Patent US3899438A successfully refreshed from Google Patents.
US3899438A
Expired / Lapsed
US
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Simultaneous reaction and dispersion of 4,4-methylene dianiline-salt mixtures to form complexes thereof
Assignee: Uniroyal Chemical Co Inc
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Filing: 1973-10-17
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Granted: 1975-08-12
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Expires: 1993-10-17
Abstract
Abstract A method for preparing small particles of a complex of 4,4''methylene dianiline and selected alkali metal salts including sodium chloride in an inert liquid which comprises agitating a mixture of tris-(4,4''-methylene dianiline), alkali metal salt, an inert liquid vehicle and water; the amount of water being at least 0.5 part per 100 parts of salt and not more than that quantity which would provide a saturated solution throughout at least 50% of the complex-forming reaction.
Inventors
- 👤 James Kalil
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-08 03:29
CPC Classifications
C; C08; C08K; C08K5/00; C08K5/16; C08K5/17; C08K5/18; C08G; C08G18/00; C08G18/06; C08G18/08; C08G18/10
Claims Analysis
Total Claims: 14
Claim 1
Independent Claim
137 words
IN A PROCESS FOR FORMING A COMPLEX OF 4,4'' -METHYLENE DIANILINE (MDA) AND AN ALKALI METAL SALT SELECTED FROM THE GROUP CONSISTING OF SODIUM CHLORIDE, SODIUM BROMIDE, SODIUM IODIDE, LITHIUM CHLORIDE, LITHIUM BROMIDE, LITIUM IODIDE, AND SODIUM CYANIDE, THE MOLE RATIO OF MDA/SALT IN SAID COMPLEX BEING 3:1, THE IMPROVEMENT COMPRISING ADDING TO THE MDA/ SALT MIXTURE 1) AT LEAST ABOUT 0.5 PARTS OF WATER PER 100 PARTS OF SALT BUT NOT ENOUGH TO DISSOLVE ALL THE SALT UNTIL THE COMPLEXFORMING REACTIONS IS AT LEAST 50% COMPLETE, AND 2) 2-35 PARTS OF AN INERT LIQUID CARRIER PER PART OF SALT, CONDUCTING THE REACTION BETWEN THE MDA AND SALT WITH AGITATION, AND RECOVERING DIRECTLY FROM SAID REACTION A DISPERSION OF MDA/SALT COMPLEX PARTICLES OF SUCH FINENESS THAT AT LEAST 95% HAVE A MAXIMUM DIAMETER OF ABOUT 10 MICRONS.
Claim 2
Dependent Claim
137 words
IN A PROCESS FOR FORMING A COMPLEX OF 4,4'' -METHYLENE DIANILINE (MDA) AND AN ALKALI METAL SALT SELECTED FROM THE GROUP CONSISTING OF SODIUM CHLORIDE, SODIUM BROMIDE, SODIUM IODIDE, LITHIUM CHLORIDE, LITHIUM BROMIDE, LITIUM IODIDE, AND SODIUM CYANIDE, THE MOLE RATIO OF MDA/SALT IN SAID COMPLEX BEING 3:1, THE IMPROVEMENT COMPRISING ADDING TO THE MDA/ SALT MIXTURE 1) AT LEAST ABOUT 0.5 PARTS OF WATER PER 100 PARTS OF SALT BUT NOT ENOUGH TO DISSOLVE ALL THE SALT UNTIL THE COMPLEXFORMING REACTIONS IS AT LEAST 50% COMPLETE, AND 2) 2-35 PARTS OF AN INERT LIQUID CARRIER PER PART OF SALT, CONDUCTING THE REACTION BETWEN THE MDA AND SALT WITH AGITATION, AND RECOVERING DIRECTLY FROM SAID REACTION A DISPERSION OF MDA/SALT COMPLEX PARTICLES OF SUCH FINENESS THAT AT LEAST 95% HAVE A MAXIMUM DIAMETER OF ABOUT 10 MICRONS.
Claim 3
Dependent Claim
130 words
In a process for forming a complex of 4,4''-methylene dianiline (MDA) and sodium chloride in a mole ratio of 3:1, the improvement comprising adding to a mixture of the MDA and sodium chloride 1) at least about 0.5 parts of water per 100 parts of sodium chloride but not enough to dissolve all the sodium chloride until the complex-forming reaction is at least 50% completed, and 2) 2-35 parts of an inert liquid carrier per part of sodium chloride; employing a sodium chloride/MDA ratio of about 1:10 in parts by weight, conducting the reaction between the MDA and sodium chloride with agitation, and recovering directLy from said reaction a dispersion of MDA/sodium chloride complex particles of such fineness that at least 95% have a maximum diameter of about 10 microns.
Claim 4
Dependent Claim
130 words
In a process for forming a complex of 4,4''-methylene dianiline (MDA) and sodium chloride in a mole ratio of 3:1, the improvement comprising adding to a mixture of the MDA and sodium chloride 1) at least about 0.5 parts of water per 100 parts of sodium chloride but not enough to dissolve all the sodium chloride until the complex-forming reaction is at least 50% completed, and 2) 2-35 parts of an inert liquid carrier per part of sodium chloride; employing a sodium chloride/MDA ratio of about 1:10 in parts by weight, conducting the reaction between the MDA and sodium chloride with agitation, and recovering directLy from said reaction a dispersion of MDA/sodium chloride complex particles of such fineness that at least 95% have a maximum diameter of about 10 microns.
Claim 5
Dependent Claim
19 words
The process of claim 1 wherein said process is carried out in the presence of an oil-soluble dispersing agent.
Claim 6
Dependent Claim
11 words
The process of claim 1 wherein said salt is sodium chloride.
Claim 7
Dependent Claim
14 words
The process of claim 1 wherein said reaction takes place at substantially ambient conditions.
Claim 8
Dependent Claim
18 words
The process of claim 1 wherein the reaction takes place at a temperature of less than about 80*C.
Claim 9
Dependent Claim
11 words
The process of claim 1 wherein the salt is lithium chloride.
Claim 10
Dependent Claim
11 words
The process of claim 3 wherein said dispersing agent is lecithin.
Claim 11
Dependent Claim
15 words
The process of claim 3 wherein said dispersing agent is a polyoxypropylated quaternary ammonium halide.
Claim 12
Dependent Claim
11 words
The process of claim 1 wherein said inert liquid is di(2-ethylhexyl)phthalate.
Claim 13
Dependent Claim
13 words
The process of claim 1 wherein said inert liquid is tetraethylene glycol bis(2-ethylhexanoate).
Claim 14
Dependent Claim
26 words
The process of claim 1 wherein said inert liquid is an aromatic process oil which comprises 18% polar compounds, 76% aromatics, and 6% saturated petroleum derivatives.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-08-11 | 1979-02-10 | 1979-08-12 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-08-11 | 1983-02-10 | 1983-08-12 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-08-11 | 1987-02-10 | 1987-08-12 | $7700.00 | Window Closed / Lapsed |