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Method for synthesizing phthalocyanine blue dye

A synthesis method and phthalocyanine blue technology, applied in the field of phthalocyanine blue dye synthesis, can solve the problems of increased energy consumption, high ammonia nitrogen waste water, complex synthesis process flow, etc., and achieve low consumption of raw materials, good product quality and simple process. Effect

Active Publication Date: 2020-08-18
ZHEJIANG RUIHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional synthesis process of phthalocyanine blue IBN is relatively complicated, and mainly has the following disadvantages: (1) The cobalt chloride used in the synthesis process of cobalt phthalocyanine is generally anhydrous cobalt chloride, and most of the supplies on the market are chlorine hexahydrate Cobalt chloride, cobalt chloride hexahydrate obtained from outsourcing needs to be dried in an oven to remove crystal water to obtain anhydrous cobalt chloride
However, cobalt phthalocyanine consumes a large amount of materials in these processes, which not only increases energy consumption, but also produces a large amount of high-COD, high-ammonia-nitrogen wastewater and a large amount of ammonia-containing waste gas
(3) In the reaction stage of dichlorocobalt phthalocyanine and N,N-dimethyl-1,3-propanediamine, a heating and cooling process is required, which increases the reaction energy consumption and the complexity of operation, and is also easy to increase Escape of the reaction solvent
[0004] At present, the requirements for environmental protection are getting higher and higher, and the production of highly polluting dyes is becoming more and more difficult to carry out

Method used

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  • Method for synthesizing phthalocyanine blue dye
  • Method for synthesizing phthalocyanine blue dye
  • Method for synthesizing phthalocyanine blue dye

Examples

Experimental program
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Effect test

Embodiment

[0033] at 10m 3 Put 4000 kg of mixed dichlorotoluene (content ≥ 99.5%) into the cobalt phthalocyanine glass-lined reactor, start stirring, and put in 240 kg of weighed ammonium chloride (content ≥ 99.0%), cobalt chloride hexahydrate ( Content ≥ 24.0% (calculated as cobalt)) 335 kg, ammonium molybdate (content ≥ 99.0%) 19.5 kg, then heat up to about 160°C to remove the moisture in the raw materials. After the dehydration is basically complete, the temperature is naturally lowered to below 130°C, 840 kg of phthalic anhydride (content ≥ 99.0%) is fed from the feeding port of the reaction pot, and 1440 kg of urea (total nitrogen content ≥ 46.6%) is added after the temperature is lower than 110°C . After the temperature rises, the temperature is maintained at 192° C. to 197° C. and the reaction is kept for about 12 hours to complete the reaction. Then put the material into a rake dryer for vacuum rake dry distillation to recover mixed dichlorotoluene, and the rake dry temperature...

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Abstract

The invention discloses a method for synthesizing a phthalocyanine blue dye represented by a formula (1). The method comprises the following steps: (a) mixing ammonium chloride, cobalt chloride, a catalyst and a reaction solvent dichlorotoluene, heating and dehydrating; (b) cooling the mixture obtained in the step (a), then adding phthalic anhydride and urea, dehydrating, and then heating for reaction; (c) distilling the mixture obtained in the step (b), and recovering dichlorotoluene to obtain a crude product cobalt dichloride phthalocyanine; and (d) carrying out a reaction on the crude product cobalt dichloride phthalocyanine obtained in the step (c) with N,N-dimethyl-1,3-propane diamine, and then carrying out filter pressing, water washing and drying, so as to obtain the cobalt dichloride phthalocyanine. The synthesis method has the characteristics of simple production process, low three-waste yield, high product yield and good quality, and has good economic and social benefits.

Description

technical field [0001] The invention belongs to the technical field of fine chemical production, and in particular relates to a synthesis method of phthalocyanine blue dye. Background technique [0002] Phthalocyanine blue IBN is an important phthalocyanine dye with bright color, excellent chlorine fastness, light fastness and washing fastness. In printing and dyeing, it is mainly used in dyeing or printing in the production of imitation wax and real batik. It has a special color, which is bright blue with red light. [0003] The traditional synthesis process of phthalocyanine blue IBN is relatively complicated, and mainly has the following disadvantages: (1) The cobalt chloride used in the cobalt phthalocyanine synthesis process is generally anhydrous cobalt chloride, and most of the supplies on the market are chlorine hexahydrate Cobalt chloride, the cobalt chloride hexahydrate obtained from outsourcing needs to be dried in an oven to remove crystal water to obtain anhydr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B47/06C09B47/08
CPCC09B47/06C09B47/08Y02P20/10
Inventor 柳长江方岩波杨逢午连张杰
Owner ZHEJIANG RUIHUA CHEM
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