IP Library Granted Patent US 6,986,846
Granted Patent B2
US 6,986,846 · App. 10/932,559 · Granted Jan 17, 2006

Method and apparatus for enhanced size reduction of particles using supercritical fluid liquefaction of materials

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Quick Facts
Patent No.
US 6,986,846
App. No.
10/932,559
Granted
Jan 17, 2006
Kind
B2
Abstract

The present invention provides a method and an apparatus for forming particles using supercritical fluid. The method includes the steps of mixing a load material with a first flow of a supercritical fluid in a first mixing chamber having a primary mixing device disposed therein to form a melt, transferring the melt from the first mixing chamber to a second mixing chamber having a secondary mixing device disposed therein, mixing the melt with a second flow of the supercritical fluid in the second mixing chamber to form a lower viscosity melt, expanding the lower viscosity melt across a pressure drop into an expansion chamber that is at a pressure below the critical pressure of the supercritical fluid to convert the supercritical fluid to a gas and thereby precipitate the load material in the form of particles.

Claims (16)

1. A method of forming particles, the method comprising:

mixing a load material with a first flow of a supercritical fluid in a first mixing chamber having a primary mixing device disposed therein to form a melt;

transferring the melt from the first mixing chamber to a second mixing chamber having a secondary mixing device disposed therein;

mixing the melt with a second flow of the supercritical fluid in the second mixing chamber to form a lower viscosity melt; and

expanding the lower viscosity melt across a pressure drop into an expansion chamber that is at a pressure below the critical pressure of the supercritical fluid to convert the supercritical fluid to a gas and thereby precipitate the load material in the form of particles.

2. The method according to claim 1 wherein the primary mixing device comprises a mechanical agitator.

3. The method according to claim 1 wherein the secondary mixing device comprises a static mixing assembly.

4. The method according to claim 1 wherein the supercritical fluid comprises supercritical carbon dioxide.

5. The method according to claim 4 wherein the load material comprises a biologically active agent and a carrier.

6. The method according to claim 5 wherein the carrier is a biodegradable polymer.

7. The method according to claim 1 wherein the lower viscosity melt passes from the second mixing chamber into the expansion chamber through a nozzle having one or more small apertures formed therein.

8. The method according to claim 1 wherein the load material is dissolved in a solvent prior to being mixed with the supercritical fluid in the first mixing chamber.

9. The method according to claim 8 wherein the solvent is soluble in the supercritical fluid and is extracted from the first mixing chamber before the melt is transferred to the second mixing chamber.

10. The method according to claim 1 further comprising:

contacting the melt with a solvent in the in the second mixing chamber; and

recovering the particles in the expansion chamber as a suspension in the solvent.

Assignments (18)
SECURITY INTEREST Recorded May 2, 2022
From: CHROMAFLO TECHNOLOGIES CORPORATION; FERRO CORPORATION; FERRO ELECTRONIC MATERIALS INC.; PRINCE ENERGY LLC; PRINCE MINERALS LLC; PRINCE SPECIALTY PRODUCTS LLC
To: CREDIT SUISSE AG, CAYMAN ISLANDS BRANCH, AS ADMINISTRATIVE AGENT
Reel/Frame 059845/0082 →
RELEASE OF SECURITY INTEREST IN PATENTS RECORDED AT R/F 041736/0178 Recorded Apr 21, 2022
From: PNC BANK NATIONAL ASSOCIATION, AS COLLATERAL AGENT
To: FERRO CORPORATION
Reel/Frame 059747/0129 →
SECURITY INTEREST Recorded Feb 16, 2017
From: FERRO CORPORATION
To: PNC BANK, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
Reel/Frame 041736/0178 →
RELEASE OF SECURITY INTEREST Recorded Feb 15, 2017
From: PNC BANK, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
To: FERRO CORPORATION
Reel/Frame 041718/0307 →
RELEASE OF SECURITY INTEREST IN PATENT COLLATERAL (RELEASES RF 024804/0117) Recorded Aug 12, 2014
From: PNC BANK, NATIONAL ASSOCIATION (AS SUCCESSOR-BY-MERGER TO NATIONAL CITY BANK)
To: FERRO CORPORATION
Reel/Frame 033522/0839 →
RELEASE OF SECURITY INTEREST IN PATENT COLLATERAL (RELEASES RF 024906/0728) Recorded Aug 12, 2014
From: PNC BANK, NATIONAL ASSOCIATION (AS SUCCESSOR-BY-MERGER TO NATIONAL CITY BANK)
To: FERRO CORPORATION
Reel/Frame 033522/0875 →
PATENT SECURITY AGREEMENT Recorded Aug 12, 2014
From: FERRO CORPORATION
To: PNC BANK, NATIONAL ASSOCIATION
Reel/Frame 033522/0966 →
RELEASE OF SECURITY INTEREST IN PATENT COLLATERAL (RELEASES RF 017527/0047) Recorded Aug 12, 2014
From: PNC BANK, NATIONAL ASSOCIATION (AS SUCCESSOR-BY-MERGER TO NATIONAL CITY BANK)
To: FERRO PFANSTIEHL LABORATORIES, INC.
Reel/Frame 033522/0253 →
RELEASE OF SECURITY INTEREST IN PATENT COLLATERAL (RELEASES RF 017746/0052) Recorded Aug 12, 2014
From: PNC BANK, NATIONAL ASSOCIATION (AS SUCCESSOR-BY-MERGER TO NATIONAL CITY BANK)
To: FERRO PFANSTIEHL LABORATORIES, INC.
Reel/Frame 033522/0284 →
RELEASE OF SECURITY INTEREST IN PATENT COLLATERAL (RELEASES RF 024804/0139) Recorded Aug 12, 2014
From: PNC BANK, NATIONAL ASSOCIATION (AS SUCCESSOR-BY-MERGER TO NATIONAL CITY BANK)
To: FERRO CORPORATION
Reel/Frame 033522/0755 →
AMENDED AND RESTATED PATENT SECURITY AGREEMENT Recorded Aug 30, 2010
From: FERRO CORPORATION
To: PNC BANK NATIONAL ASSOCIATION (AS SUCCESSOR-BY-MERGER TO NATIONAL CITY BANK)
Reel/Frame 024906/0728 →
AFTER-ACQUIRED INTELLECTUAL PROPERTY SECURITY AGREEMENT (SECOND SUPPLEMENTAL FILING) Recorded Aug 6, 2010
From: FERRO CORPORATION
To: PNC BANK, NATIONAL ASSOCIATION (AS SUCCESSOR-BY-MERGER TO NATIONAL CITY BANK), AS COLLATERAL AGENT
Reel/Frame 024804/0139 →
ATTESTATION & CONFIRMATION OF SECURITY INTEREST Recorded Aug 6, 2010
From: FERRO CORPORATION
To: PNC BANK, NATIONAL ASSOCIATION (AS SUCCESSOR-BY-MERGER TO NATIONAL CITY BANK), AS COLLATERAL AGENT
Reel/Frame 024804/0117 →
RELEASE OF SECURITY INTEREST Recorded Sep 29, 2008
From: THE BANK OF NEW YORK MELLON TRUST COMPANY, N.A. (AS SUCCESSOR-IN-INTEREST TO J.P. MORGAN TRUST COMPANY)
To: FERRO CORPORATION
Reel/Frame 021590/0591 →
SECURITY AGREEMENT Recorded Jun 15, 2006
From: FERRO PFANSTIEHL LABORATORIES, INC.
To: J.P. MORGAN TRUST COMPANY, NATIONAL ASSOCIATION, AS TRUSTEE
Reel/Frame 017794/0402 →
SECURITY AGREEMENT Recorded Jun 8, 2006
From: FERRO PFANSTIEHL LABORATORIES, INC.
To: NATIONAL CITY BANK, AS COLLATERAL AGENT
Reel/Frame 017746/0052 →
SECURITY AGREEMENT Recorded Apr 26, 2006
From: FERRO PFANSTIEHL LABORATORIES, INC.
To: NATIONAL CITY BANK, AS ADMINISTRATIVE AGENT
Reel/Frame 017527/0047 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 20, 2004
From: SHEKUNOV, BORIS Y.; CHATTOPADHYAY, PRATIBHASH; SEITZINGER, JEFFREY S.
To: FERRO CORPORATION
Reel/Frame 016091/0894 →