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US4523924A
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US
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Process for the preparation of stable aqueous solutions of water-soluble reactive dyes by membrane separation
Assignee: BASF Corp
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Filing: 1983-12-12
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Granted: 1985-06-18
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Expires: 2003-12-12
Abstract
Abstract The invention describes a process for the preparation of stable aqueous solutions of water-soluble reactive dyes, starting from an aqueous solution or suspension of the crude reactive dye which is concentrated and at least partially desalted by a membrane separation process. The process of the invention comprises continuously replacing part of the water which is drawn off from the dyestuff solution or suspension during the membrane separation process with demineralized water, whereby the concentration of calcium and magnesium ions in the dyestuff solution does not exceed 0.01% by weight. The concentrated and desalted dyestuff solution is stabilized by addition of a polyphosphate or dihydrogen phosphate/polyphosphate buffer, and a component which improves the water-solubility of the dye is optionally added. The formulations so obtained are readily storable for several months in the temperature range from -10° to +40° C.
Inventors
- 👤 Roger Lacroix
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-22 23:46
CPC Classifications
C; C09; C09B; C09B67/00; C09B67/0071; C09B67/0072; C09B67/0073; C09B67/0096; Y; Y10; Y10S; Y10S8/00; Y10S8/916; Y10S8/918
Claims Analysis
Total Claims: 12
Claim 1
Independent Claim
154 words
A process for the preparation of a stable aqueous formulation which contains a water-soluble reactive dye, comprising the steps of (i) treating, under a pressure of 10 to 100 bar, an aqueous solution or suspension of the crude dye with a semipermeable asymmetrical membrane, suitable for reverse osmosis and having a pore diameter of 0.1 to 50 nm, which membrane is modified by polyfunctional compounds containing ionic groups, the basic skeleton consisting of cellulose acetate, polyacrylonitrile or a copolymer of acrylonitrile and ethylenically unsaturated monomer; so as to concentrate the dye solution and at least partially remove salts thereform; and, at the same time, replacing part of the water which is drawn off from the dye solution or suspension with demineralized water so that the total calcium and magnesium ion concentration does not exceed 0.01% by weight and (ii) further stabilizing the obtained dye solution by addition of a polyphosphate or dihydrogen phosphate/polyphosphate buffer.
Claim 2
Dependent Claim
154 words
A process for the preparation of a stable aqueous formulation which contains a water-soluble reactive dye, comprising the steps of (i) treating, under a pressure of 10 to 100 bar, an aqueous solution or suspension of the crude dye with a semipermeable asymmetrical membrane, suitable for reverse osmosis and having a pore diameter of 0.1 to 50 nm, which membrane is modified by polyfunctional compounds containing ionic groups, the basic skeleton consisting of cellulose acetate, polyacrylonitrile or a copolymer of acrylonitrile and ethylenically unsaturated monomer; so as to concentrate the dye solution and at least partially remove salts thereform; and, at the same time, replacing part of the water which is drawn off from the dye solution or suspension with demineralized water so that the total calcium and magnesium ion concentration does not exceed 0.01% by weight and (ii) further stabilizing the obtained dye solution by addition of a polyphosphate or dihydrogen phosphate/polyphosphate buffer.
Claim 3
Dependent Claim
22 words
The process of claim 1, wherein the overall salt concentration in the dye solution is lowered to less than 1% by weight.
Claim 4
Dependent Claim
17 words
The process of claim 2, wherein the salt concentration is lowered to less than 0.5% by weight.
Claim 5
Dependent Claim
15 words
The process of claim 1, wherein the buffer is a tripolyphosphate or dihydrogen phosphate/tripolyphosphate mixture.
Claim 6
Dependent Claim
25 words
The process of claim 1, wherein the buffer is added in an amount of 0.5 to 5% by weight, based on the final dyestuff formulation.
Claim 7
Dependent Claim
21 words
The process of claim 1, wherein the pH of the dyestuff solution is adjusted to 7-8 by addition of the buffer.
Claim 8
Dependent Claim
18 words
The process of claim 1, wherein a component is added which further improves the water-solubility of the dye.
Claim 9
Dependent Claim
11 words
The process of claim 6, wherein ε-caprolactam or N-methylpyrrolidone is added.
Claim 10
Dependent Claim
61 words
An aqueous dye solution obtained by the process of claim 1, said solution comprising 10 to 40% by weight of a water-soluble reactive dye, 0.5 to 5% by weight of a polyphosphate or dihydrogen phosphate/polyphosphate buffer, less than 0.01% by weight of calcium and/or magnesium ions, less than 1% by weight of inert salts, 50 to 85% by weight of water.
Claim 11
Dependent Claim
24 words
The dye solution of claim 9, which further contains 1 to 20% by weight of a component which improves the water-solubility of the dye.
Claim 12
Dependent Claim
25 words
A process for dyeing or printing cellulose fiber material, which comprises applying to said material a dye solution obtained by the process of claim 1.
References Cited (Backward Citations)
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1988-06-17 | 1988-12-17 | 1989-06-18 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1992-06-17 | 1992-12-17 | 1993-06-18 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1996-06-17 | 1996-12-17 | 1997-06-18 | $7700.00 | Window Closed / Lapsed |