US3644263A
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US
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High polymer latices and methods and means for producing same
Assignee: BURKE OLIVER W JUN
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Filing: 1968-12-18
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Granted: 1972-02-22
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Expires: 1988-12-18
Abstract
Abstract The preparation of aqueous latices from solvent dispersions of elastomers and other high-polymer compositions has presented problems including excessive viscosity during processing and foaming and coagulation, which have produced losses and increased costs. Herein combinations of steps are disclosed which reduce or eliminate various of these problems, especially coagulum; enable the preparation of latices of high-solids content; enable preparation of high-solids content latices of grafted or fillerextended or filler-reinforced elastomers; enable preparation of high-solids latices of low molecular weight polymer which are then modified to materially increase the molecular weight of the polymer; and enable the preparation of improved stable latices both dilute and of high-solids content, which are useful for example for adhesive and film-forming purposes. The process in common with that of related copending applications is characterized, inter alia, by the establishment of a flow of steam as a continuous phase into which an emulsion of a cement of the polymer is dispersed as an aerosol of latex droplets in a solvent-vapor continuum, followed by coalescence of the latex droplets and separation of the resulting coalesced liquid phase from the resulting solvent-vapor phase. In one embodiment of the present method an unstable emulsion is prepared employing only a limited quantity of emulsifier, so that the homogenizing thereof produces an emulsion the dispersed phase of which is only temporarily of precursor latex particle size. This unstable emulsion is converted to a stable latex by provisions for dispersing the same as the aerosol before coalescence of over 5 percent of the dispersed polymer phase of the emulsion into droplets of greater than precursor latex particle size, (or for stabilizing the same by the addition of a secondary emulsifier to the same before such condition is reached without further reducing the size of the cement droplets of the dispersed phase) so that the latex in the aerosol and separated therefrom is kept free of coagulum during the coalescing of the latex droplets and the separation and further treatment, e.g., stripping and concentrating, with or without correlated further additions or emulsifier to stabilize the latex for storage or use. The separation of the gaseous and liquid latex phases is preferably effected with the aid of partially concentrated liquid latex; and in certain embodiments herein disclosed a mixture of such partially concentrated latex commingled with water vapor generated therefrom is added to and commingled with the aerosol before or after at least a part of the aerosol has been coalesced, and the combined liquid phases and combined gas phases of the resulting mixture are thereafter separated. Also in certain embodiments of the invention a liquid flow of secondary emulsifier may be added to the uncoalesced or partially coalesced aerosol, or to the mixture thereof with the partially concentrated latex, prior to the separation of the gaseous and liquid phases thereof.
Inventors
- 👤 Oliver W Burke Jr
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 22:44
CPC Classifications
C; C08; C08J; C08J3/00; C08J3/02; C08J3/03; C08J3/07; B; B01; B01D; B01D19/00; B01D19/0068
Claims Analysis
Total Claims: 33
Claim 1
Independent Claim
28 words
A method as claimed in claim 1, in which, following step (f) the latex is concentrated to a solids content, dry basis, of over 50 percent, by weight.
Claim 2
Independent Claim
406 words
A method for preparing a latex the dispersed phase of which is a composition of an organic solvent soluble or dispersible polymer, the latex particles of which are of such size that the latex when at a concentration of 50 percent solids, dry basis by weight, has a viscosity no greater than 5,000 cps., the latex containing and being stabilized by an amount of emulsifier material in the range of 4 to 12 parts per 100 parts of the dispersed phase, by weight; said polymer being selected from the class consisting of natural rubber and polymerized ethylenically unsaturated monomer material containing from two to 20 carbon atoms; and said emulsifier material being selected from the class consisting of the anionic, cationic and nonionic emulsifiers which contain from eight to 22 carbon atoms, when nonpolymeric, and the polymeric emulsifiers; which method comprises: a. providing a moving flow of gas comprising steam as an initial continuous phase, b. providing a cement of the polymer composition in essentially water-immiscible volatile organic solvent which itself or as an azeotrope with water has a boiling point lower than that of water at atmospheric pressure, c. emulsifying together said cement and water in the proportions of 0.5 to 2.5 volumes of water per volume of cement with not less than one-fourth and not more than three-fourths of the said amount of emulsifier material based on the dry solids content of said cement, by weight, to form an unstable emulsion of temporarily precursor latex particle size, d. then, before coalescence of more than 5 percent of the dispersed phase Of said emulsion into greater than precursor latex particle size, dispersing the unstable emulsion of temporarily precursor latex particle size into the flow of steam as the initial continuous phase and subjecting the phases to a decrease of pressure while maintaining the temperature thereof below the limiting temperature for maintaining the temporary stability of the emulsion, thereby vaporizing solvent from the dispersed droplets and forming an aerosol of latex in vapor, e. separating the latex droplets from the vapor phase of the aerosol, f. concentrating the latex to a solids content, dry basis, of over 50 percent by weight, and g. dispersing further emulsifier into said latex, to the extent of at least one-fourth of said amount of emulsifier, after the dispersion of the emulsion in step (d) and before the concentration of the latex beyond 45 percent solids, dry basis, in step (f).
Claim 3
Dependent Claim
29 words
A method as claimed in claim 3, in which the emulsifier material comprises at least two emulsifiers, one having an aromatic nucleus and the other having an aliphatic nucleus.
Claim 4
Dependent Claim
51 words
A method as claimed in claim 1, in which the solvent is an aromatic solvent, the polymer is an aliphatic polymer, the emulsifier material employed in step (b) consists essentially of emulsifier having an aromatic nucleus, and the emulsifier employed in step (e) consists essentially of emulsifier having an aliphatic nucleus.
Claim 5
Dependent Claim
17 words
A method as claimed in claim 3, in which step (g) is practiced prior to step (e).
Claim 6
Dependent Claim
16 words
A method as claimed in claim 3, in which step (g) is practiced after step (e).
Claim 7
Independent Claim
371 words
A method for preparing a latex the dispersed phase of which is a composition of an organic solvent soluble or dispersible polymer, the latex particles of which are of such size that the latex when at a concentration of 50 percent solids, dry basis by weight, has a viscosity no greater than 5,000 cps., the latex containing and being stabilized by an amount of emulsifier material in the range of 4 to 12 parts per 100 parts of the dispersed phase, by weight; said polymer being selected from the class consisting of natural rubber and polymerized ethylenically unsaturated monomer material containing from two to 20 carbon atoms; and said emulsifier material being selected from the class consisting of the anionic, cationic and nonionic emulsifiers which contain from eight to 22 carbon atoms, when nonpolymeric, and the polymeric emulsifiers, which method comprises: a. providing a moving flow of gas comprising steam as an initial continuous phase, b. providing a cement of the polymer composition in essentially water-immiscible volatile organic solvent which itself or as an azeotrope with water has a boiling point lower than that of water at atmospheric pressure, c. emulsifying together said cement and water in the proportions of 0.5 to 2.5 volumes of water per volume of cement with not less than one-fourth and not more than three-fourths of the said amount of emulsifier material based on the dry solids content of said cement, by weight, to form an unstable emulsion of temporarily precursor latex particle size, d. mixing into said unstable emulsion, before coalescence of more than 5 percent of the dispersed phase of said emulsion into greater than precursor latex particle size, further emulsifier material to the extent of at least one-fourth of said amount of emulsifier material while maintaining essentially unchanged the particle size of the dispersed phase, e. dispersing the mixture formed in step (d) into the flow of steam as the initial continuous phase and subjecting the phases to a decrease of pressure while maintaining the temperature thereof below the limiting temperature for stability of the emulsion, thereby vaporizing solvent from the dispersed droplets and forming an aerosol of latex in vapor, and f. separating the latex from the vapor phase of the aerosol.
Claim 8
Independent Claim
368 words
A method for preparing a latex the Dispersed phase of which is a composition of an organic solvent soluble or dispersible polymer, the latex particles of which are of such size that the latex, when at a concentration of 50 percent solids, dry basis by weight, has a viscosity no greater than 5,000 cps., the latex containing sufficient emulsifier material to stabilize the same; said polymer being selected from the class consisting of natural rubber and polymerized ethylenically unsaturated monomer material containing from two to 20 carbon atoms; and said emulsifier material being selected from the class consisting of the anionic, cationic and nonionic emulsifiers which contain from eight to 22 carbon atoms, when nonpolymeric, and the polymeric emulsifiers, which method comprises: a. providing a moving flow of gas comprising steam as an initial continuous phase, b. providing a cement of the polymer composition in essentially water-immiscible volatile organic solvent which itself or as an azeotrope with water has a boiling point lower than that of water at atmospheric pressure, c. forming an unstable emulsion of temporarily precursor latex particle size in two emulsifying steps, in the first of which said cement and water are emulsified with sufficient emulsifier to form an unstable crude emulsion, in which more than 5 percent of the dispersed phase droplets are of greater than precursor latex particle size, and in the second of which said unstable crude emulsion is reduced to an unstable fine emulsion essentially of temporarily precursor latex particle size having no more than 5 percent of its dispersed phase of greater than precursor latex particle size, d. delivering said unstable fine emulsion, as soon as it is formed in said second emulsifying step, directly into said flow of steam as the initial continuous phase and dispersing the same therein and subjecting the phases to a decrease of pressure while maintaining the temperature thereof below the limiting temperature for maintaining the temporary stability of the emulsion, thereby vaporizing solvent from the dispersed droplets and forming an aerosol of latex in vapor, e. separating the latex droplets from the vapor phase of the aerosol, and f. concentrating the latex to a solids content dry basis, of over 50 percent by weight.
Claim 9
Dependent Claim
49 words
A method as defined in claim 9, in which the proportion of emulsifier employed in step (c) while only sufficient to yield a temporarily stable emulsion of the cement, is sufficient to produce a stable latex of the polymer after removal of the solvent from the dispersed cement phase.
Claim 10
Dependent Claim
80 words
A method as claimed in claim 9, in which the proportion of emulsifier employed in step (c) is sufficient to produce only a temporarily stable latex of the polymer after removal of solvent from the dispersed cement phase, and in which the method further comprises: g. before coalescence of more than 5 percent of the dispersed phase of the latex into particles of greater than latex particle size, dispersing sufficient additional emulsifier material into the latex to stabilize the latex.
Claim 11
Dependent Claim
38 words
A method as claimed in claim 11, in which step (g) is practiced after the dispersion of the emulsion in step (d) and before the concentration of the latex beyond 45 percent solids, dry basis, in step (f).
Claim 12
Dependent Claim
42 words
A method as claimed in claim 12, in which step (g) is practiced by dispersing the additional emulsifier material into the aerosol prepared by step (d) and separating the same from the vapor phase thereof with the latex droplets in step (e).
Claim 13
Dependent Claim
390 words
A process for preparing a latex by forming and removing solvent from an aqueous emulsion of a cement which is essentially an organic solvent dispersion of high polymer composition; the latex containing and being stabilized by emulsifier material; said polymer being selected from the class consisting of natural rubber and polymerized ethylenically unsaturated monomer material containing from two to 20 caRbon atoms; and said emulsifier material being selected from the class consisting of the anionic, cationic and nonionic emulsifiers which contains from eight to 22 carbon atoms, when nonpolymeric, and the polymeric emulsifiers, which process comprises, in combination, the steps of: a. providing a moving flow of gas comprising steam as an initial continuous phase, b. providing a cement of not more than 40 weight parts of the polymer composition in essentially not less than 60 weight parts of water immiscible volatile organic solvent which itself, or as an azeotrope with water, has a boiling point lower than water, at atmospheric pressure, c. forming from said cement and water and emulsifier material an emulsion of at least temporarily precursor latex particle size, d. dispersing a flow of said emulsion as a discontinuous phase into said flow of steam as an initial continuous phase, in such proportion that sufficient heat is provided by condensation of steam in said flow to vaporize substantially all the solvent from the liquid phase into the gaseous phase of said flow to form an aerosol while adding the condensate formed to the discontinuous phase of said aerosol, e. withdrawing a flow of said aerosol, f. subjecting the withdrawn flow of said aerosol to a separation of its discontinuous liquid phase from its continuous gaseous phase to form a latex, g. withdrawing a flow of said latex and subjecting said withdrawn flow of latex to vaporization of a part of its water content to convert said flow into a flow of water vapor mixed with bodies of more concentrated latex, h. commingling the flow produced by step (g) with the flow withdrawn by step (e) and i. subjecting the commingled flow produced by step (h) to step (f) for effecting separation of the liquid phase of said water vapor and latex flow from the vapor phase thereof simultaneously with the practice of step (f), and j. withdrawing a part of the latex formed by said step (f).
Claim 14
Dependent Claim
51 words
A process as claimed in claim 14 in which the combination of steps further comprises: k. subjecting the flow of aerosol withdrawn in step (e) to coalescing stresses to coalesce fine liquid droplets carried by the gaseous phase of the aerosol before subjecting said flow to the commingling of step (h).
Claim 15
Dependent Claim
48 words
A process as claimed in claim 14, in which the combination of steps further comprises: k. subjecting the commingled flows produced by step (h) to coalescing stresses to coalesce liquid bodies carried thereby into larger bodies before subjecting the same to step (f) in accordance with step (i).
Claim 16
Dependent Claim
51 words
A process as claimed in claim 16, in which the combination of steps further comprises: l. subjecting the flow of aerosol withdrawn in step (e) to coalescing stresses to coalesce fine liquid droplets carried by the gaseous phase of the aerosol before subjecting said flow to the commingling of step (h).
Claim 17
Dependent Claim
350 words
A process for forming a latex by forming and removing solvent from an aqueous emulsion of a cement which is essentially an organic solvent dispersion of high polymer composition; the latex containing and being stabilized by emulsifier material; said polymer being selected from the class consisting of natural rubber and polymerized ethylenically unsaturated monomer material containing from two to 20 carbon atoms; and said emulsifier material being selected from the class consisting of the anionic, cationic and nonionic emulsifiers which contains from eight to 22 carbon atoms, when nonpolymeric, and the polymeric emulsifiers, which process comprises, in combination, the steps of: a. providing a moving flow of gas comprising steam as an initial continuous phase, b. providing a cement of not more than 40 weight parts of the polymer composition in essentially not less than 60 weight parts of water immiscible volatile organic solvent which itself, or as an azeotrope with water, has a boiling point lower than water, at atmospheriC pressure, c. forming from said cement and water and emulsifier material an emulsion of at least temporarily precursor latex particle size, d. dispersing a flow of said emulsion as a discontinuous phase into said flow of steam as an initial continuous phase, in such proportion that sufficient heat is provided by condensation of steam in said flow to vaporize substantially all the solvent from the liquid phase into the gaseous phase of said flow to form an aerosol while adding the condensate formed to the discontinuous phase of said aerosol, e. withdrawing a flow of said aerosol, f. subjecting the withdrawn flow of said aerosol to a separation of its discontinuous liquid phase, from its continuous gaseous phase, to form a latex, g. withdrawing a flow of said latex, h. mixing the flows withdrawn in steps (e) and (g), i. subjecting the mixed flow produced by step (h) to step (f) so that the admixture of the flow withdrawn in step (g) with the flow withdrawn in step (e) may assist the separation in step (f), and j. withdrawing a part of the latex formed by said step (f).
Claim 18
Independent Claim
343 words
A method for preparing a latex the dispersed phase of which is a composition of an organic solvent soluble or dispersible polymer, the latex particles of which are of such size that the latex when at a concentration of 50 percent solids, dry basis by weight, has a viscosity no greater than 5,000 cps., the latex containing and being stabilized by an amount of emulsifier material in the range of 4 to 12 parts per 100 parts of the dispersed phase, by weight; said polymer being selected from the class consisting of natural rubber and polymerized ethylenically unsaturated monomer material containing from two to 20 carbon atoms; and said emulsifier material being selected from the class consisting of the anionic, cationic and nonionic emulsifiers which contain from eight to 22 carbon atoms, when nonpolymeric, and the polymeric emulsifiers; which method comprises: a. providing a moving flow of gas comprising steam as an initial continuous phase, b. providing a cement of the polymer composition in essentially water-immiscible volatile organic solvent which itself or as an azeotrope with water has a boiling point lower than that of water at atmospheric pressure, c. emulsifying together said cement and water in proportions of 0.5 to 2.5 volumes of water per volume of cement with not less than one-fourth and not more than three-fourths of the said amount of emulsifier material based on the dry solids content of said cement, by weight, to form an emulsion the polymer-solvent phase of which is of a size which, on removal of its solvent, will produce latex particles in the range of 2,000 to 10,000 A. average diameter, d. dispersing the emulsion formed by step (c) into the flow of steam to form an aerosol of dilute latex in vapor therein, e. separating the latex from the vapor phase of the aerosol, f. concentrating the same to at least 50 percent solids, dry basis by weight, g. recovering the concentrated latex product, and h. adding the remainder of said amount of emulsifier subsequent to step (c) and prior to step (g).
Claim 19
Dependent Claim
49 words
A method as claimed in claim 19, wherein in step (h) at least a part of said remainder of emulsifier is added to the emulsion produced by step (c), but without treatment that would further reduce the precursor latex particle size thereof, prior to the performance of step (d).
Claim 20
Dependent Claim
35 words
A method as claimed in claim 19, wherein in step (h) at least a part of said remainder of emulsifier is added to the aerosol formed in step (d) before subjecting it to step (e).
Claim 21
Dependent Claim
46 words
A method as claimed in claim 19, wherein in step (h) at least a part of said remainder of emulsifier is added to the latex separated in step (e) before concentration thereof beyond the solids content of 45 percent, dry basis by weight, in step (f).
Claim 22
Dependent Claim
157 words
A sYnthetic aqueous latex prepared from emulsifier and an organic solvent-cement of synthetic hydrocarbon polymer material having a molecular weight of at least 2,000, said latex characterized in that a. it contains at least 60 percent solids, by weight, b. it has an average particle diameter in the range of 2,000 to 10,000 angstroms, c. it is corrosion inhibiting to ferrous metals, d. it contains from 4 to 12 percent emulsifier based on its polymer content, e. its corrosion inhibiting characteristic is imparted by its inclusion of emulsifier selected from the class consisting essentially of the amine salts which are the reaction products of amines containing not more than 20 carbon atoms and not more than five amine groups and selected from the primary, secondary and tertiary amines, with water-soluble acids selected from the group consisting of phosphoric acid, alkali metal mono-phosphate, alkali metal diphosphate, mono- and di-esters of phosphoric acid, and the water-soluble alpha-hydroxy carboxylic acids.
Claim 23
Dependent Claim
21 words
A synthetic aqueous latex as claimed in claim 23 in which the emulsifier includes a glycolic acid salt of a diamine.
Claim 24
Dependent Claim
23 words
A synthetic aqueous latex as claimed in claim 23 in which the latex further includes emulsifying material selected from the quaternary ammonium compounds.
Claim 25
Dependent Claim
40 words
A synthetic aqueous latex as claimed in claim 23 in which the hydrocarbon polymer material consists essentially of ethylene-propylene polymer selected from the ethylene-propylene copolymers and the ethylene-propylene-diene terpolymers wherein the diene component contains not more than 12 carbon atoms.
Claim 26
Dependent Claim
281 words
A process for producing a polar interpolymer latex from polar monomer and hydrocarbon polymer, which process comprises: a. providing a moving flow of gas comprising steam as an initial continuum, b. forming a cement of not more than 40 weight parts of the hydrocarbon polymer in essentially not less than 60 weight parts of water immiscible volatile organic solvent which itself, or as an azeotrope with water, has a boiling point lower than that of water, c. mixing with the polymer cement (1) 0.2 to 40 percent by weight based on the polymer, of monomer material which contains and is polymerizable through at least one ethylenically unsaturated group and which contains at least one polar group and (2) sufficient free radical generating polymerization catalyst to cause polymerization of said monomer material, d. subjecting the mixture produced by step (c) to polymerization of said monomer material to form a polar interpolymer cement, e. forming from said polar interpolymer cement, water, and emulsifier material an emulsion of at least temporarily precursor latex particle size, f. dispersing a flow of said emulsion as a discontinuous phase into said flow of steam as an initial continuous phase, in such proportion that sufficient heat is provided by condensation of steam in said flow to vaporize substantially all the solvent from the liquid phase into the gaseous phase of said flow to form an aerosol while adding the condensate formed to the discontinuous phase of said aerosol, g. separating the interpolymer latex droplets from the vapor phase of the aerosol, h. concentrating said interpolymer latex to a solids content of at least 50 percent, dry basis by weight, and i. recovering the concentrated polar interpolymer latex product.
Claim 27
Dependent Claim
26 words
A process as claimed in claim 27, which further comprises j. adding a further quantity of emulsifier subsequent to step (e) and prior to step (i).
Claim 28
Dependent Claim
50 words
A process as claimed in claim 28, wherein in step (j) at least a part of said further quantity of emulsifier is added to the emulsion produced by step (e) but without treatment that would further reduce the precursor latex particle size thereof, prior to the performance of step (f).
Claim 29
Dependent Claim
36 words
A process as claimed in claim 28, wherein in step (J) at least a part of said further quantity of emulsifier is added to the aerosol formed in step (f) before subjecting it to step (g).
Claim 30
Dependent Claim
47 words
A process as claimed in claim 28, wherein in step (j) at least a part of said further quantity of emulsifier is added to the latex separated in step (g) before concentration thereof beyond a solids content of 45 percent, dry basis by weight, in step (h).
Claim 31
Dependent Claim
307 words
A process for producing a polar interpolymer latex from polar monomer and hydrocarbon polymer composition which comprises: a. providing a moving flow of gas comprising steam as an initial continuous phase, b. providing a cement consisting essentially of a dispersion of not more than 40 weight parts of the polymer composition in essentially not less than 60 weight parts of water-immiscible volatile organic solvent which itself, or as an azeotrope with water, has a boiling point lower than that of water, c. forming from said cement and water and emulsifier material an emulsion of at least temporarily precursor latex particle size, d. dispersing a flow of said emulsion as a discontinuous phase into said flow of steam as an initial continuous phase, in such proportion that sufficient heat is provided by condensation of steam in said flow to vaporize substantially all the solvent from the liquid phase into the gaseous phase of said flow to form an aerosol while adding the condensate formed to the discontinuous phase of said aerosol, e. separating the latex from the vapor phase of the aerosol, f. concentrating the latex to a solids content of at least 50 percent, dry solids by weight, g. recovering the concentrated latex product, and h. mixing with the latex separated in step (e), prior to concentration thereof beyond 45 percent, dry solids, by weight in step (f), (1) 0.2 to 40 percent by weight, based on the polymer of the latex, of monomer material which contains and is polymerizable through at least one ethylenically unsaturated group and which contains at least one polar group, and (2) enough free radical generating polymerization catalyst to cause polymerization of said monomer material, and subjecting the so formed mixture to polymerization of said monomer material to form an interpolymer latex which is subjected to the subsequent portions of the process.
Claim 32
Dependent Claim
26 words
A process as claimed in claim 32, which process comprises: i. adding a further quantity of emulsifier subsequent to step (c) and prior to step (g).
Claim 33
Dependent Claim
34 words
A process as claimed in claim 33, wherein in step (i) at least a part of said further quantity of emulsifier is added to the latex after step (h) and prior to step (g).
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) | 1975-02-21 | 1975-08-23 | 1976-02-22 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1979-02-21 | 1979-08-23 | 1980-02-22 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1983-02-21 | 1983-08-23 | 1984-02-22 | $7700.00 | Window Closed / Lapsed |