US4642336A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Ammonium lignosulfonates
Assignee: WESTVACO Corp A CORP OF
•
Filing: 1984-12-10
•
Granted: 1987-02-10
•
Expires: 2004-12-10
Abstract
Abstract A method of producing ammonium salts of sulfomethylated lignins suited for use as dyestuff and coal-water slurry additives comprising of the steps of ionizing the phenol component of a lignin material by-product of the black liquor of a kraft paper-making process in an alkaline liquid medium, methylolating the lignin material, lowering the pH of the liquid medium to an acid pH to precipitate the methylolated lignin material, washing the precipitated lignin material with water to remove inorganic salts and residual reactants therefrom, and sulfonating the washed, purified methylolated lignin material with an ammonium salt of a sulphur-oxygen containing compound in a liquid medium. The washed, purified methylolated lignin material is preferably sulfonated at an acid pH level to minimize the production of electrolytes when the lignin is to be used for dyeing at low pH. Lignin products produced by the method, as well as dye and coal-water slurry compositions containing such products are also disclosed.
Inventors
- 👤 Peter Dilling
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-26 00:05
CPC Classifications
C; C07; C07G; C07G1/00; C08; C08H; C08H6/00
Claims Analysis
Total Claims: 10
Claim 1
Independent Claim
108 words
A method of producing ammonium salts of lignosulfonates particularly suited for use as additives in dyestuff compositions and coal-water slurries comprising the steps of: (a) ionizing a phenol component of a kraft lignin material in an alkaline liquid medium, (b) methylolating the lignin material in the ortho position of the phenol component, (c) lowering the pH of the liquid medium to an acid pH to precipitate the methylolated lignin material, (d) washing the precipitated lignin material with water to remove inorganic salts and residual reactants therefrom, and (e) sulfonating the washed, purified methylolated lignin material with an ammonium salt of a sulphur-oxygen containing compound in a liquid medium.
Claim 2
Independent Claim
108 words
A method of producing ammonium salts of lignosulfonates particularly suited for use as additives in dyestuff compositions and coal-water slurries comprising the steps of: (a) ionizing a phenol component of a kraft lignin material in an alkaline liquid medium, (b) methylolating the lignin material in the ortho position of the phenol component, (c) lowering the pH of the liquid medium to an acid pH to precipitate the methylolated lignin material, (d) washing the precipitated lignin material with water to remove inorganic salts and residual reactants therefrom, and (e) sulfonating the washed, purified methylolated lignin material with an ammonium salt of a sulphur-oxygen containing compound in a liquid medium.
Claim 3
Dependent Claim
26 words
A method as defined in claim 1 wherein the lignin material is sulfonated while maintaining the pH of the liquid medium at about 7.0 or below.
Claim 4
Dependent Claim
20 words
A method as defined in claim 2 wherein the methylolated lignin material is sulfonated at a pH of about 6.3.
Claim 5
Dependent Claim
23 words
A method as defined in claim 2 wherein the lignin material is methylolated at a pH level of between about 9.5 to 12.5.
Claim 6
Dependent Claim
14 words
A method as defined in claim 3 wherein the methylolation pH is about 11.0.
Claim 7
Dependent Claim
22 words
A method as defined in claim 5 wherein the lignin material is sulfonated by reaction with an ammonium sulfite or bisulfite compound.
Claim 8
Independent Claim
134 words
A method of preparing sulfonated lignins particularly suited for use as additives in dyestuff compositions and coal-water slurries comprising the steps of: (a) isolating a lignin material from black liquor of a kraft paper-making process, (b) dispersing the material in an alkaline liquid medium to ionize the phenolic component of the lignin material, (c) treating the ionized lignin material with a formaldehyde to methylolate the same, (d) reducing the pH of the liquid medium to an acidic level to precipitate the methylolated lignin, (e) washing the precipitated methylolated lignin with water to remove inorganic salts and residual reactants therefrom, and (f) treating the methylolated lignin with an ammonium salt of a sulfonating compound in a liquid medium under conditions to produce an ammonium salt of a sulfomethylated lignin product having low inorganic electrolyte content.
Claim 9
Independent Claim
134 words
A method of preparing sulfonated lignins particularly suited for use as additives in dyestuff compositions and coal-water slurries comprising the steps of: (a) isolating a lignin material from black liquor of a kraft paper-making process, (b) dispersing the material in an alkaline liquid medium to ionize the phenolic component of the lignin material, (c) treating the ionized lignin material with a formaldehyde to methylolate the same, (d) reducing the pH of the liquid medium to an acidic level to precipitate the methylolated lignin, (e) washing the precipitated methylolated lignin with water to remove inorganic salts and residual reactants therefrom, and (f) treating the methylolated lignin with an ammonium salt of a sulfonating compound in a liquid medium under conditions to produce an ammonium salt of a sulfomethylated lignin product having low inorganic electrolyte content.
Claim 10
Dependent Claim
35 words
A method as defined in claim 7 wherein the sulfomethylated lignin products produced thereby have a non-sulfomethylated lignin residue of less than about 0.1% by weight, based on the dry weight of the sulfomethylated lignin.
References Cited (Backward Citations)
US2525433A
Cited
US2680113A
Cited
US2690973A
Cited
US3094515A
Cited
US3156520A
Cited
US3503762A
Cited
US3726850A
Cited
US3769272A
Cited
US3841887A
Cited
US4184845A
Cited
US4001202A
Cited
US4047567A
Cited
US4131564A
Cited
US4308203A
Cited
US4355996A
Cited
US4465495A
Cited
US4546173A
Cited
US4521336A
Cited
US4551151A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1990-02-09 | 1990-08-11 | 1991-02-10 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1994-02-09 | 1994-08-11 | 1995-02-10 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1998-02-09 | 1998-08-11 | 1999-02-10 | $7700.00 | Window Closed / Lapsed |