IP Library Granted Patent US 7,122,503
Granted Patent B2
US 7,122,503 · App. 11/051,744 · Granted Oct 17, 2006

Uniform microcapsules

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Quick Facts
Patent No.
US 7,122,503
App. No.
11/051,744
Granted
Oct 17, 2006
Kind
B2
Abstract

The present invention teaches an improved process for preparing a population of microcapsules having a substantially uniform size distribution, especially useful for manufacture of carbonless paper. The improved process teaches use of membrane material having a pre-selected pore size in the capsule manufacture process. A core material is provided along with a receiving solution for receiving the core material. The receiving solution is a nonsolvent for the core material. The core material is passed under pressure through the membrane into a moving or turbulent receiving solution forming uniform droplets of core material dispersed in the receiving solution. Wall-forming material is added to the receiving solution for coating the core material droplets. The coating on the droplets is polymerized forming microcapsules. This novel process also lends itself to microcapsule formation in a continuous process.

Claims (13)

1. A population of microcapsules having a substantially uniform size distribution and a mean diameter wherein at least 90% of the microcapsules on a numerical basis are within ±1 micron of the mean diameter, said population of microcapsules being useful for manufacture of carbonless paper,

said microcapsules produced by providing a membrane having a selected pore size,

providing a core material wherein the core material is a hydrophobic material and solvent for a chromogenic material,

providing an aqueous solution for receiving the core material,

passing the core material under pressure through said membrane into the aqueous solution to form uniform droplets of core material dispersed in the aqueous solution,

adding wall-forming material to the aqueous solution to coat the core material droplets to form microcapsules,

heating the microcapsules to polymerize the wall material,

adjusting the pH to harden the wall material.

2. The microcapsules according to claim 1 wherein the wall forming material is comprised of two reactive wall forming components, the first wall forming reactive component is dissolved in the core material, the second wall forming component is dissolved in the receiving solution.

3. The microcapsules according to claim 2 wherein the two reactive wall forming components comprise a diacid and a diol, a diester and a diol, a metal salt of dibasic acid and a dihalide, glycol ester and diacid, diacid chloride and diol, ethylene carbonate and diacid, anhydride and diol, diphenol and diacid, diacetate of diphenol and diacid, alkali metal salt of diphenol and a diacid halogen, a diamine and a dianhydride, a tetramine and a dianhydride.

4. The microcapsules according to claim 1 wherein the core material comprises a chromogen and a solvent selected from a dialkyl phathalate, alkyl biphenyl, alkyl benzene, diaryl ether, di(aralkyl)ether, aryl aralkyl ether, alkyl ketone, alkyl benzoate, aralkyl benzoate, alkylated naphthalene, a partially hydrogenated terphenyl, a vegetable oil, and a vegetable oil ester.

5. The microcapsules according to claim 1 wherein the wall-forming material comprises a material comprises a material selected from a gellable colloid, carboxy methyl cellulose, gelatin, gelatin-gum arabic, melamine formaldehyde, methylol melamine, urea formaldehyde, dimethylol urea, methylated dimethylol urea, methylated melamine formaldehyde, methylated methylol melamine, a gelatin-anionic polymer, alkylacrylate-acrylic acid copolymer, or reaction product with any of the foregoing.

6. The microcapsules according to claim 1 wherein the microcapsules have a broadness index of less than 1.0.

Assignments (33)
RELEASE OF SECURITY INTEREST Recorded Oct 7, 2021
From: CREDIT SUISSE AG, CAYMAN ISLANDS BRANCH, AS COLLATERAL AGENT
To: ENCAPSYS, LLC; IPS STRUCTURAL ADHESIVES, INC.; IPS CORPORATION; WATERTITE PRODUCTS, INC.; WELD-ON ADHESIVES, INC.; IPS ADHESIVES LLC
Reel/Frame 057750/0945 →
CORRECTIVE ASSIGNMENT TO CORRECT THE APPLICATION NUMBER SERIAL NUMBER PREVIOUSLY RECORDED AT REEL: 44444 FRAME: 0932. ASSIGNOR(S) HEREBY CONFIRMS THE SECOND LIEN SECURITY AGREEMENT. Recorded Aug 8, 2019
From: ENCAPSYS, LLC; IPS STRUCTURAL ADHESIVES, INC.; IPS CORPORATION; WATERTITE PRODUCTS, INC.; WELD-ON ADHESIVES, INC.; IPS ADHESIVES LLC
To: CREDIT SUISSE AG, CAYMAN ISLANDS BRANCH, AS SECOND LIEN COLLATERAL AGENT
Reel/Frame 050021/0359 →
CORRECTIVE ASSIGNMENT TO CORRECT THE PROPERTY NUMBER PREVIOUSLY RECORDED AT REEL: 49891 FRAME: 807. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT. Recorded Aug 8, 2019
From: CREDIT SUISSE AG, CAYMAN ISLANDS BRANCH, AS ADMINISTRATIVE AGENT
To: ENCAPSYS, LLC; IPS STRUCTURAL ADHESIVES, INC.; IPS CORPORATION; WATERTITE PRODUCTS, INC.; WELD-ON ADHESIVES, INC.; IPS ADHESIVES LLC
Reel/Frame 050003/0400 →
CORRECTIVE ASSIGNMENT TO CORRECT THE APPLICATION NUMBER SERIAL NUMBER PREVIOUSLY RECORDED AT REEL: 44444 FRAME: 0905. ASSIGNOR(S) HEREBY CONFIRMS THE FIRST LIEN SECURITY AGREEMENT. Recorded Aug 8, 2019
From: ENCAPSYS, LLC; IPS STRUCTURAL ADHESIVES, INC.; IPS CORPORATION; WATERTITE PRODUCTS, INC.; WELD-ON ADHESIVES, INC.; IPS ADHESIVES LLC
To: CREDIT SUISSE AG, CAYMAN ISLANDS BRANCH, AS FIRST LIEN COLLATERAL AGENT
Reel/Frame 050021/0307 →
RELEASE OF SECURITY INTEREST IN PATENTS Recorded Jul 1, 2019
From: CREDIT SUISSE AG, CAYMAN ISLANDS BRANCH, AS ADMINISTRATIVE AGENT
To: ENCAPSYS, LLC; IPS STRUCTURAL ADHESIVES, INC.; IPS CORPORATION; WATERTITE PRODUCTS, INC.; WELD-ON ADHESIVES, INC.; IPS ADHESIVES LLC
Reel/Frame 049891/0807 →
RELEASE OF PATENT COLLATERAL AGREEMENT Recorded Jun 17, 2018
From: JEFFERIES FINANCE LLC, AS ADMINISTRATIVE AGENT
To: APPVION, INC.; PAPERWEIGHT DEVELOPMENT CORP.
Reel/Frame 046377/0195 →
RELEASE OF SECOND LIEN PATENT COLLATERAL AGREEMENT Recorded Jun 17, 2018
From: U.S. BANK NATIONAL ASSOCIATION, AS COLLATERAL AGENT
To: APPVION, INC.; PAPERWEIGHT DEVELOPMENT CORP.
Reel/Frame 046377/0179 →
RELEASE OF SECURITY INTEREST Recorded Jun 17, 2018
From: JEFFERIES FINANCE LLC, AS ADMINISTRATIVE AGENT
To: APPVION, INC.; PAPERWEIGHT DEVELOPMENT CORP.
Reel/Frame 046392/0438 →
FIRST LIEN SECURITY AGREEMENT Recorded Nov 14, 2017
From: ENCAPSYS, LLC; IPS STRUCTURAL ADHESIVES, INC.; IPS CORPORATION; WATERTITE PRODUCTS, INC.; WELD-ON ADHESIVES, INC.; IPS ADHESIVES LLC
To: CREDIT SUISSE AG, CAYMAN ISLANDS BRANCH, AS FIRST LIEN COLLATERAL AGENT
Reel/Frame 044444/0905 →
RELEASE OF SECURITY INTEREST Recorded Nov 14, 2017
From: BANK OF AMERICA, N.A., AS ADMINISTRATIVE AGENT
To: ENCAPSYS, LLC
Reel/Frame 044123/0160 →
SECOND LIEN SECURITY AGREEMENT Recorded Nov 14, 2017
From: ENCAPSYS, LLC; IPS STRUCTURAL ADHESIVES, INC.; IPS CORPORATION; WATERTITE PRODUCTS, INC.; WELD-ON ADHESIVES, INC.; IPS ADHESIVES LLC
To: CREDIT SUISSE AG, CAYMAN ISLANDS BRANCH, AS SECOND LIEN COLLATERAL AGENT
Reel/Frame 044444/0932 →
RELEASE OF SECURITY INTEREST Recorded Feb 1, 2017
From: WILMINGTON TRUST, NATIONAL ASSOCIATION
To: ENCAPSYS, LLC
Reel/Frame 041144/0570 →
SECURITY INTEREST Recorded Aug 27, 2015
From: ENCAPSYS, LLC
To: WILMINGTON TRUST, NATIONAL ASSOCIATION, AS ADMINISTRATIVE AGENT
Reel/Frame 036437/0821 →
SECURITY INTEREST Recorded Aug 7, 2015
From: ENCAPSYS, LLC
To: BANK OF AMERICA, N.A., AS ADMINISTRATIVE AGENT
Reel/Frame 036275/0792 →
CHANGE OF NAME Recorded Aug 6, 2015
From: RISE ACQUISTION, LLC
To: ENCAPSYS, LLC
Reel/Frame 036303/0617 →
RELEASE OF SECURITY INTEREST Recorded Aug 4, 2015
From: JEFFERIES FINANCE LLC, AS ADMINISTRATIVE AGENT
To: APPVION, INC.; PAPERWEIGHT DEVELOPMENT CORP.
Reel/Frame 036251/0893 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 4, 2015
From: APPVION, INC.
To: RISE ACQUISTION, LLC
Reel/Frame 036245/0688 →
RELEASE OF SECURITY INTEREST Recorded Aug 4, 2015
From: U.S. BANK NATIONAL ASSOCIATION, AS COLLATERAL AGENT
To: APPVION, INC.; PAPERWEIGHT DEVELOPMENT CORP.
Reel/Frame 036249/0419 →
RELEASE OF SECURITY INTEREST Recorded Aug 4, 2015
From: JEFFERIES FINANCE LLC, AS ADMINISTRATIVE AGENT
To: APPVION, INC.; PAPERWEIGHT DEVELOPMENT CORP.
Reel/Frame 036250/0466 →
RELEASE OF SECURITY INTEREST Recorded Aug 4, 2015
From: JEFFERIES FINANCE LLC, AS ADMINISTRATIVE AGENT
To: APPVION, INC.; PAPERWEIGHT DEVELOPMENT CORP.
Reel/Frame 036250/0630 →
PATENT COLLATERAL AGREEMENT Recorded Nov 21, 2013
From: APPVION, INC.; PAPERWEIGHT DEVELOPMENT CORP.
To: JEFFERIES FINANCE LLC
Reel/Frame 031694/0323 →
RELEASE OF SECURITY INTEREST Recorded Nov 20, 2013
From: U.S. BANK NATIONAL ASSOCIATION
To: APPLETON PAPERS INC.
Reel/Frame 031690/0774 →
SECOND LIEN PATENT COLLATERAL AGREEMENT Recorded Nov 19, 2013
From: APPVION, INC.; PAPERWEIGHT DEVELOPMENT CORP.
To: U.S. BANK NATIONAL ASSOCIATION
Reel/Frame 031689/0593 →
SECURITY AGREEMENT Recorded Jul 3, 2013
From: APPVION, INC.; PAPERWEIGHT DEVELOPMENT CORP.
To: JEFFERIES FINANCE LLC, AS ADMINISTRATIVE AGENT
Reel/Frame 030740/0153 →
RELEASE OF SECURITY INTEREST Recorded Jul 1, 2013
From: U.S. BANK NATIONAL ASSOCIATION
To: APPLETON PAPERS, INC.; PAPERWEIGHT DEVELOPMENT CORP.; AMERICAN PLASTICS COMPANY; NEW ENGLAND EXTRUSIONS, INC.
Reel/Frame 030724/0312 →
RELEASE OF SECURITY INTEREST Recorded Jun 28, 2013
From: FIFTH THIRD BANK
To: APPLETON PAPERS, INC.
Reel/Frame 030712/0054 →
CHANGE OF NAME Recorded Jun 17, 2013
From: APPLETON PAPERS INC.
To: APPVION, INC.
Reel/Frame 030641/0381 →
RELEASE OF SECURITY INTEREST Recorded Feb 11, 2010
From: BANK OF AMERICA, N.A., AS ADMINISTRATIVE AGENT
To: APPLETON PAPERS INC.
Reel/Frame 023915/0760 →
SECURITY AGREEMENT Recorded Feb 9, 2010
From: PAPERWEIGHT DEVELOPMENT CORP.; APPLETON PAPERS INC.; AMERICAN PLASTICS COMPANY, INC.; NEW ENGLAND EXTRUSION INC.
To: U.S. BANK NATIONAL ASSOCIATION
Reel/Frame 023905/0953 →
SECURITY AGREEMENT Recorded Feb 8, 2010
From: APPLETON PAPERS INC.
To: FIFTH THIRD BANK, AS ADMINISTRATIVE AGENT
Reel/Frame 023905/0532 →
GRANT OF SECURITY INTEREST Recorded Oct 7, 2009
From: APPLETON PAPERS INC.
To: U.S. BANK NATIONAL ASSOCIATION, AS COLLATERAL AGENT
Reel/Frame 023337/0132 →
NOTICE OF GRANT OF SECURITY INTEREST Recorded Jun 29, 2007
From: APPLETON PAPERS INC.
To: BANK OF AMERICA, N.A., AS ADMINISTRATIVE AGENT
Reel/Frame 019489/0751 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 4, 2005
From: SEEHAFER, TROY RONALD; STAHLER, GEORGE ARTHUR
To: APPLETON PAPERS INC.
Reel/Frame 016419/0363 →