US4104276A
Expired / Lapsed
US
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Conversion of crude copper phthalocyanines to a pigmentary form
Assignee: BASF SE
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Filing: 1976-11-08
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Granted: 1978-08-01
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Expires: 1996-11-08
Abstract
Abstract A process for converting crude copper phthalocyanine to a pigmentary form, wherein finely divided and heavily agglomerated crude copper phthalocyanine which exhibits disturbed crystallization and which has a primary particle size of less than 0.1 μum is introduced into an organic or aqueous organic medium together with from 0.5 to 7% by weight, based on the crude copper phthalocyanine, of a basic copper phthalocyanine of the formula ##STR1## or of mixtures thereof (where CuPc is an n-valent copper phthalocyanine radical, R 1 is H or alkyl of 1 to 4 carbon atoms, A is linear or branched alkylene, R 2 is alkyl of 1 to 20 carbon atoms, alkoxyalkyl of 3 to 12 carbon atoms or cycloalkyl of 6 to 8 carbon atoms, R 3 is H, alkyl of 1 to 4 carbon atoms or cycloalkyl of 6 to 8 carbon atoms or ##STR2## is a saturated heterocyclic 5-membered, 6-membered or 7-membered ring, and n is an integer from 1 to 6), and the suspension is heated at from room temperature to 180° C until the pigment exhibits optimum tinctorial strength. Pigments of high tinctorial strength, which give colorations having a pure hue, are obtained.
Inventors
- 👤 Joachim Kranz
- 👤 Werner Jettmar
- 👤 Rudolf Polster
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 03:28
CPC Classifications
C; C09; C09B; C09B67/00; C09B67/0033; C09B67/0034; C09B67/0035; C09B47/00; C09B47/04; C09B47/08; C09B47/12; C09B47/24; C09B47/26
Claims Analysis
Total Claims: 11
Claim 1
Independent Claim
251 words
In a process for converting crude copper phthalocyanines to a pigmentary form by treating finely divided and heavily agglomerated copper phthalocyanines which exhibit disturbed crystallization and have a primary particle size of less than 0.1 μm, and which are obtained by ball-milling crude copper phthalocyanines while suspending the milled material in an organic or aqueous organic phase, the improvement wherein the finely divided milled material is introduced into the organic or aqueous organic medium together with from 0.5 to 7 percent by weight, based on the crude copper phthalocyanine, of one or more basic copper phthalocyanines of the formula ##STR22## where CuPc is an n-valent copper phthalocyanine radical, R 1 is hydrogen or alkyl of 1 to 4 carbon atoms, A is saturated, linear or branched alkylene of 2 to 6 carbon atoms, the N atoms being on different carbon atoms, R 2 is alkyl of 1 to 20 carbon atoms or alkoxyalkyl of 3 to 12 carbon atoms or cycloalkyl of 6 to 8 carbon atoms, R 3 is hydrogen, alkyl of 1 to 4 carbon atoms or cycloalkyl of 6 to 8 carbon atoms, or the group ##STR23## is a saturated heterocyclic 5-membered, 6-membered or 7-membered ring which may in addition contain an oxygen atom, sulfur atom or a further nitrogen atom as a ring member, or ##STR24## denotes ##STR25## and n is a number from 1 to 6, and the mixture is kept at from room temperature to 180° C for recrystallization, after which the pigment is isolated.
Claim 2
Dependent Claim
251 words
In a process for converting crude copper phthalocyanines to a pigmentary form by treating finely divided and heavily agglomerated copper phthalocyanines which exhibit disturbed crystallization and have a primary particle size of less than 0.1 μm, and which are obtained by ball-milling crude copper phthalocyanines while suspending the milled material in an organic or aqueous organic phase, the improvement wherein the finely divided milled material is introduced into the organic or aqueous organic medium together with from 0.5 to 7 percent by weight, based on the crude copper phthalocyanine, of one or more basic copper phthalocyanines of the formula ##STR22## where CuPc is an n-valent copper phthalocyanine radical, R 1 is hydrogen or alkyl of 1 to 4 carbon atoms, A is saturated, linear or branched alkylene of 2 to 6 carbon atoms, the N atoms being on different carbon atoms, R 2 is alkyl of 1 to 20 carbon atoms or alkoxyalkyl of 3 to 12 carbon atoms or cycloalkyl of 6 to 8 carbon atoms, R 3 is hydrogen, alkyl of 1 to 4 carbon atoms or cycloalkyl of 6 to 8 carbon atoms, or the group ##STR23## is a saturated heterocyclic 5-membered, 6-membered or 7-membered ring which may in addition contain an oxygen atom, sulfur atom or a further nitrogen atom as a ring member, or ##STR24## denotes ##STR25## and n is a number from 1 to 6, and the mixture is kept at from room temperature to 180° C for recrystallization, after which the pigment is isolated.
Claim 3
Dependent Claim
25 words
A process as claimed in claim 1, wherein from 1 to 5% by weight, based on the copper phthalocyanine, of basic copper phthalocyanine is used.
Claim 4
Dependent Claim
22 words
A process as claimed in claim 1, wherein compounds of the formulae ##STR26## or mixtures thereof are used as basic copper phthalocyanines.
Claim 5
Dependent Claim
68 words
A process as claimed in claim 1, wherein aliphatic ketones of 3 to 10 carbon atoms, saturated cyclic ethers of 4 to 6 carbon atoms, aliphatic alcohols of 1 to 8 carbon atoms, benzenehydrocarbons, saturated cycloaliphatic hydrocarbons of 6 to 8 carbon atoms or aliphatic chlorohydrocarbons of 1 to 4 carbon atoms are used as the organic medium or as the organic constituent of the aqueous organic medium.
Claim 6
Dependent Claim
68 words
A process as claimed in claim 2, wherein aliphatic ketones of 3 to 10 carbon atoms, saturated cyclic ethers of 4 to 6 carbon atoms, aliphatic alcohols of 1 to 8 carbon atoms, benzenehydrocarbons, saturated cycloaliphatic hydrocarbons of 6 to 8 carbon atoms or aliphatic chlorohydrocarbons of 1 to 4 carbon atoms are used as the organic medium or as the organic constituent of the aqueous organic medium.
Claim 7
Dependent Claim
90 words
A process as claimed in claim 2, wherein acetone, methyl ethyl ketone, diethyl ketone, methyl propyl ketone, methyl isopropyl ketone, methyl butyl ketone, methyl isobutyl ketone, tetrahydrofuran, dioxane, tetrahydropyran, methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, sec.-butanol, amyl alcohol, isoamyl alcohol, n-hexanol, isohexanol, heptanol, isoheptanol, octanol, isooctanol, 2-ethylhexanol, benzene, toluene, xylene, mesitylene, ethylbenzene, cyclohexane, methylcyclohexane, dimethylcyclohexane, methylcyclopentane, chloroform, methylene chloride, carbon tetrachloride, 1,2-dichloroethane, trichloroethane, tetrachloroethane, trichloroethylene, propyl chloride, butyl chloride, dichloropropane, dichlorobutane or mixtures thereof are used as the organic medium or as the organic constituent of the aqueous organic medium.
Claim 8
Dependent Claim
49 words
A process as claimed in claim 2, wherein methyl ethyl ketone, diethyl ketone, tetrahydrofuran, dioxane, isobutanol, benzene, toluene, xylene, cyclohexane, methylcyclohexane, methylene chloride, chloroform, carbon tetrachloride, 1,2-dichloroethane, dichloropropane, trichloroethylene, tetrachloroethane or mixtures thereof are used as the organic medium or as the organic constituent of the aqueous organic medium.
Claim 9
Dependent Claim
18 words
A process as claimed in claim 2, wherein the mixture is kept at from 20° to 130° C.
Claim 10
Dependent Claim
31 words
A process as claimed in claim 1, wherein the amount of organic or aqueous organic medium used is from 2 to 20 times the amount by weight of the crude pigment.
Claim 11
Dependent Claim
26 words
A process as claimed in claim 1, wherein the ratio of water to the organic constituent in the aqueous organic medium is from 1:100 to 6:1.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1981-07-31 | 1982-01-30 | 1982-08-01 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1985-07-31 | 1986-01-30 | 1986-08-01 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1989-07-31 | 1990-01-30 | 1990-08-01 | $7700.00 | Window Closed / Lapsed |