Copper phthalocyanine liquid solid phase mixed type continuous reactor and its process

Abstract

The invention discloses a special device continuously preparing copper phthalocyanine liquid-solid mixing continuous reactor. The benzoic anhydride, urea, copper chloride and a little catalyst are input by automatic feeder according to set parameter, and said reactor prepares copper phthalocyanine continuously. It is characterized in that: the reaction of liquid and solid and reaction of liquid phase employ urea as solvent, the product is 1- iminoisoindoline and 1, 3- diiminoisoindoline; copper phthalocyanine is prepared in solid-phase reactor with product got in liquid-reactor; the solid-phase reactor employs rake stirrer to solve problem of large viscosity of material, the control of discharging amount of liquid material in liquid-phase reactor applies communication pipe principle, which makes use of potential difference between charging and discharging to control feeding speed and solves problem of hard mechanical conveying for high-temperature viscous material.

Description

Technical field [0001] The present invention relates to the production equipment and the production process of fine chemical organic pigments, in particular to the production equipment and the production process of phthalocyanine pigments. Background technique [0002] At present, the known copper phthalocyanine synthesis technology mainly includes phthalic anhydride, urea process and phthalonitrile process. Method: One is the liquid phase method, also known as the solvent method, and the other is the solid phase method; the main advantages of the liquid phase method in chemical production are fast heat transfer, mass transfer, and high reaction efficiency, so the purity of the product copper phthalocyanine can be Reach 97%-98.2%, product yield can reach 95.5% (references: Zhou Chunlong Mu Zhenyi edited Organic Pigment-Structure, Characteristic and Applied Chemical Industry Press January 2002 142-143), but due to liquid phase condensation After the reaction is completed, to...

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Problems solved by technology

[0002] At present, the known copper phthalocyanine synthesis technology mainly includes phthalic anhydride, urea process and phthalonitrile process. Method: One is the liquid phase method, also known as the solvent method, and the other is the solid phase method; the main advantages of the liquid phase method in chemical production are fast heat transfer, mass transfer, and high reaction efficiency, so the purity of the product copper phthalocyanine can be Reach 97%-98.2%, product yield can reach 95.5% (references: Zhou Chunlong Mu Zhenyi edited Organic Pigment-Structure, Characteristic and Applied Chemical Industry Press January 2002 142-143), but due to liquid phase condensation After the reaction is completed, to remove and recycle the solvent from the product, a large amount of equipment and energy consumption need to be invested, large investment, high energy consumption, and long process cycle are its main disadvantages; The heat transfer and mass transfer are not as fast as the heat transfer and mass transfer of the material in the liquid state, so the reaction efficiency is poor. At present, the latest technology and equipment for producing copper phthalocyanine by the solid phase method in China are vertical kettles equipped with strong stirrers. Reactor, this technique and equipment have strengthened the heat transfer and the mass transfer between the reaction materials by the strong stirrer, can make the reaction yield reach 85% (references: Shen Yongjia edited the synthesis and application of phthalocyanine Chemical Industry Press 2000 February 84-85), but in actual production, the general product purity is only 80%. The main reason is that the vertical reactor has a large diameter and poor heat transfer, so the material can only be divided into multiple times in small quantities. Add at high material temperature (180°C-190°C), otherwise, when the instantaneous temperature drops below 150°C, the entire material in the reactor will become a plastic solid material (very high viscosity) and the production equipment will not be able to The reaction material under this condition is basically a reaction in the solid state. When a small amount of material put in in batches enters a large amount of high-temperature solid powder or fine granular material, the current of the agitator motor will suddenly and sharply The increase and rapid drop can know that a small amount of material input in batches only has an instantaneous melting state in a large amount of solid powder or fine granular high-temperature material, and the rapid drop of current reflects that the material returns to solid powder or fine particle. Granular solid phase state, (confirmed by experiments), it can be considered that this reactor and the corresponding process make the material still react in the solid phase, and its mass transfer has not been improved, but due to the improved heat transfer Better improvement, the content of the product has increased by nearly 10 percentage points compared with the previous solid-phase reactor. Since the product content is only about 80%, the product needs to be boiled in acid before it can be pigmented, which increases energy consumption and waste water; the above reactors are all batch reactors; the special equipment for continuous production of copper phthalocyanine cannot be produced in China at present, and DRAIS Werke GmbH of Germany is the main manufacturer of this equipment. The purity of the copper phthalocyanine produced by this equipment produced by Laishi Co., Ltd. still can only reach 75%-80%, (refer to Literature review: Shen Yongjia edited the synthesis of phthalocyanine and applied Chemical Industry Press, February 85-86, 2000), there are still deficiencies in the purity and yield of the product;

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