US4474577A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Modified acid dyestuff
Assignee: Bayer Corp
•
Filing: 1983-10-26
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Granted: 1984-10-02
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Expires: 2003-10-26
Abstract
Abstract The present disclosure is concerned with new modifications of the dyestuff Color Index Acid Blue 324 which have significant advantages over the known form of this dyestuff. In particular, the preferred modification is much easier to isolate from an aqueous medium by filtration and the isolated product has a higher purity. The filtration proceeds much more rapidly and gives a filter residue of a much higher solids content. Furthermore, this new form of the dyestuff imparts a dramatically lower viscosity to aqueous dispersions or slurries prepared from it than are obtained using the old form of this dyestuff. These modifications are obtained by heating an aqueous dispersion or slurry of the known form of Color Index Acid Blue 324 to temperatures in excess of about 97° C. and for the preferred form in the presence of a substance which reduces the surface tension between the dispersed organic dyestuff phase and the aqueous dispersing medium. The obtained dyestuff modifications display Debye-Scherrer X-ray diffraction patterns substantially different from that of the commercially available Color Index Acid Blue 324 evidencing that new crystal forms have been obtained. This is confirmed by optical microscopy which shows that the dyestuff undergoes a transformation from sharp, thin needles to either parallelograms or hexagons.
Inventors
- 👤 Charles W. Sandefur
- 👤 Thomas J. Thomas
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 11:51
CPC Classifications
C; C09; C09B; C09B67/00; C09B67/0025; Y; Y10; Y10S; Y10S8/00; Y10S8/916; Y10S8/917; Y10S8/92; Y10S8/924
Claims Analysis
Total Claims: 36
Claim 1
Independent Claim
60 words
A modified form of the dyestuff Color Index Acid Blue 324 selected from the group consisting of a form displaying very strong to moderately strong Debye-Scherrer X-ray diffraction pattern reflections representative of d-spacings at approximately 14.0; 6.8; 5.7; 5.4; 4.6; 4.5; 3.75 and 3.29 angstroms and one displaying such reflections only representative of d-spacings at approximately 14.2 and 4.6 angstroms.
Claim 2
Dependent Claim
60 words
A modified form of the dyestuff Color Index Acid Blue 324 selected from the group consisting of a form displaying very strong to moderately strong Debye-Scherrer X-ray diffraction pattern reflections representative of d-spacings at approximately 14.0; 6.8; 5.7; 5.4; 4.6; 4.5; 3.75 and 3.29 angstroms and one displaying such reflections only representative of d-spacings at approximately 14.2 and 4.6 angstroms.
Claim 3
Dependent Claim
53 words
A modified form of the dyestuff Color Index Acid Blue 324 selected from the group consisting of one displaying a solids content in excess of about 80 wt. % on filtration from an aqueous medium in which it is slurried and one displaying a solids content between about 60 and 80 wt. %.
Claim 4
Dependent Claim
53 words
A modified form of the dyestuff Color Index Acid Blue 324 selected from the group consisting of one displaying a solids content in excess of about 80 wt. % on filtration from an aqueous medium in which it is slurried and one displaying a solids content between about 60 and 80 wt. %.
Claim 5
Dependent Claim
38 words
A form of the dyestuff of the following structural formula: ##STR2## which displays very strong to moderately strong Debye-Scherrer X-ray diffraction pattern reflections representative of d-spacings at approximately 14.0; 6.8; 5.7; 5.4; 4.6; 4.5; 3.75; and 3.29 angstroms.
Claim 6
Dependent Claim
38 words
A form of the dyestuff of the following structural formula: ##STR2## which displays very strong to moderately strong Debye-Scherrer X-ray diffraction pattern reflections representative of d-spacings at approximately 14.0; 6.8; 5.7; 5.4; 4.6; 4.5; 3.75; and 3.29 angstroms.
Claim 7
Dependent Claim
22 words
A form of the dyestuff of the following structural formula: ##STR3## which is characterized by the X-ray diffraction pattern of FIG. 1.
Claim 8
Dependent Claim
22 words
A form of the dyestuff of the following structural formula: ##STR3## which is characterized by the X-ray diffraction pattern of FIG. 1.
Claim 9
Dependent Claim
32 words
A form of the dyestuff Color Index Acid Blue 324 which displays a solids content in excess of 80 wt. % upon filtration from an aqueous medium in which it is slurried.
Claim 10
Dependent Claim
32 words
A form of the dyestuff Color Index Acid Blue 324 which displays a solids content in excess of 80 wt. % upon filtration from an aqueous medium in which it is slurried.
Claim 11
Dependent Claim
42 words
A form of the dyestuff Color Index Acid Blue 324 which can be dispersed at a 30 wt. % solids level into an aqueous medium without causing the room temperature viscosity at 12 rpm of the dispersion to exceed about 100 cps.
Claim 12
Dependent Claim
42 words
A form of the dyestuff Color Index Acid Blue 324 which can be dispersed at a 30 wt. % solids level into an aqueous medium without causing the room temperature viscosity at 12 rpm of the dispersion to exceed about 100 cps.
Claim 13
Dependent Claim
86 words
The form of the dyestuff Color Index Acid Blue 324 which is obtained by subjecting the dyestuff in the form of sharp thin needles to a temperature in excess of 97° C. in an aqueous medium having a pH of 7 or greater which also contains a material which reduces the surface tension between the dyestuff and the aqueous medium with the weight ratio of this material to the dyestuff being greater than about 0.05 until the dyestuff is in the form of sharp edged parallelograms.
Claim 14
Dependent Claim
86 words
The form of the dyestuff Color Index Acid Blue 324 which is obtained by subjecting the dyestuff in the form of sharp thin needles to a temperature in excess of 97° C. in an aqueous medium having a pH of 7 or greater which also contains a material which reduces the surface tension between the dyestuff and the aqueous medium with the weight ratio of this material to the dyestuff being greater than about 0.05 until the dyestuff is in the form of sharp edged parallelograms.
Claim 15
Dependent Claim
90 words
A process for producing an improved form of the dyestuff of the structural formula ##STR4## comprising slurrying it in an aqueous medium which has a pH in excess of about 6.0 and which also contains a material which reduces the surface tension between the organic dyestuff phase and the aqueous medium with the weight ratio of this material to the dyestuff being greater than about 0.05 and maintaining this slurry at a temperature in excess of about 97° C. until the dyestuff is in the form of sharp edged parallelograms.
Claim 16
Dependent Claim
90 words
A process for producing an improved form of the dyestuff of the structural formula ##STR4## comprising slurrying it in an aqueous medium which has a pH in excess of about 6.0 and which also contains a material which reduces the surface tension between the organic dyestuff phase and the aqueous medium with the weight ratio of this material to the dyestuff being greater than about 0.05 and maintaining this slurry at a temperature in excess of about 97° C. until the dyestuff is in the form of sharp edged parallelograms.
Claim 17
Dependent Claim
16 words
The process of claim 8 wherein the surface tension reducing material is a surfactant or dispersant.
Claim 18
Dependent Claim
12 words
The process of claim 9 wherein the dispersant or surfactant is anionic.
Claim 19
Dependent Claim
13 words
The process of claim 10 wherein the dispersant is a sodium lignin sulphonate.
Claim 20
Dependent Claim
18 words
The process of claim 8 wherein the slurry is held at reflux until the improved form is obtained.
Claim 21
Dependent Claim
17 words
The process of claim 8 wherein the pH of the aqueous medium is greater than about 7.0.
Claim 22
Dependent Claim
18 words
The process of claim 13 wherein the pH of the aqueous medium is between about 7 and 10.
Claim 23
Dependent Claim
21 words
The process of claim 8 wherein the weight ratio of surface tension reducing material to dyestuff is at least about 0.08.
Claim 24
Dependent Claim
88 words
A process for producing an improved form of the dyestuff Color Index Acid Blue 324 comprising slurrying it in an aqueous medium which has a pH in excess of about 6 and which also contains a material which reduces the surface tension between the organic dyestuff phase and the aqueous medium with the weight ratio of this material to the dyestuff being greater than about 0.05 and maintaining this slurry at a temperature in excess of about 97° C. until the viscosity of the slurry ceases to decrease.
Claim 25
Dependent Claim
88 words
A process for producing an improved form of the dyestuff Color Index Acid Blue 324 comprising slurrying it in an aqueous medium which has a pH in excess of about 6 and which also contains a material which reduces the surface tension between the organic dyestuff phase and the aqueous medium with the weight ratio of this material to the dyestuff being greater than about 0.05 and maintaining this slurry at a temperature in excess of about 97° C. until the viscosity of the slurry ceases to decrease.
Claim 26
Dependent Claim
53 words
The process of claim 16 wherein: (a) the pH is at least about 7; (b) the surface tension reducing material is an anionic surfactant or dispersant; (c) the weight ratio of dispersant to dyestuff is at least about 0.08; and (d) the slurry is held at reflux until its viscosity ceases to decrease.
Claim 27
Dependent Claim
36 words
A process of dispersing a Color Index Acid Blue 324 having a crystal structure with d-spacings at approximately 14.0; 6.8; 5.7; 5.4; 4.6; 4.5; 3.75 and 3.29 angstroms comprising combining the dyestuff with water and agitating.
Claim 28
Dependent Claim
36 words
A process of dispersing a Color Index Acid Blue 324 having a crystal structure with d-spacings at approximately 14.0; 6.8; 5.7; 5.4; 4.6; 4.5; 3.75 and 3.29 angstroms comprising combining the dyestuff with water and agitating.
Claim 29
Dependent Claim
32 words
The process of claim 18 wherein the room temperature 12 rpm viscosity of the dispersion at 30% solids is less than 100 cps and at 50% solids is less than 3000 cps.
Claim 30
Dependent Claim
41 words
A process of spray drying the dyestuff Color Index Acid Blue 324 comprising using a slurry of at least 40 wt. % solids of the crystal form having d-spacings at approximately 14.0; 6.8; 5.7; 5.4; 4.6; 4.5; 3.75 and 3.29 angstroms.
Claim 31
Dependent Claim
41 words
A process of spray drying the dyestuff Color Index Acid Blue 324 comprising using a slurry of at least 40 wt. % solids of the crystal form having d-spacings at approximately 14.0; 6.8; 5.7; 5.4; 4.6; 4.5; 3.75 and 3.29 angstroms.
Claim 32
Dependent Claim
95 words
A process of recovering the dyestuff Color Index Acid Blue 324 from its synthesis bath comprising (a) adding an anionic surfactant or dispersant to the reaction slurry in a weight ratio to the dyestuff present of greater than about 0.05; (b) controlling the pH of the slurry to a value in excess of 6; (c) holding the slurry at a temperature in excess of about 97° C. until either the viscosity of the slurry ceases to decrease or the dyestuff is in the form of sharp edged parallelograms; and (d) isolating the dyestuff by filtration.
Claim 33
Dependent Claim
95 words
A process of recovering the dyestuff Color Index Acid Blue 324 from its synthesis bath comprising (a) adding an anionic surfactant or dispersant to the reaction slurry in a weight ratio to the dyestuff present of greater than about 0.05; (b) controlling the pH of the slurry to a value in excess of 6; (c) holding the slurry at a temperature in excess of about 97° C. until either the viscosity of the slurry ceases to decrease or the dyestuff is in the form of sharp edged parallelograms; and (d) isolating the dyestuff by filtration.
Claim 34
Dependent Claim
15 words
The process of claim 19 wherein the filtration is accomplished by a continuous belt filter.
Claim 35
Dependent Claim
94 words
A process for modifying the dyestuff Color Index Acid Blue 324 obtained in the form of thin sharp crystals comprising slurrying it into an aqueous medium which has a pH in excess of about 6 and which contains less than 5 wt. %, based on the weight of the dyestuff, of a substance which reduces the surface tension between the organic dyestuff phase and the aqueous medium and holding the slurry at a temperature in excess of about 97° C. until a substantial portion of the dyestuff is in the form of hexagonal crystals.
Claim 36
Dependent Claim
94 words
A process for modifying the dyestuff Color Index Acid Blue 324 obtained in the form of thin sharp crystals comprising slurrying it into an aqueous medium which has a pH in excess of about 6 and which contains less than 5 wt. %, based on the weight of the dyestuff, of a substance which reduces the surface tension between the organic dyestuff phase and the aqueous medium and holding the slurry at a temperature in excess of about 97° C. until a substantial portion of the dyestuff is in the form of hexagonal crystals.
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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) | 1987-10-02 | 1988-04-02 | 1988-10-02 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1991-10-02 | 1992-04-02 | 1992-10-02 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1995-10-02 | 1996-04-02 | 1996-10-02 | $7700.00 | Window Closed / Lapsed |