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US4077767A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for the preparation of concentrated solutions of urea compounds

Assignee: Bayer AG
•
Filing: 1975-10-14
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Granted: 1978-03-07
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Expires: 1995-10-14
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Abstract

Abstract The invention relates to the preparation of storage-stable, concentrated solutions of urea compounds of the formula F.sub.1 --HN--CO--NH--F.sub.2 wherein F 1 and F 2 denote radicals of dyestuffs or dyestuff intermediates containing acid groups by reacting 2 equivalents of amines of the formula F.sub.1,2 --NH.sub.2 with one equivalent of a compound of the formula Cl--CO--X wherein X is chlorine or an aryloxy radical in the presence of alkaline earth metal ions in the pH range of 4.0 to 8.0, separating off the sparingly soluble alkaline earth metal salt of the resulting urea compounds, adding -- for example -- a salt of lithium of which the anion forms a salt, which is sparingly soluble in the reaction medium, with the alkaline earth metal cation of the urea compound to the suspension of these urea compounds and separating off the alkaline earth metal salt which has precipitated.

Inventors

  • 👤 Wolf-Eckhard Bleck
  • 👤 Horst Nickel
  • 👤 Erich Kramer

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-05 14:56
CPC Classifications
C; C09; C09B; C09B67/00; C09B67/0071; C09B67/0072; C09B67/0073; C09B43/00; C09B43/12; C09B43/136; C09B43/14; C09B69/00; C09B69/02; C09B69/04

Claims Analysis

Total Claims: 8
Claim 1
Independent Claim 264 words
In a process for preparing a concentrated aqueous or aqueous/organic solution of low electrolyte content containing 10-60% by weight of an urea compound of the formula F.sub.1 --NH--CO--NH--F.sub.2 wherein F 1 and F 2 are identical or different radicals of dyestuffs or dyestuff intermediates containing acid groups, by reaction of an equivalent of each of two amines of the formulas F.sub.1 --NH.sub.2 and F.sub.2 --NH.sub.2 with one equivalent of Cl--CO--X wherein X is chlorine or aryloxy; the improvement which comprises: (1) conducting the reaction of a pH at 4.0-8.0 in the presence of an amount of alkaline earth metal ions equivalent to the acid groups present in F 1 and F 2 ; (2) removing the sparingly soluble alkaline earth metal salt of said urea compound; (3) suspending said alkaline earth metal salt of said urea compound in water or a mixture of water and a water miscible organic solvent; (4) adding to the resulting suspension (a) a salt of lithium, an ammonium salt, or a salt of an organic base wherein the amount of such salt and said alkaline earth metal ions are capable of forming an second alkaline earth metal salt which is not more than sparingly soluble in the liquid medium of said suspension, or (b) equivalent amounts of the appropriate acid and base to form in situ said salt of lithium, said ammonium salt, or said salt or an organic base; (5) removing said second alkaline earth metal salt as a precipitate; and (6) recovering a solution containing a low electrolyte concentration and 10%-10% by weight of said urea compound.
Claim 2
Dependent Claim 264 words
In a process for preparing a concentrated aqueous or aqueous/organic solution of low electrolyte content containing 10-60% by weight of an urea compound of the formula F.sub.1 --NH--CO--NH--F.sub.2 wherein F 1 and F 2 are identical or different radicals of dyestuffs or dyestuff intermediates containing acid groups, by reaction of an equivalent of each of two amines of the formulas F.sub.1 --NH.sub.2 and F.sub.2 --NH.sub.2 with one equivalent of Cl--CO--X wherein X is chlorine or aryloxy; the improvement which comprises: (1) conducting the reaction of a pH at 4.0-8.0 in the presence of an amount of alkaline earth metal ions equivalent to the acid groups present in F 1 and F 2 ; (2) removing the sparingly soluble alkaline earth metal salt of said urea compound; (3) suspending said alkaline earth metal salt of said urea compound in water or a mixture of water and a water miscible organic solvent; (4) adding to the resulting suspension (a) a salt of lithium, an ammonium salt, or a salt of an organic base wherein the amount of such salt and said alkaline earth metal ions are capable of forming an second alkaline earth metal salt which is not more than sparingly soluble in the liquid medium of said suspension, or (b) equivalent amounts of the appropriate acid and base to form in situ said salt of lithium, said ammonium salt, or said salt or an organic base; (5) removing said second alkaline earth metal salt as a precipitate; and (6) recovering a solution containing a low electrolyte concentration and 10%-10% by weight of said urea compound.
Claim 3
Dependent Claim 11 words
Process of claim 1, wherein said alkaline earth metal is calcium.
Claim 4
Dependent Claim 10 words
Process of claim 1, wherein said acid is sulfuric acid.
Claim 5
Dependent Claim 23 words
Process of claim 1, wherein said reaction is carried out in the absence of an organic solvent and said suspension liquid is water.
Claim 6
Dependent Claim 17 words
Process of claim 1, wherein F 1 --NH 2 and F 2 --NH 2 are aminomonoazo dyestuffs.
Claim 7
Dependent Claim 9 words
Concentrated solutions obtained by the process of claim 1.
Claim 8
Dependent Claim 13 words
Concentrated solutions of claim 6 containing 20-50% by weight of said urea compound.

References Cited (Backward Citations)

GB1202800A Cited
GB1202798A Cited
US3643269A Cited
GB1202799A Cited
US3701624A Cited
GB1331142A Cited
US3898033A Cited
NL7204084A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1981-03-06 1981-09-05 1982-03-07 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-03-06 1985-09-05 1986-03-07 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-03-06 1989-09-05 1990-03-07 $7700.00 Window Closed / Lapsed

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