Patent US4298526A successfully refreshed from Google Patents.
US4298526A
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US
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Preparation of easily dispersible and deeply colored pigmentary forms
Assignee: BASF SE
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Filing: 1979-11-16
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Granted: 1981-11-03
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Expires: 1999-11-16
Abstract
Abstract A process for the preparation of pigmentary forms of phthalocyanine and of insoluble polycyclic compounds, wherein the crude pigment is milled in the presence of one or more acids which have a pK of <4.9 and are non-oxidizing under the milling conditions, until the primary particle size is ≦0.1 μm, the milled material is then finished in the conventional manner in a solvent in the presence or absence of water, and the pigment is isolated. The pigments give very deep colorations and are very easily dispersible in the media in which they are used.
Inventors
- 👤 Reinhard Sappok
- 👤 Fritz Guellich
- 👤 Karl Roth
- 👤 Alois Wiesenberger
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 08:55
CPC Classifications
C; C09; C09B; C09B67/00; C09B67/0001; C09B67/0017; C09B67/0014
Claims Analysis
Total Claims: 10
Claim 1
Independent Claim
127 words
In a process for the preparation of an easily dispersible and deeply colored pigmentary form of a phthalocyanine selected from the group consisting of metal-free phthalocyanine, metalized phthalocyanines containing up to 2 chlorine or bromine atoms in the molecule, and polyhalophthalocyanines, by comminuting the crude pigment under shearing stress and impact stress in the absence of milling assistants, converting the milled material to a pigmentary form by recrystallization in organic solvent, and isolating the pigment, the improvement which comprises comminuting the crude pigment in the presence of from 0.5 to 15 percent by weight, based on crude pigment, of one or more acids which have a pK of <4.9 and are non-oxidizing under the milling conditions until the primary particle size is not greater than 0.1 μm.
Claim 2
Dependent Claim
127 words
In a process for the preparation of an easily dispersible and deeply colored pigmentary form of a phthalocyanine selected from the group consisting of metal-free phthalocyanine, metalized phthalocyanines containing up to 2 chlorine or bromine atoms in the molecule, and polyhalophthalocyanines, by comminuting the crude pigment under shearing stress and impact stress in the absence of milling assistants, converting the milled material to a pigmentary form by recrystallization in organic solvent, and isolating the pigment, the improvement which comprises comminuting the crude pigment in the presence of from 0.5 to 15 percent by weight, based on crude pigment, of one or more acids which have a pK of <4.9 and are non-oxidizing under the milling conditions until the primary particle size is not greater than 0.1 μm.
Claim 3
Dependent Claim
34 words
A process as claimed in claim 1, wherein the crude pigment is comminuted in the presence of from 1 to 10 percent by weight, based on crude pigment, of one or more non-oxidizing acids.
Claim 4
Dependent Claim
34 words
A process as claimed in claim 1, wherein the crude pigment is comminuted in the presence of from 2 to 7 percent by weight, based on crude pigment, of one or more non-oxidizing acids.
Claim 5
Dependent Claim
29 words
A process as claimed in claim 1 or 3, wherein one or more acids which have a pK of <2.5 and are non-oxidizing under the milling conditions are used.
Claim 6
Dependent Claim
142 words
A process as claimed in claim 1 or 2, wherein the acids used are 85-100% strength by weight sulfuric acid, 85-100% strength by weight phosphoric acid, C 1 -C 20 -alkanesulfonic acids, benzenesulfonic acid, naphthalenesulfonic acids, mono-C 1 -C 20 -alkylbenzenesulfonic acids, di-C 1 -C 20 -alkylbenzenesulfonic acids, mono-C 1 -C 20 -alkylnaphthalenesulfonic acids, di-C 1 -C 20 -alkylnaphthalenesulfonic acids, mono-C 1 -C 20 -alkylphenolsulfonic acids, di-C 1 -C 20 -alkylphenolsulfonic acids, mono-C 1 -C 20 -alkylnaphtholsulfonic acids, di-C 1 -C 20 -alkylnaphtholsulfonic acids, alk-1-ene-1-sulfonic acids of 8 to 20 carbon atoms, 2-hydroxy-alkane-1-sulfonic acids of 8 to 20 carbon atoms, monochloroacetic acid, dichloroacetic acid, trichloroacetic acid, trifluoroacetic acid, maleic acid, dihydroxymaleic acid, tartaric acid, dihydroxytartaric acid, sulfuric acid half-esters of C 1 -C 20 -alkanols, alkanoic acids of 1 to 5 carbon atoms, or mixtures of two or more of these acids.
Claim 7
Dependent Claim
52 words
A process claimed in claim 1 or 3, wherein the acid used is 85-100% strength by weight sulfuric acid, 85-100% strength by weight phosphoric acid, formic acid, glacial acetic acid, propionic acid, trichloroacetic acid, methanesulfonic acid, benzenesulfonic acid, toluenesulfonic acids, naphthalenesulfonic acids, or a mixture of two or more of these acids.
Claim 8
Dependent Claim
43 words
A process as claimed in claim 1, wherein the crude pigment used is copper phthalocyanine which contains up to 2 chlorine or bromine atoms per molecule, metal-free phthalocyanine, polychloro-copper phthalocyanines, or polychloro-bromo-copper phthalocyanines which contain up to 14 bromine atoms in the molecule.
Claim 9
Dependent Claim
24 words
A process as claimed in claim 1, wherein the recrystallization is carried out in one or more organic solvents in the presence of water.
Claim 10
Dependent Claim
129 words
A process as claimed in claim 1 or 8, wherein the organic solvents used are selected from the grup consisting of aliphatic and aromatic hydrocarbons, C 1 -C 8 -alkanols, C 2 -C 4 -diols, mono-C 1 -C 5 -alkyl ethers of C 2 -C 4 -diols, diethylene glycol, triethylene glycol, C 1 -C 4 -alkyl ethers of diethylene glycol, of triethylene glycol and of dipropylene glycol, cyclohexanol, C 3 -C 8 -alkanones, aliphatic C 4 -C 8 -ethers, tetrahydrofuran, dioxane, C 3 -C 16 -alkylamines, aniline, N,N-dimethylaniline, toluidines, xylidines, C 1 -C 3 -alkanoic acid amides, N-C 1 -C 4 -alkyl-C 1 -C 3 -alkanoic acid amides, N,N-di-C 1 -C 4 -alkyl-C 1 -C 3 -alkanoic acid amides, N-methylpyrrolidone, pyrrolidone, and mixtures of two or more of these.
References Cited (Backward Citations)
US2716649A
Cited
US2930796A
Cited
DE1239270B
Cited
DE2103030A1
Cited
DE2252461A1
Cited
US3872103A
Cited
DE2316536A1
Cited
US3976649A
Cited
DE2357077A1
Cited
US4141904A
Cited
DE2512610A1
Cited
DE2506832A1
Cited
US4039346A
Cited
DE2545701A1
Cited
US4115386A
Cited
DE2546266A1
Cited
DE2554252A1
Cited
US4104276A
Cited
DE2635157A1
Cited
DE2745893A1
Cited
US4158572A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1984-11-02 | 1985-05-04 | 1985-11-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-11-02 | 1989-05-04 | 1989-11-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-11-02 | 1993-05-04 | 1993-11-03 | $7700.00 | Window Closed / Lapsed |