US4590262A
Expired / Lapsed
US
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Low electrolyte sodium lignosulfonates
Assignee: Westvaco Corp
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Filing: 1984-10-05
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Granted: 1986-05-20
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Expires: 2004-10-05
Abstract
Abstract A method of producing sodium salts of low electrolyte-containing sulfonates suited for use as dye and print paste additives comprising of the steps of ionizing the phenol component of a lignin material in an alkaline liquid medium, methylolating the ionized phenol component of 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 a sodium 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 salts and electrolytes produced when acidifying the lignin for dye and print paste composition additives. Lignin products produced by the method, and dye and print paste 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 08:30
CPC Classifications
C; C07; C07G; C07G1/00; C08; C08H; C08H6/00; C09; C09B; C09B67/00; C09B67/0071; C09B67/0084; C09B67/0085; C09B67/0086; C09D; C09D17/00
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
103 words
A method of producing sodium salts of low electrolyte-containing lignosulfonates suited for use as dye and print paste additives comprising the steps of: (a) ionizing a phenol component of kraft lignin material in an alkaline liquid medium, (b) methylolating the ionized phenol component of the lignin material, (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 a sodium salt of a sulphur-oxygen containing compound in a liquid medium.
Claim 2
Independent Claim
103 words
A method of producing sodium salts of low electrolyte-containing lignosulfonates suited for use as dye and print paste additives comprising the steps of: (a) ionizing a phenol component of kraft lignin material in an alkaline liquid medium, (b) methylolating the ionized phenol component of the lignin material, (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 a sodium salt of a sulphur-oxygen containing compound in a liquid medium.
Claim 3
Dependent Claim
25 words
A method as defined in claim 1 wherein the lignin material is sulfonated while maintaining the pH of the liquid medium at 7.0 or below.
Claim 4
Dependent Claim
28 words
A method as defined in claim 2 wherein the ionized phenol component of the lignin material is methylolated at a pH level of between about 9.5 to 12.5.
Claim 5
Dependent Claim
13 words
A method as defined in claim 3 wherein the methylolation pH is 11.0.
Claim 6
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 7
Dependent Claim
18 words
A method as defined in claim 5 wherein the lignin material is sulfonated by reaction with sodium bisulfite.
Claim 8
Independent Claim
140 words
A method of preparing sulfonated lignins particularly suited for use as dye and print paste additives comprising the steps of: (a) isolating a lignin material from black liquor of a 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 methylolating compound 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 a sulfonating compound in a liquid medium under conditions to produce a sulfomethylated lignin product having low inorganic salt and electrolyte content and a pH level in a liquid medium of less than about 7.0.
Claim 9
Independent Claim
140 words
A method of preparing sulfonated lignins particularly suited for use as dye and print paste additives comprising the steps of: (a) isolating a lignin material from black liquor of a 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 methylolating compound 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 a sulfonating compound in a liquid medium under conditions to produce a sulfomethylated lignin product having low inorganic salt and electrolyte content and a pH level in a liquid medium of less than about 7.0.
Claim 10
Dependent Claim
105 words
A sodium salt of a low electrolyte-containing sulfomethylated lignin particularly suited for use as a dye and print paste additive prepared by the steps of: (a) ionizing a phenol component of kraft lignin material in an alkaline liquid medium; (b) methylolating the ionized phenol component of the lignin material; (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 a sodium salt of a sulphur-oxygen containing compound in a liquid medium.
Claim 11
Dependent Claim
105 words
A sodium salt of a low electrolyte-containing sulfomethylated lignin particularly suited for use as a dye and print paste additive prepared by the steps of: (a) ionizing a phenol component of kraft lignin material in an alkaline liquid medium; (b) methylolating the ionized phenol component of the lignin material; (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 a sodium salt of a sulphur-oxygen containing compound in a liquid medium.
Claim 12
Dependent Claim
60 words
The sodium salt of a low electrolyte-containing sulfomethylated lignin as defined in claim 8 wherein the lignin is further defined as having about one mole or less sulfonation per 1,000 grams lignin and a free inorganic salt content of between about 0.5 to 3% by weight based on the dry weight of the lignin at a pH of about 7.
Claim 13
Dependent Claim
62 words
The sodium salt of a low electrolyte-containing sulfomethylated lignin as defined in claim 8 wherein the lignin is further defined as having a sulfonation of about 1.6 moles or greater per 1,000 grams of lignin and a free inorganic salt content of between about 6.7 to 10% by weight based on dry weight of the lignin at a pH of about 7.0.
References Cited (Backward Citations)
US2525433A
Cited
US2680113A
Cited
US2690973A
Cited
US3094515A
Cited
US3296159A
Cited
US3156520A
Cited
US3503762A
Cited
US3546197A
Cited
US3726850A
Cited
US3769272A
Cited
US3841887A
Cited
US4184845A
Cited
US4001202A
Cited
US4047567A
Cited
US4069217A
Cited
US4131564A
Cited
US4236579A
Cited
US4308203A
Cited
US4355996A
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) | 1989-05-19 | 1989-11-18 | 1990-05-20 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-05-19 | 1993-11-18 | 1994-05-20 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-05-19 | 1997-11-18 | 1998-05-20 | $7700.00 | Window Closed / Lapsed |