Crystal modification of C.I. Pigment Red 53:2 (γ-phase)
AssigneeClariant GmbH
InventorsMartin Ulrich Schmidt, Hans Joachim Metz
Life of this patent
Estimating the term…
Abstract
The invention relates to a novel crystal modification (γ-modification ) of C.I. Pigment Red 53:2 of the formula (1) having the following characteristic reflections in the X-ray powder diffraction pattern: 2Θ d Relative intensity in % 4.4 20.2 49 5.8 15.4 100 8.8 10.0 23 10.3 8.6 25 10.9 8.1 33 12.2 7.3 15 13.9 6.4 16 15.4 5.8 15 16.7 5.3 28 17.6 5.0 16 18.4 4.8 18 18.6 4.8 18 19.7 4.5 20 20.8 4.3 18 23.2 3.8 48 24.0 3.7 21 24.8 3.6 37 25.2 3.5 34 26.6 3.3 19 27.3 3.3 19 27.9 3.2 12 29.3 3.0 14
Claims17
A C.I. Pigment Red 53:2 of the formula (I)
- in which M is a cation, with the proviso that at least 50% of the cations are calcium ions,
- in the γ-modification, which has the following characteristic reflections in the X-ray powder diffraction pattern, measured using Cu-Kα radiation:
- γ:
- 2Θ d Relative intensity in % 4.4 20.2 49 5.8 15.4 100 8.8 10.0 23 10.3 8.6 25 10.9 8.1 33 12.2 7.3 15 13.9 6.4 16 15.4 5.8 15 16.7 5.3 28 17.6 5.0 16 18.4 4.8 18 18.6 4.8 18 19.7 4.5 20 20.8 4.3 18 23.2 3.8 48 24.0 3.7 21 24.8 3.6 37 25.2 3.5 34 26.6 3.3 19 27.3 3.3 19 27.9 3.2 12 29.3 3.0 14
A process for the preparation of C.I. Pigment Red 53:2 of the formula (I)
- in which M is a cation, with the proviso that at least 50% of the cations are calcium ions,
- in the γ-modification, which has the following characteristic reflections in the X-ray powder diffraction pattern, measured using Cu-Kα radiation:
- γ:
- 2Θ d Relative intensity in % 4.4 20.2 49 5.8 15.4 100 8.8 10.0 23 10.3 8.6 25 10.9 8.1 33 12.2 7.3 15 13.9 6.4 16 15.4 5.8 15 16.7 5.3 28 17.6 5.0 16 18.4 4.8 18 18.6 4.8 18 19.7 4.5 20 20.8 4.3 18 23.2 3.8 48 24.0 3.7 21 24.8 3.6 37 25.2 3.5 34 26.6 3.3 19 27.3 3.3 19 27.9 3.2 12 29.3 3.0 14
- wherein β-naphthol is reacted with the diazonium salt of the formula (2)
- in which M1 is hydrogen or a cation equivalent and X is an anion;
- and with a calcium salt, in the presence of one or more solvents selected from the group consisting of N-methylpyrrolidone, isopropanol, isobutanol and amyl alcohol, or is heated in a mixture of one or more of said solvents with up to 99% by weight of water.
A process for the preparation of C.I. Pigment Red 53:2 of the formula (I)
- in which M is a cation, with the proviso that at least 50% of the cations are calcium ions,
- in the γ-modification, which has the following characteristic reflections in the X-ray powder diffraction pattern, measured using Cu-Kα radiation:
- γ:
- 2Θ d Relative intensity in % 4.4 20.2 49 5.8 15.4 100 8.8 10.0 23 10.3 8.6 25 10.9 8.1 33 12.2 7.3 15 13.9 6.4 16 15.4 5.8 15 16.7 5.3 28 17.6 5.0 16 18.4 4.8 18 18.6 4.8 18 19.7 4.5 20 20.8 4.3 18 23.2 3.8 48 24.0 3.7 21 24.8 3.6 37 25.2 3.5 34 26.6 3.3 19 27.3 3.3 19 27.9 3.2 12 29.3 3.0 14
- wherein C.I. Pigment Red 53:2 which is present wholly or partially in the α-modification is heated, together with one or more solvents selected from the group consisting of N-methylpyrrolidone, isopropanol, isobutanol and amyl alcohol, or is heated in a mixture of one or more of said solvents with up to 99% by weight of water, to a temperature of from 40 to 200° C., and then cooled to a temperature of from −20 to +90° C., optionally water, a second solvent having low dissolving power or a combination thereof are added and, optionally, an acid, an alkali or a salt is added.
A process for the preparation of C.I. Pigment Red 53:2 of the formula (I)
- in which M is a cation, with the proviso that at least 50% of the cations are calcium ions,
- in the γ-modification, which has the following characteristic reflections in the X-ray powder diffraction pattern, measured using Cu-Kα radiation:
- γ:
- 2Θ d Relative intensity in % 4.4 20.2 49 5.8 15.4 100 8.8 10.0 23 10.3 8.6 25 10.9 8.1 33 12.2 7.3 15 13.9 6.4 16 15.4 5.8 15 16.7 5.3 28 17.6 5.0 16 18.4 4.8 18 18.6 4.8 18 19.7 4.5 20 20.8 4.3 18 23.2 3.8 48 24.0 3.7 21 24.8 3.6 37 25.2 3.5 34 26.6 3.3 19 27.3 3.3 19 27.9 3.2 12 29.3 3.0 14
- wherein C.I. Pigment Red 53:2 which is present wholly or partly in the α-modification is kneaded or milled in the presence of one or more solvents N-methylpyrrolidone, isopropanol, isobutanol and amyl alcohol or in a mixture of one or more of said solvents with up to 99% by weight of water at a temperature of from 40 to 200° C.
A method of pigmenting coatings, plastics, printing inks, electrophotographic toners and developers, powder coatings, inkjet inks, aqueous pigment preparations and seeds comprising the step of adding C.I. Pigment Red 53:2 of the formula (I)
- in which M is a cation, with the proviso that at least 50% of the cations are calcium ions,
- in the γ-modification, which has the following characteristic reflections in the X-ray powder diffraction paftern, measured using Cu-Kα radiation:
- γ:
- 2Θ d Relative intensity in % 4.4 20.2 49 5.8 15.4 100 8.8 10.0 23 10.3 8.6 25 10.9 8.1 33 12.2 7.3 15 13.9 6.4 16 15.4 5.8 15 16.7 5.3 28 17.6 5.0 16 18.4 4.8 18 18.6 4.8 18 19.7 4.5 20 20.8 4.3 18 23.2 3.8 48 24.0 3.7 21 24.8 3.6 37 25.2 3.5 34 26.6 3.3 19 27.3 3.3 19 27.9 3.2 12 29.3 3.0 14
- into a coating, plastic, printing ink liquor, electrophotographic toner and developer, powder coating, inkjet ink liquor, aqueous preparation or seed.
Dependencies are inferred from the claim text.