Clean production method of high-purity copper phthalocyanine

A production method and technology of copper phthalocyanine, which is applied in the field of dye preparation, can solve the problems of copper phthalocyanine such as low purity, poor coloring effect, and poor color stability, and achieve bright color, excellent color stability, and coloring effect Good results

Inactive Publication Date: 2019-03-22
滨海康益医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purity of the copper phthalocyanine produced is not high, and the product is a mixed crystal form, the coloring effect is not good, and the color stability is not good

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Synthesis: Put 500g of toluene into the condensation tank, raise the temperature to 130°C, continue to add 220g of phthalic anhydride, keep stirring at 130°C until the phthalic anhydride is completely dissolved, then put in 220g of urea, 40g of cuprous chloride and 1g of catalyst ammonium molybdate , after the feeding is completed, seal and increase the pressure to 0.5Mpa, continue to react at 185°C for 7 hours, reduce the pressure to normal pressure, cool to normal temperature, and get 302g copper phthalocyanine crude product after discharging and drying; the tail gas produced in the condensation reaction is sequentially Use 25wt% dilute sulfuric acid and water to spray and absorb, and the obtained two absorption liquids are combined and separated by sedimentation to obtain the lower clear liquid M for use;

[0029] (2) Refining: Add 30g of copper phthalocyanine crude product obtained in step (1) to be beaten and mixed evenly with 450g of water, then emulsify throug...

Embodiment 2

[0033](1) Synthesis: Put 480g of o-xylene into the condensation tank, raise the temperature to 125°C, continue to add 250g of phthalic anhydride, keep stirring at 125°C until the phthalic anhydride is completely dissolved, then put in 250g of urea, 45g of cuprous chloride and 1g of catalyst molybdenum ammonium acid, after the feeding is completed, the pressure is sealed and raised to 0.45Mpa, and after the reaction is continued for 8 hours at 195°C, the pressure is reduced to normal pressure, the temperature is lowered to normal temperature, and 328g of copper phthalocyanine crude product is obtained after discharging and drying; The tail gas is absorbed by spraying with 25wt% dilute sulfuric acid and water in sequence, and the two absorption liquids obtained are combined and separated by sedimentation to obtain the lower clear liquid M for use;

[0034] (2) Refining: Add 540g of water to the crude product of 30g of copper phthalocyanine obtained in step (1) and mix evenly, the...

Embodiment 3

[0038] (1) Synthesis: Put 520g of m-xylene into the condensation tank, raise the temperature to 135°C, continue to add 200g of phthalic anhydride, keep stirring at 135°C until the phthalic anhydride is completely dissolved, then put in 200g of urea, 42g of cuprous chloride and 1g of catalyst molybdenum Ammonium acid ammonium, after feeding, sealed and boosted to 0.4Mpa, continued to react at 190°C for 6 hours, decompressed to normal pressure, cooled to normal temperature, and obtained 278g copper phthalocyanine crude product after discharging and drying; The tail gas is absorbed by spraying with 25wt% dilute sulfuric acid and water in sequence, and the two absorption liquids obtained are combined and separated by sedimentation to obtain the lower clear liquid M for use;

[0039] (2) Refining: Add 600g of water to the crude product of 30g of copper phthalocyanine obtained in step (1) and mix evenly, then emulsify through a colloid mill to make 630g of copper phthalocyanine slurr...

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Abstract

The invention provides a clean production method of high-purity copper phthalocyanine. The method comprises following steps: (1), synthesis: alkylbenzene is added to a condensation tank, phthalic anhydride is continuously added after the temperature is increased, urea, cuprous chloride and ammonium molybdate are added after phthalic anhydride is dissolved, the components are subjected to a reaction, and a crude copper phthalocyanine product is prepared; (2), refining: copper phthalocyanine slurry is prepared from the crude copper phthalocyanine product and added to a mixed solution N preparedfrom dilute sulfuric acid and a cosolvent, heating and stirring are performed until the crude copper phthalocyanine product is completely dissolved, then water is dropwise added until copper phthalocyanine crystals are not separated out, filtering is performed, a filter cake is subjected to ethanol washing, water washing, filtering and vacuum drying, and the high-purity copper phthalocyanine product is obtained; (2), waste liquor recovery: a large amount of filter liquor produced in a reaction process is adsorbed by ion exchange resin, neutralized, concentrated, evaporated and centrifuged, andan ammonium sulfate product is prepared. Copper phthalocyanine prepared with the method is high in purity and has single crystal form, good coloring effect and excellent color stability, meanwhile, tail gas and wastewater in the production are effectively treated, and economic benefits of energy conservation and emission reduction are obtained.

Description

technical field [0001] The invention belongs to the technical field of dye preparation, in particular to a production method of copper phthalocyanine, in particular to a clean production method of high-purity copper phthalocyanine. Background technique [0002] Copper phthalocyanine, molecular formula: C 32 h 16 CuN 8 , is a macrocyclic compound containing a special structure of porphyrazine. In 1907, copper phthalocyanine was accidentally discovered by German chemists A. Braun and J. Tchemiac in an experiment. Copper phthalocyanine has a bright blue color, high tinting strength, acid and alkali resistance, solvent resistance, and good light resistance and weather resistance. It is a kind of pigment with various excellent properties. Therefore, it occupies an Important position. Copper phthalocyanine is covalently bonded and has good stability. It can sublime in a vacuum at 400-500°C or in an inert gas without changing, and it will not demetallize even if it is in cont...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B47/06C07D487/22
Inventor 王庆刚
Owner 滨海康益医药化工有限公司
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