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Preparation process of epsilon-crystal form copper phthalocyanine

A preparation process and technology of copper phthalocyanine, applied in the field of preparation of new crystal forms of organic pigments, can solve problems such as the inability to prepare stable

Inactive Publication Date: 2010-09-01
美利达颜料工业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, according to the description of the patent application, it is not possible to prepare a stable phthalocyanine blue 15:6 pigment

Method used

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  • Preparation process of epsilon-crystal form copper phthalocyanine
  • Preparation process of epsilon-crystal form copper phthalocyanine
  • Preparation process of epsilon-crystal form copper phthalocyanine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 1,500 kg of alkylbenzene solvent (Japanese AS-P2) into the enamel kettle, then add 500 kg of phthalic anhydride, 300 kg of chlorinated phthalic acid (anhydride), 1,600 kg of urea, and 210 kg of cuprous chloride kg, 16 kg of ammonium molybdate, the temperature is raised to 220°C, and the pressure in the enamel kettle is controlled at 3.5 kg / cm 2 , under the condition of 220±5° C., heat preservation for 5 hours to obtain 850 kg of low-chlorinated copper phthalocyanine crude product (85%).

[0039] Add 870 liters of sulfuric acid with a concentration of 50% into the second enamel kettle, cool to 30° C., then drop into 200 kilograms of the low-chlorinated copper phthalocyanine crude product (85%) obtained above, start stirring and dissolve in acid for 6 hours, put Put it into the dilution tank, heat up to 100°C, keep it warm for 8 hours, filter, wash with water and spray dry at a temperature of 70°C to obtain 165 kg of an intermediate product with a purity of 98%.

[0...

Embodiment 2

[0042] Add 1,500 kg of alkylbenzene solvent (Japanese AS-P2) into the enamel kettle, then add 800 kg of phthalic anhydride, 200 kg of chlorinated phthalic acid (anhydride), 2,000 kg of urea, and 250 kg of cuprous chloride kg, 15 kg of molybdic acid, the temperature is raised to 210°C, and the pressure in the enamel kettle is controlled at 3.5 kg / cm 2 , under the condition of 210±5° C., heat preservation for 8 hours to obtain 1082 kg of low-chlorinated copper phthalocyanine crude product (85%).

[0043] Add 850 liters of sulfuric acid with a concentration of 60% into the second enamel kettle, cool to 30° C., then drop into 200 kilograms of the low-chlorinated copper phthalocyanine crude product (85%) obtained above, start stirring and dissolve in acid for 7 hours, put Put it into the dilution tank, heat up to 100°C, keep it warm for 7 hours, filter, wash with water and spray dry at a temperature of 85°C to obtain 160 kg of an intermediate product with a purity of 99%.

[0044]...

Embodiment 3

[0046] Add 1,500 kg of alkylbenzene solvent (Japanese AS-P2) into the enamel kettle, then add 700 kg of phthalic anhydride, 400 kg of chlorinated phthalic acid (anhydride), 1,800 kg of urea, and 230 kg of cuprous chloride kg, 18 kg of ammonium molybdate, the temperature is raised to 210°C, and the pressure in the enamel kettle is controlled at 3.5 kg / cm 2 , under the condition of 210±5° C., heat preservation for 7 hours to obtain 1200 kilograms of monochloro-low-copper phthalocyanine crude product (85%).

[0047] Add 820 liters of sulfuric acid with a concentration of 70% into the second enamel kettle, cool to 30° C., then drop into 200 kilograms of the low-chlorinated copper phthalocyanine crude product (85%) obtained above, start stirring and dissolve in acid for 5 hours, put Put it into the dilution tank, heat up to 100°C, keep it warm for 7.5 hours, filter, wash with water, and spray dry at a temperature of 75°C to obtain 170 kg of an intermediate product with a purity of ...

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Abstract

The invention belongs to the technical field of copper phthalocyanine, and discloses a preparation process of epsilon-crystal form copper phthalocyanine which is also called C.I. pigment blue 15:6.The invention has a main technical scheme comprising the following steps: adopting phthalic anhydride, chlorophthalic anhydride, carbamide and copper chloride to synthesize monochloro copper phthalocyanine in the presence of a specific catalyst; carrying out acid treatment on the monochloro copper phthalocyanine to prepare an alpha-crystal form copper phthalocyanine intermediate product; and adding copper phthalocyanine derivates and a small amount of the epsilon-crystal form copper phthalocyanine of a known crystal form as seed crystals, and kneading with a high shear force in an organic solvent DEG to prepare the epsilon-crystal form copper phthalocyanine (C.I. pigment blue 15:6) which has fine heat resistance and weather resistance and pure and bright strong royal blue tone.

Description

technical field [0001] The invention relates to a preparation technology of a new crystal form of an organic pigment, especially a preparation technology of ε-crystal form copper phthalocyanine (or C.I. pigment blue 15:6). Background technique [0002] Copper phthalocyanine pigments are known to have more than five crystal forms, which are called α-crystal form, β-crystal form, γ-crystal form, δ-crystal form and ε-crystal form copper phthalocyanine, and are called R-crystal form in patents. Type copper phthalocyanine is essentially equivalent to the ε-crystal form. Various crystal forms of copper phthalocyanine pigments show different physical properties and color properties, such as: α-crystal form copper phthalocyanine gives a reddish blue tone in the binder, including unstable α-crystal form (C.I. Pigment Blue 15) With stable α-crystal form (C.I. Pigment Blue 15:1); β-crystal form copper phthalocyanine gives green light blue tone, including anti-crystallization β-crystal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B47/06C09B67/50
Inventor 李庆豹
Owner 美利达颜料工业有限公司