US4777154A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Hollow microspheres made from dispersed particle compositions and their production
Assignee: Individual
•
Filing: 1986-07-28
•
Granted: 1988-10-11
•
Expires: 2006-07-28
Abstract
Abstract Hollow microspheres are made by a process which comprises forming a film of a dispersed particle film-forming composition (containing dispersed particles, a binder, a film stabilizing agent and a continuous liquid phase) across a coaxial blowing nozzle, applying a blowing gas at a positive pressure on the inner surface of the dispersed particle composition film to blow the film and form, in the region of the coaxial blowing nozzle orifice, hollow dispersed particle microspheres having stable film walls, removing the hollow microspheres, treating them to bring dispersed particles into point to point contact and harden them to obtain hollow green microspheres, and subsequently subjecting them to a sufficiently high temperature for a sufficient period of time to remove the continuous liquid phase and to sinter the dispersed particles at their points of contact to form within the walls of said hollow microspheres interconnecting voids that are continuous from the outer wall surface to the inner wall surface of the hollow microspheres, and to obtain hollow porous microspheres having substantially uniform void content and substantially uniform distribution of the voids in their walls.
Inventors
- 👤 Leonard B. Torobin
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-26 21:05
CPC Classifications
B; B01; B01J; B01J20/00; B01J20/28; B01J20/28054; B01J20/28095; B01J20/28097; B01J13/00; B01J13/02; B01J13/04; B01J13/20; B01J13/22; B01J20/28002; B01J20/28004; B01J20/28014; B01J20/28016; B01J20/28021; B01J20/2803; B22; B22F; B22F1/00; B22F1/06; B22F1/065; B22F1/0655; B22F1/08; B29; B29C; B29C49/00; B29C49/0005; B29C49/0042; B29C49/42; B29C49/46; B29C70/00; B29C70/58; B29C70/66; C; C03; C03B; C03B19/00; C03B19/10; C03B19/107; C03B19/1075; C03B19/108; C03B19/1085; C03B37/00; C03B37/01; C03B37/02; C03B37/022; C03B37/04; C03B37/075; C03B37/0756; C03C; C03C11/00; C03C11/002; C03C17/00; C03C17/06; C03C17/09; C04; C04B; C04B14/00; C04B14/02; C04B14/04; C04B14/22; C04B14/24; C04B18/00; C04B18/02; C04B18/027; C04B20/00; C04B20/10; C04B20/1055; C04B38/00; C04B38/08; C04B41/00; C04B41/45; C04B41/4584; C08; C08J; C08J9/00; C08J9/32; F; F24; F24S; F24S80/00; F24S80/50; F24S80/52; F24S80/525; F24S80/60; B01J35/00; B01J35/50; B01J35/51; B01J35/52; B29C2049/4602; B29C2049/4605; B29C2049/465; B29C2049/4655; B29C2049/4664; B29K; B29K2105/00; B29K2105/06; B29K2105/16; B29K2105/165; C03B2203/00; C03B2203/10; C03B2203/14; C03B2203/16; Y; Y02; Y02E; Y02E10/00; Y02E10/40; Y10; Y10S; Y10S521/00; Y10S521/919; Y10T; Y10T428/00; Y10T428/29; Y10T428/2982; Y10T428/2984; Y10T428/2989
Claims Analysis
Total Claims: 43
Claim 1
Independent Claim
269 words
A method for making hollow green microspheres of 200 to 10,000 micron diameter and of 1 to 1000 microns wall thickness from a stable dispersion of a dispersed particle film forming composition, said composition comprising dispersed particles in a continuous liquid phase, said method comprising feeding said dispersed particle composition and a blowing gas to a coaxial blowing nozzle, said coaxial blowing nozzle having an inner coaxial nozzle for said blowing gas and an outer coaxial nozzle for said dispersed particle composition and a coaxial blowing nozzle orifice, feeding said blowing gas to said inner nozzle, feeding said dispersed particle composition to said outer nozzle to blow and form, in the region of said coaxial blowing nozzle orifice, hollow dispersed particle composition microspheres having stable film walls, removing said hollow microspheres from the region of said coaxial blowing nozzle orifice, surface tension forces acting on said hollow microspheres to cause said hollow microspheres to form a spherical shape, said dispersed particle composition forming the walls of said hollow microspheres and said dispersed particles being uniformly dispersed in said continuous liquid phase, treating said removed hollow microspheres to remove a portion of the continuous liquid phase to bring the dispersed particles into point to point contact and to harden them, said dispersed particles being of sufficient size and in a sufficient amount such that the dispersed particles in the walls of the hollow microspheres link up and form a relatively rigid lattice work of dispersed particles, and obtaining hollow green microspheres that have substantially uniform distribution of the dispersed particles in the continuous phase of the walls of the microspheres.
Claim 2
Independent Claim
269 words
A method for making hollow green microspheres of 200 to 10,000 micron diameter and of 1 to 1000 microns wall thickness from a stable dispersion of a dispersed particle film forming composition, said composition comprising dispersed particles in a continuous liquid phase, said method comprising feeding said dispersed particle composition and a blowing gas to a coaxial blowing nozzle, said coaxial blowing nozzle having an inner coaxial nozzle for said blowing gas and an outer coaxial nozzle for said dispersed particle composition and a coaxial blowing nozzle orifice, feeding said blowing gas to said inner nozzle, feeding said dispersed particle composition to said outer nozzle to blow and form, in the region of said coaxial blowing nozzle orifice, hollow dispersed particle composition microspheres having stable film walls, removing said hollow microspheres from the region of said coaxial blowing nozzle orifice, surface tension forces acting on said hollow microspheres to cause said hollow microspheres to form a spherical shape, said dispersed particle composition forming the walls of said hollow microspheres and said dispersed particles being uniformly dispersed in said continuous liquid phase, treating said removed hollow microspheres to remove a portion of the continuous liquid phase to bring the dispersed particles into point to point contact and to harden them, said dispersed particles being of sufficient size and in a sufficient amount such that the dispersed particles in the walls of the hollow microspheres link up and form a relatively rigid lattice work of dispersed particles, and obtaining hollow green microspheres that have substantially uniform distribution of the dispersed particles in the continuous phase of the walls of the microspheres.
Claim 3
Dependent Claim
62 words
The method of claim 1 wherein the lower portion of the outer coaxial nozzle is tapered inwardly to form with the outer edge of the inner nozzle a fine gap and the dispersed particle composition is fed under pressure through said gap to form a stable thin film of film forming dispersed particle composition across the orifice of the coaxial blowing nozzle.
Claim 4
Dependent Claim
38 words
The method of claim 1 wherein the hollow green microspheres obtained contain macro particles 1 to 1000 micron in size distributed in the walls of said microspheres and which can be seen through the walls of the microspheres.
Claim 5
Dependent Claim
18 words
The method of claim 1 wherein the dispersed particle composition has a viscosity of 20 to 350 poises.
Claim 6
Dependent Claim
37 words
The method of claim 1 wherein the dispersed particle composition comprises one or more of 0.1 to 10 weight percent binder, 0.5 to 1.5 weight percent film stabilizing agent and 0.05 to 1.5 weight percent dispersing agent.
Claim 7
Independent Claim
269 words
A method for making hollow green microspheres of 500 to 6,000 microns diameter and of 5 to 400 microns wall thickness from a stable dispersion of a dispersed particle film forming composition, said composition comprising dispersed particles in a continuous liquid phase, said method comprising feeding said dispersed particle composition and a blowing gas to a coaxial blowing nozzle, said coaxial blowing nozzle having an inner coaxial nozzle for said blowing gas and an outer coaxial nozzle for said dispersed particle composition and a coaxial blowing nozzle orifice, feeding said blowing gas to said inner nozzle, feeding said dispersed particle composition to said outer nozzle to blow and form, in the region of said coaxial blowing nozzle orifice, hollow dispersed particle composition microspheres having stable film walls, removing said hollow microspheres from the region of said coaxial blowing nozzle orifice, surface tension forces acting on said hollow microspheres to cause said hollow microspheres to form a spherical shape, said dispersed particle composition forming the walls of said hollow microspheres and said dispersed particles being uniformly dispersed in said continuous liquid phase, treating said removed hollow microspheres to remove a portion of the continuous liquid phase to bring the dispersed particles into point to point contact and to harden them, said dispersed particles being of sufficient size and in a sufficient amount such that the dispersed particles in the walls of the hollow microspheres link up and form a relatively rigid lattice work of dispersed particles, and obtaining hollow green microspheres that have substantially uniform distribution of the dispersed particles in the continuous phase of the walls of the microspheres.
Claim 8
Independent Claim
269 words
A method for making hollow green microspheres of 500 to 6,000 microns diameter and of 5 to 400 microns wall thickness from a stable dispersion of a dispersed particle film forming composition, said composition comprising dispersed particles in a continuous liquid phase, said method comprising feeding said dispersed particle composition and a blowing gas to a coaxial blowing nozzle, said coaxial blowing nozzle having an inner coaxial nozzle for said blowing gas and an outer coaxial nozzle for said dispersed particle composition and a coaxial blowing nozzle orifice, feeding said blowing gas to said inner nozzle, feeding said dispersed particle composition to said outer nozzle to blow and form, in the region of said coaxial blowing nozzle orifice, hollow dispersed particle composition microspheres having stable film walls, removing said hollow microspheres from the region of said coaxial blowing nozzle orifice, surface tension forces acting on said hollow microspheres to cause said hollow microspheres to form a spherical shape, said dispersed particle composition forming the walls of said hollow microspheres and said dispersed particles being uniformly dispersed in said continuous liquid phase, treating said removed hollow microspheres to remove a portion of the continuous liquid phase to bring the dispersed particles into point to point contact and to harden them, said dispersed particles being of sufficient size and in a sufficient amount such that the dispersed particles in the walls of the hollow microspheres link up and form a relatively rigid lattice work of dispersed particles, and obtaining hollow green microspheres that have substantially uniform distribution of the dispersed particles in the continuous phase of the walls of the microspheres.
Claim 9
Dependent Claim
50 words
The method of claim 6 wherein substantially uniform size macro particles comprise 2 to 6 volume percent, based on volume of dispersed particles plus macro particles of the dispersed particle composition and which macro particles on formation of the hollow microspheres can be seen through the walls of the microspheres.
Claim 10
Dependent Claim
17 words
The method of claim 6 wherein the dispersed composition has a viscosity of 10 to 200 poises.
Claim 11
Dependent Claim
19 words
The method of claim 6 wherein binder comprises 0.1 to 10 percent by weight of the dispersed particle composition.
Claim 12
Dependent Claim
22 words
The method of claim 6 wherein a film stabilizing agent comprises 0.05 to 1.5 percent by weight of the dispersed particle composition.
Claim 13
Dependent Claim
20 words
The method of claim 6 wherein a dispersing agent comprises 0.05 to 1.5 weight percent of the dispersed particle composition.
Claim 14
Dependent Claim
23 words
The method of claim 1 or 6 for making hollow green microspheres wherein the dispersed particle composition comprises an aqueous continuous liquid phase.
Claim 15
Independent Claim
388 words
A method for making hollow green microspheres of substantially uniform diameter of 500 to 6000 microns and of substantially uniform wall thickness of 5 to 400 microns from a stable dispersion of a dispersed particle film forming composition, said composition comprising uniformly dispersed particles in a continuous liquid phase, said method comprising feeding said dispersed particle composition and a blowing gas to a coaxial blowing nozzle, said coaxial blowing nozzle having an inner coaxial nozzle for said blowing gas and an outer nozzle for said dispersed particle composition and a coaxial blowing nozzle orifice, feeding said blowing gas to said inner nozzle, feeding said dispersed particle composition to said outer nozzle to form and blow, at said coaxial blowing nozzle orifice, hollow dispersed particle microspheres having stable film walls, continuously feeding said dispersed particle composition to said outer coaxial nozzle while said microspheres are being formed, directing an entraining fluid at said coaxial nozzle at an angle relative to a line drawn through the center axis of the coaxial blowing nozzle, said entraining fluid passing over and around said coaxial blowing nozzle to fluid dynamically induce a pulsating or fluctuating pressure field having periodic oscillations at the opposite or lee side of the blowing nozzle in the wake or shadow of said blowing nozzle, said entraining fluid acting on the microspheres to pinch and close-off the microspheres at a point proximate to the coaxial blowing nozzle and said entraining fluid acting to detach the microspheres from the coaxial blowing nozzle and move the microspheres away from the coaxial nozzle, surface tension forces acting on said hollow microspheres to cause said hollow microspheres to form a spherical shape, said dispersed particle composition forming the walls of said hollow microspheres and said dispersed particles being uniformly dispersed in said continuous liquid phase, treating said detached hollow microspheres to remove a portion of the continuous liquid phase to bring the dispersed particles into point to point contact and to harden them, said dispersed particles being of sufficient size and in a sufficient amount such that the dispersed particles in the walls of the hollow microspheres link up and form a relatively rigid lattice work of dispersed particles, and obtaining hollow green microspheres that have substantially uniform distribution of the dispersed particles in the continuous phase of the walls of the microspheres.
Claim 16
Independent Claim
388 words
A method for making hollow green microspheres of substantially uniform diameter of 500 to 6000 microns and of substantially uniform wall thickness of 5 to 400 microns from a stable dispersion of a dispersed particle film forming composition, said composition comprising uniformly dispersed particles in a continuous liquid phase, said method comprising feeding said dispersed particle composition and a blowing gas to a coaxial blowing nozzle, said coaxial blowing nozzle having an inner coaxial nozzle for said blowing gas and an outer nozzle for said dispersed particle composition and a coaxial blowing nozzle orifice, feeding said blowing gas to said inner nozzle, feeding said dispersed particle composition to said outer nozzle to form and blow, at said coaxial blowing nozzle orifice, hollow dispersed particle microspheres having stable film walls, continuously feeding said dispersed particle composition to said outer coaxial nozzle while said microspheres are being formed, directing an entraining fluid at said coaxial nozzle at an angle relative to a line drawn through the center axis of the coaxial blowing nozzle, said entraining fluid passing over and around said coaxial blowing nozzle to fluid dynamically induce a pulsating or fluctuating pressure field having periodic oscillations at the opposite or lee side of the blowing nozzle in the wake or shadow of said blowing nozzle, said entraining fluid acting on the microspheres to pinch and close-off the microspheres at a point proximate to the coaxial blowing nozzle and said entraining fluid acting to detach the microspheres from the coaxial blowing nozzle and move the microspheres away from the coaxial nozzle, surface tension forces acting on said hollow microspheres to cause said hollow microspheres to form a spherical shape, said dispersed particle composition forming the walls of said hollow microspheres and said dispersed particles being uniformly dispersed in said continuous liquid phase, treating said detached hollow microspheres to remove a portion of the continuous liquid phase to bring the dispersed particles into point to point contact and to harden them, said dispersed particles being of sufficient size and in a sufficient amount such that the dispersed particles in the walls of the hollow microspheres link up and form a relatively rigid lattice work of dispersed particles, and obtaining hollow green microspheres that have substantially uniform distribution of the dispersed particles in the continuous phase of the walls of the microspheres.
Claim 17
Dependent Claim
18 words
The method of claim 13 wherein the dispersed particle composition has a viscosity of 20 to 350 poises.
Claim 18
Dependent Claim
18 words
The method of claim 13 wherein the dispsersed particle composition has a viscosity of 10 to 200 poises.
Claim 19
Dependent Claim
64 words
The method of claim 6 or 13 wherein the lower portion of the outer coaxial nozzle is tapered inwardly to form with the outer edge of the inner nozzle a fine gap and the dispersed particle composition is fed under pressure through said gap to form a stable thin film of film forming dispersed particle composition across the orifice of the coaxial blowing nozzle.
Claim 20
Dependent Claim
22 words
The method of claim 6 or 13 wherein the dispersed particles comprise 40 to 60 volume percent of the dispersed particle composition.
Claim 21
Dependent Claim
23 words
The method of claim 6 or 13 wherein the dispersed particles have a particle size in the range of 0.10 to 10 microns.
Claim 22
Dependent Claim
40 words
The method of claim 6 or 13 wherein the hollow green microspheres obtained contain macro particles 5 to 400 microns in size distributed in the walls of said microspheres and which can be seen through the walls of the microspheres.
Claim 23
Dependent Claim
77 words
The method of claim 6 or 13 wherein the dispersed particle composition has a viscosity of 10 to 200 poises, the dispersed particle composition comprises one or more of 0.1 to 10 weight percent binder, 0.05 to 1.5 weight percent film stabilizing agent and 0.05 to 1.5 weight percent dispersing agent, said dispersed particles comprise 40 to 60 volume percent of the dispersed particle composition and said dispersed particles have a particle size 0.10 to 10 microns.
Claim 24
Dependent Claim
23 words
The method of claim 1, 6 or 13 wherein the dispersed particles comprise 30 to 70 volume percent of the dispersed particle composition.
Claim 25
Dependent Claim
21 words
The method of claim 1, 6 or 13 wherein the dispersed particles have a particle size of 0.05 to 20 microns.
Claim 26
Dependent Claim
40 words
The method of claim 1, 6 or 13 wherein said dispersed particle composition comprises one or more of 0.1 to 10 weight percent binder, 0.05 to 1.5 weight percent film stabilizing agent and 0.05 to 1.5 weight percent dispersing agent.
Claim 27
Dependent Claim
15 words
The method of claim 1, 6 or 13 wherein the dispersed particles comprise ceramic particles.
Claim 28
Dependent Claim
15 words
The method of claim 1, 6 or 13 wherein the dispersed particles comprise alumina particles.
Claim 29
Dependent Claim
129 words
Hollow green microspheres of substantially uniform diameter of 500 to 6000 microns and of substantially uniform wall thickness of 5 to 400 microns, the walls of said hollow microspheres comprise a dispersed particle composition comprising dispersed particles in a continuous phase, said dispersed particles being uniformly dispersed in said continuous phase and said dispersed particles being of sufficient size and in a sufficient amount such that the dispersed particles in the walls of the hollow microspheres are in point to point contact and are linked up and form a relatively rigid lattice work of the dispersed particles, said hollow green microspheres are free of latent solid or liquid blowing gas materials and the walls of said hollow microspheres are substantially free of relatively thinned wall portions, holes and bubbles.
Claim 30
Dependent Claim
129 words
Hollow green microspheres of substantially uniform diameter of 500 to 6000 microns and of substantially uniform wall thickness of 5 to 400 microns, the walls of said hollow microspheres comprise a dispersed particle composition comprising dispersed particles in a continuous phase, said dispersed particles being uniformly dispersed in said continuous phase and said dispersed particles being of sufficient size and in a sufficient amount such that the dispersed particles in the walls of the hollow microspheres are in point to point contact and are linked up and form a relatively rigid lattice work of the dispersed particles, said hollow green microspheres are free of latent solid or liquid blowing gas materials and the walls of said hollow microspheres are substantially free of relatively thinned wall portions, holes and bubbles.
Claim 31
Dependent Claim
39 words
The hollow green microspheres of claim 26 wherein macro particles comprise 0.5 to 10% by volume of the dispersed particles plus the macro particles and the macro particles can be seen through the walls of the hollow green microspheres.
Claim 32
Dependent Claim
39 words
The hollow green microspheres of claim 26 wherein the microspheres contain macro particles 5 to 400 microns in size distributed in the walls of said microspheres and the macro particles can be seen through the wall of the microspheres.
Claim 33
Dependent Claim
22 words
The hollow green microspheres of claim 26, wherein the dispersed particles comprise 30 to 70 volume percent of the dispersed particle composition.
Claim 34
Dependent Claim
20 words
The hollow green microspheres of claim 26 wherein the dispersed particles have a particle size of 0.05 to 20 microns.
Claim 35
Dependent Claim
129 words
Hollow green microspheres of substantially uniform diameter of 1200 to 6000 microns and of substantially uniform wall thickness of 10 to 200 microns, the walls of said hollow microspheres comprise a dispersed particle composition comprising dispersed particles in a continuous phase, said dispersed particles being uniformly dispersed in said continuous phase, and said dispersed particles being of sufficient size and in a sufficient amount such that the dispersed particles in the walls of the hollow microspheres are in point to point contact and are linked up and form a relatively rigid lattice work of the dispersed particles, said hollow green microspheres are free of latent solid or liquid blowing gas materials and the walls of said hollow microspheres are substantially free of relatively thinned wall portions, holes and bubbles.
Claim 36
Dependent Claim
129 words
Hollow green microspheres of substantially uniform diameter of 1200 to 6000 microns and of substantially uniform wall thickness of 10 to 200 microns, the walls of said hollow microspheres comprise a dispersed particle composition comprising dispersed particles in a continuous phase, said dispersed particles being uniformly dispersed in said continuous phase, and said dispersed particles being of sufficient size and in a sufficient amount such that the dispersed particles in the walls of the hollow microspheres are in point to point contact and are linked up and form a relatively rigid lattice work of the dispersed particles, said hollow green microspheres are free of latent solid or liquid blowing gas materials and the walls of said hollow microspheres are substantially free of relatively thinned wall portions, holes and bubbles.
Claim 37
Dependent Claim
37 words
The hollow green microspheres of claim 31 wherein the microspheres contain macro particles 10 to 2000 microns in size distributed in the walls of said microspheres and which can be seen through the walls of said microspheres.
Claim 38
Dependent Claim
24 words
The hollow green microspheres of claim 26 or 31 wherein the walls of said hollow microspheres comprise dispersed particles, a binder and continuous phase.
Claim 39
Dependent Claim
41 words
The hollow green microspheres of claim 26 or 31 wherein macro particles comprise 2 to 6% by volume of the dispersed particles plus the macro particles and the macro particles can be seen through the walls of the hollow green microspheres.
Claim 40
Dependent Claim
16 words
The hollow green microspheres of claim 26 or 31 wherein the dispersed particles comprise ceramic particles.
Claim 41
Dependent Claim
15 words
The hollow green microspheres of claim 26 or 31 wherein the dispersed particles comprise alumina.
Claim 42
Dependent Claim
24 words
The hollow green microspheres of claim 26 or 31 wherein the dispersed particles comprise 40 to 60 volume percent of the dispersed particle composition.
Claim 43
Dependent Claim
22 words
The hollow green microspheres of claim 26 or 31 wherein the dispersed particles have a particle size of 0.10 to 10 microns.
References Cited (Backward Citations)
US3177161A
Cited
US3528809A
Cited
US3674461A
Cited
US3264073A
Cited
US3423489A
Cited
US3792136A
Cited
US3954678A
Cited
US4001480A
Cited
US4111713A
Cited
US4059423A
Cited
US4349456A
Cited
US4230463A
Cited
US4214020A
Cited
US4329157A
Cited
US4268278A
Cited
US4222977A
Cited
US4344787A
Cited
US4279632A
Cited
US4303431A
Cited
US4303603A
Cited
US4303732A
Cited
US4303736A
Cited
US4415512A
Cited
US4257798A
Cited
US4348458A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1991-10-11 | 1992-04-11 | 1992-10-11 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1995-10-11 | 1996-04-11 | 1996-10-11 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1999-10-11 | 2000-04-11 | 2000-10-11 | $7700.00 | Window Closed / Lapsed |