber maintained under vacuum and having an internal chamber wall maintained at an elevated temperature; introducing solvent-borne particles and organic matrix into the internal chamber; and compounding the solvent-borne particles and the organic matrix in the internal evaporator chamber by forming a thin film against the internal chamber wall, the thin film including organic matrix and particles, and the vacuum conditions and elevated temperature being sufficient to remove solvent from the particles and organic matrix to provide the filled resin. Less than about 10% of the particles in the resulting filled resin are agglomerated.

## Claims

### Claim 1

A method of making a filled resin, comprising:
providing a wiped film evaporator comprising an internal evaporator chamber maintained under vacuum conditions and an internal chamber wall maintained at an elevated temperature;
introducing solvent-borne particles and organic matrix into the internal chamber; and
compounding the solvent-borne particles and the organic matrix in the internal evaporator chamber by forming a thin film against the internal chamber wall, the thin film comprised of organic matrix and particles, the vacuum conditions and elevated temperature being sufficient to remove solvent from the particles and organic matrix to provide the filled resin;
wherein, less than about 10% of the particles in the filled resin are agglomerated; and
wherein, the organic matrix comprises a thermoset or an ethylenically-unsaturated crosslinkable resin.

### Claim 2 (depends on 1)

The method of claim 1, wherein the process further comprises functionalizing the particles prior to compounding, and wherein functionalizing the particles comprises treating the particles with surface-modifying agent to provide functionalized solvent-borne particles.

### Claim 3 (depends on 2)

The method of claim 2, wherein the particles have an average thickness up to about 30 micrometers.

### Claim 4 (depends on 2)

The method of claim 2, wherein the particles comprise nanoparticles having an average thickness less than about 500 nm.

### Claim 5 (depends on 4)

The method of claim 4, wherein the nanoparticles comprise functionalized silicon dioxide.

### Claim 6 (depends on 4)

The method of claim 4, wherein the nanoparticles comprise functionalized calcium carbonate.

### Claim 7 (depends on 1)

The method of claim 1, further comprising pre-mixing the solvent-borne particles and the organic matrix prior to introducing particles and organic matrix into the internal chamber of the wiped film evaporator.

### Claim 8 (depends on 1)

The method of claim 1, further comprising:
providing a feedstock by combining
(i) untreated particles,
(ii) surface-modifying agent reactive with the particles, and
(iii) solvent; and
reacting the untreated particles with the surface-modifying agent in the feedstock to provide solvent-borne functionalized particles; and
combining the solvent-borne functionalized particles and the organic matrix to provide a mixture;
wherein, introducing solvent-borne particles and organic matrix into the internal chamber comprises directing the mixture into the internal chamber of the wiped film evaporator.

### Claim 9 (depends on 8)

The method of claim 8, wherein providing a feedstock further comprises adding rubber nano-domains.

### Claim 10 (depends on 9)

The method of claim 9, wherein the rubber nano-domains comprise core-shell rubber nanoparticles, the shell of the nanoparticles having a glass transition temperature at least 50° C. and the core having a glass transition temperature no greater than −20° C.

### Claim 11 (depends on 10)

The method of claim 10, wherein the shell comprises a material selected from the group consisting of an acrylic polymer, an acrylic copolymer, a styrenic polymer, and a styrenic copolymer.

### Claim 12 (depends on 1)

The method of claim 1, wherein the particles comprise inorganic materials selected from the group consisting of metal, oxide, sulfide, carbonate, antimonide, inorganic salt, nitride, metal-coated particle and combinations of two or more of the foregoing.

### Claim 13 (depends on 1)

The method of claim 1, wherein the particles comprise organic materials selected from the group consisting of carbon black, organic pigments and combinations thereof.

### Claim 14 (depends on 1)

The method of claim 1 wherein the particles comprise inorganic oxides selected from the group consisting of zirconium dioxide—ZrO2, aluminum oxide—Al2O3, cerium (IV) oxide—CeO2, titanium dioxide—TiO2, iron(II) oxide—FeO, iron(II,III) oxide—Fe3O4, iron(III) oxide—Fe2O3, zinc oxide—ZnO, silicon dioxide (silica)—SiO2, antimony trioxide—Sb2O3, boron oxide—B2O3, boron suboxide—B6O, bismuth(III) oxide—Bi2O3, copper(I) oxide—Cu2O, copper(II) oxide—CuO, chromium(III) oxide—Cr2O3, iron(II) oxide—FeO, iron (III) oxide—Fe2O3, magnesium oxide—MgO, manganese(IV) oxide (manganese dioxide—MnO2) and combinations of two or more of the foregoing.

### Claim 15 (depends on 1)

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

### Claim 16 (depends on 1)

The method of claim 1 wherein the particles comprise material 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.

### Claim 17 (depends on 1)

The method of claim 1 wherein the particles comprise metal oxides selected from the group consisting of titania, alumina, zirconia, vanadia, chromia, iron oxide, antimony oxide, tin oxide and mixtures of two or more of the foregoing.

### Claim 18 (depends on 17)

The method of claim 17 wherein the metal oxide particles are functionalized with organosilane surface-modifying agent(s) selected from the group consisting of polyethylene glycol(trimethoxy)silane, phenyltrimethoxysilane, 3-methacryloxypropyltrimethoxysilane and combinations of two or more of the foregoing.

### Claim 19 (depends on 1)

The method of claim 1 wherein the organic matrix comprises epoxy resin.

### Claim 20 (depends on 1)

The method of claim 1 wherein the organic matrix comprises ethylenically-unsaturated crosslinkable resin.