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Process and apparatus for preparing metal or nonmetal phthalocyanine

A non-metal and metal technology, applied in the field of preparing metal or non-metal phthalocyanine, can solve problems such as difficult mass production of phthalocyanine, unsuitable for mass production and commercialization of phthalocyanine, unfavorable processing efficiency and environmental management

Inactive Publication Date: 2010-12-08
菲萨络斯有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has the following problems: i) impurities that are difficult to remove are formed at the high-temperature portion due to the temperature difference between the inside and outside of the reactants, and ii) since phthalocyanine particles are non-uniformly dispersed and aggregated into a needle shape, they are used as The pigment must be colored for a long time before, iii) the method requires a lot of energy to recover the solvent used for the reaction, and iv) the method is disadvantageous in terms of processing efficiency and environmental management
However, despite the use of microwaves, the yield of phthalocyanine was not significantly improved because the reactants were not uniformly mixed during the reaction, it was difficult to mass-produce phthalocyanine, and the quality of phthalocyanine could not be compared with that prepared by solvent method. Phthalocyanine compared
In summary, the preparation of phthalocyanines using microwaves is not suitable for mass production and commercialization

Method used

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  • Process and apparatus for preparing metal or nonmetal phthalocyanine
  • Process and apparatus for preparing metal or nonmetal phthalocyanine
  • Process and apparatus for preparing metal or nonmetal phthalocyanine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Preparation of Copper Phthalocyanine

[0041] This example was carried out in a solvent-based device according to the invention. Specifically, 42 g of anhydrous phthalic acid, 49 g of urea, 7 g of copper chloride, 0.1 g of ammonium molybdate, and 100 g of alkylbenzene were introduced into a pyrex glass container 9, followed by microwaves at 28 kHz and ultrasonic energy at 250 W The reactant was uniformly stirred for 3 hours at 180-185° C. to prepare copper phthalocyanine. During the reaction, the temperature of the reactants was precisely controlled within a deviation range of ±1° C. using the PID temperature controller 8, and thus a microwave power of 100-3,000 W was maintained. Microwave and ultrasonic energy are used simultaneously from the initial stages of the reaction. After completing the preparation, the solvent was removed by distillation under reduced pressure. Add dry copper phthalocyanine to 500ml of 5% sulfuric acid solution, treat with acid at 85°C for ...

Embodiment 2

[0043] Preparation of other phthalocyanines

[0044] Various phthalocyanines were prepared in the same manner as shown in Example 1, but using 1,2-dicyanobenzene instead of anhydrous phthalic acid, and using a compound selected from titanium, iron, cobalt, aluminum, manganese, tin and Metal salts of nickel were used in place of equivalent weight of copper chloride as the metal source (in the case of non-metallic phthalocyanines, no metal source was used).

Embodiment 3

[0046] Preparation of Copper Phthalocyanine

[0047] 300 ml of alumina microbeads with a diameter of 30 mm were charged into an attritor 12 equipped with a microwave generating device, and then 42 g of anhydrous phthalic acid, 49 g of urea, 7 g of cuprous chloride and 0.1 g of ammonium molybdate were added thereto. The reactant was heated to 120°C at a rate of 10°C / min, while being stirred at 300-400rpm by the stirrer 17, and further heated to the final preparation temperature (180°C) at a rate of 5°C / min. The final preparation temperature was maintained for 3 hours while uniformly stirring the mixture to prepare copper phthalocyanine. During the reaction process, the temperature of the reactants is precisely controlled within a deviation range of ±1°C using a PID temperature controller, and a microwave power of 100-4,000W is maintained. After finishing the preparation, the attritor was cooled to 60° C., and 500 ml of 5% sulfuric acid solution was added thereto. After stirri...

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Abstract

Disclosed herein is a process for preparing a metal or nonmetal phthalocyanine by using both microwave and ultrasonic wave energy in the presence of a solvent, or by using microwave energy in the absence of a solvent. Specifically, according to the process, anhydrous phthalic acid, phthalimide, 1,3-diiminoisoindoline, 1,2-dicyanobenzene, an halogen derivative thereof, an alkyl_ derivative thereofor an alkoxy derivative thereof is mixed with a metal chloride or an alkoxy metal at 130250< DEG >C for 0.2515 hours by using microwave at a frequency of 0.1-1000Hz and a power of 100-3,000W and ultrasonic wave at a frequency of 1-1,000GHz and a power of 100-5,000W in the presence of a solvent, or by using microwave at a frequency of 0.1-100GHz and a power of 100-4,000W in the absence of a solvent. Further disclosed is an apparatus for preparing a metal or nonmetal phthalocyanine in the absence or presence of solvent.

Description

technical field [0001] The present invention relates to methods and apparatus for the preparation of metallic or non-metallic phthalocyanines using microwave and ultrasonic energy in the absence or presence of solvents. Background technique [0002] Phthalocyanine is figure 1 The compound represented by the structural formula shown in and exhibits excellent stability and excellent photoelectric performance due to its unique chemical structure. For these reasons, phthalocyanines are currently widely used in fields such as dyes, pigments, chemical sensors, electrochromic displays, photovoltaic cells, radiators, photodisks, catalysts, nonlinear optics, and the like. [0003] Phthalocyanine usually utilizes urea or ammonia as a nitrogen source, in an inert solvent or without any solvent, in the presence of a catalyst, at a temperature of 180 ° C or higher, by making It is prepared by reacting the starting material of imide, 1,3-diiminoisoindoline, 1,2-dicyanobenzene and its de...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F1/08C07F17/00
CPCB01J19/10B01J23/28C07F1/08C09B47/04
Inventor 权宗皓郑基锡孙宇皓朴成洙
Owner 菲萨络斯有限公司
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