US3674736A
Expired / Lapsed
US
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Process for the preparation of pigmented polymer powders of controlled particle shape and size and size distribution and product
Assignee: Millennium Petrochemicals Inc
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Filing: 1969-04-15
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Granted: 1972-07-04
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Expires: 1989-04-15
Abstract
Abstract Pigmented polymer powders of average particle size less than 30 microns, which can be of uniform shape and in a narrow size distribution, are prepared by controlled heating, melting and agitation of a liquid dispersion of pigmented polymer in bulk or particle form in the presence of a surfactant or by controlled heating and agitating a liquid containing surfactant to which molten polymer is added. Pigmented powders can thus be obtained having spherical particles of very narrow size distribution approaching uniformity.
Inventors
- 👤 Frank Lerman
- 👤 Raymond C Bartsch
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 08:20
CPC Classifications
C; C08; C08J; C08J3/00; C08J3/12; C08J2323/00; C08J2323/02; C08J2323/04; C08J2323/06; Y; Y10; Y10S; Y10S521/00; Y10S521/921; Y10S524/00; Y10S524/904
Claims Analysis
Total Claims: 22
Claim 1
Independent Claim
51 words
A process according to claim 1 in which the pigmented polymer is added as a molten mass to a hot inert dispersing liquid containing the surfactant and is sub-divided into particle form by heating and agitation as a first stage, and modifying and re-sizing the particles in subsequent stage or stages.
Claim 2
Dependent Claim
53 words
A process according to claim 1 in which the pigmented polymer is in solid bulk or particle form in the dispersing liquid and is heated above its melting point to form a mass that is sub-divided by agitation into particle form, and modifying and controlling the size of the particles in subsequent stages.
Claim 3
Dependent Claim
57 words
A process according to claim 1 in which the pigmented polymer is in solid particle form in the dispersing liquid and is heated with agitation to above its melting point without losing its particulate form and is further heated and agitated with or without sub-dividing to modify and control the size of the particles in subsequent stages.
Claim 4
Dependent Claim
30 words
A process according to claim 1 in which the average size is controlled within the range from about 1 to about 10 microns, and the GSD at less than 1.4.
Claim 5
Dependent Claim
30 words
A process according to claim 1 in which the average size is controlled within the range of about 10 to about 20 microns and the GSD is less than 1.35.
Claim 6
Dependent Claim
156 words
A process according to claim 1 in which particle size is controlled by heating the pigmented polymer in the inert liquid in at least one stage at a temperature within the range from about 100* to about 500*F. 8 A process according to claim 1 in which particle size is controlled by control of the degree of agitation in at least one stage within the range of from about 100 to about 5,000 linear feet per minute. 9 A process according to claim 1 in which particle size is controlled by control of the concentration of polymer in the dispersion within the range of from about 2.5 to 10 parts of dispersing liquid to one part of polymer. 10 A process according to claim 1 in which particle size is controlled by control of the amount of surfactant in the dispersion within the range of from about 0.1 to about 1 parts per part of polymer.
Claim 7
Dependent Claim
39 words
A process according to claim 1 in which particle size and size distribution are controlled by separation of the process into at least two stages at different dispersion temperatures, each at or above the melting temperature of the polymer.
Claim 8
Dependent Claim
116 words
A process according to claim 1 in which particle size is controlled in an initial heating stage so as to sub-divide the pigmented polymer to a small particle size by maintaining the dispersion temperature at at least from about 50*F. to about 250*F. above the melting temperature of the polymer, and then, in a subsequent heating stage, paRticle size is controlled so as to agglomerate and coalesce the particles, and increase their size and narrow their size distribution, while at the same time forming them into a regular shape and surface configuration, by maintaining the dispersion at a higher temperature of at least from about 75*F. to about 500*F. above the melting temperature of the polymer.
Claim 9
Dependent Claim
15 words
A process according to claim 1 in which the polymer is a thermoplastic synthetic resin.
Claim 10
Dependent Claim
12 words
A process according to claim 13 in which the polymer is polyethylene.
Claim 11
Dependent Claim
14 words
A process according to claim 13 in which the polymer is a methacrylate-styrene copolymer.
Claim 12
Dependent Claim
14 words
A process according to claim 1 in which the polymer is an ethylene copolymer.
Claim 13
Dependent Claim
15 words
A process according to claim 1 in which the polymer is an ethylene-vinyl acetate copolymer.
Claim 14
Dependent Claim
16 words
A process according to claim 1 in which the surfactant is a nonionic polyoxyalkylene glycol surfactant.
Claim 15
Dependent Claim
18 words
A process according to claim 1 in which the surfactant is a polyoxyethylene oxypropylene glycol block copolymer surfactant.
Claim 16
Dependent Claim
15 words
A process according to claim 1 in which the pigment is a white metal oxide.
Claim 17
Dependent Claim
255 words
A process according to claim 1 in which the pigment is carbon black. 22 A process for preparing finely divided pigmented polymer powders, containing from about 0.001 to 1 part by weight of pigment, having controlled particle size and/or shape and/or size distribution, comprising agitating a molten pigmented polymer in from about 1 to about 40 parts per part of polymer of an inert dispersing liquid which is a nonsolvent for said polymer in the presence of from about 0.05 to 2 parts by weight per part of polymer of a nonionic surfactant at a first temperature from at least about 50*F. to about 250*F. above the melting temperature of the polymer for a time sufficient to form finely divided pigmented polymer particles dispersed in the liquid, and then in a second stage heating the dispersion with agitation at a second temperature above the melting temperature of the polymer but below the decomposition temperature of any component and different from the first temperature for a time sufficient to shape the particles, and control their average size to within the range of from about 1 to about 30 microns, and narrow their size distribution to less than 1.5 GSD, whereby about 68.3 percent of said particles are within a size range determined by the particle diameters of the mean size divided by the GSD value and the mean size multiplied by the GSD value, and then cooling the pigmented particles so as to solidify them and stabilize them in that shape, average size and size distribution.
Claim 18
Dependent Claim
30 words
A process according to claim 22 in which the size distribution is controlled within the average size range from about 1 to about 10 microns, at less than 1.4 GSD.
Claim 19
Dependent Claim
30 words
A process according to claim 22 in which the size distribution is controlled within the average size range of from about 10 to 20 microns at less than 1.35 GSD.
Claim 20
Dependent Claim
19 words
A process according to claim 22 in which the particles are brought to a spherical shape and surface configuration.
Claim 21
Dependent Claim
163 words
A process according to claim 22 in which particle size is controlled by heating the dispersion in a first stage at a temperature within the range from about 100* to about 175*F., and in a second stage at a temperature within the range from about 150* to about 250*F. 27 A process according to claim 22 in which particle size is controlled by control of the degree of agitation within the range of from about 100 to about 5000 linear feet per minute. 28 A process according to claim 22 in which particle size is controlled by control of the concentration of polymer in the dispersion within the range of from about 2.5 to 10 parts of dispersing liquid to 1 part of polymer. 29 A process according to claIm 22 in which particle size is controlled by control of the amount of surfactant in the dispersion within the range of from about 0.1 to about 1 parts per part of pigmented polymer.
Claim 22
Dependent Claim
37 words
A process according to claim 22 in which particle size is controlled in the second stage by maintaining the dispersion temperature at at least about 75*F. up to about 500*F. above the melting temperature of the polymer.
References Cited (Backward Citations)
No citation records indexed.
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1975-07-04 | 1976-01-03 | 1976-07-04 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1979-07-04 | 1980-01-03 | 1980-07-04 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1983-07-04 | 1984-01-03 | 1984-07-04 | $7700.00 | Window Closed / Lapsed |