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Fine clean production process of phthalocyanine green pigment

A clean production, phthalocyanine green technology, applied in azo dyes, organic dyes, organic chemistry and other directions, can solve the problems of affecting the catalytic effect, high corrosion, poor application performance, etc., to improve the utilization rate of chlorine gas, and the steps are closely combined. , the effect of increasing the reaction pressure

Active Publication Date: 2015-07-29
双乐颜料泰兴市有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that it is highly corrosive, AlCl3 can hardly be recovered, the three wastes are serious, and during the chlorination process, the copper atoms in copper phthalocyanine are often replaced by aluminum, which darkens the color of the product and affects the quality; secondly The main catalyst sulfur in the original process is solid, which dissolves slowly in the reaction, which affects the catalytic effect, and the two kinds of iron trichloride and antimony trichloride commonly used in the production process of phthalocyanine green are not difficult to dissolve and low In addition, according to the general production method, phthalocyanine green is directly used for sale after drying. At this time, the strength of the pigment is low, the color is dark, the application performance is poor, and the coloring power of the pigment , vividness, dispersibility, transparency and other properties are not maximized, resulting in serious problems such as pigment agglomeration during use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment one A kind of refinement clean production process of phthalocyanine green pigment, comprises the following steps:

[0027] (1) Preparation of phthalonitrile: phthalimide reacts with ammonia to obtain phthalic acid amide, and then dehydrates to obtain phthalonitrile, and then recrystallizes 3-5 times with ethanol for later use. ;

[0028] (2) Preparation of copper source: using CuCl: CuCl 2 The copper source is obtained by crushing, grinding, filtering and mixing thoroughly in a ratio of 1:1, and it is treated with hydrochloric acid-acetone solution before use, using CuCl and CuCl 2 The two copper sources contain the same chemical elements, which can reduce the pollution caused by too many types of elements in the later production process and the difficult problem of treatment;

[0029] (3) Selection of solvent: select nitrobenzene as reaction solvent;

[0030] (4) Obtaining copper phthalocyanine: Add 30kg of phthalonitrile prepared in step (1), 10kg of co...

Embodiment 2

[0036] Embodiment two : Different from Example 1 is the acquisition of phthalonitrile (4) copper phthalocyanine in step (4): add phthalonitrile 40kg prepared in step (1) in the reaction kettle, in step (2) The prepared copper source is 13kg, ethylene glycol is 95L, and the Cl 2 The volume is controlled at 0.7L / min by a gas flow meter, and 35g of molybdic anhydride is added;

[0037] (5) Preparation of crude phthalocyanine green product: Next, the temperature in the reactor was lowered to 120°C at a rate of 2°C per minute, and 5.5L of three catalysts, chlorosulfonic acid, 2.5L of liquid sulfur chloride and 2.5 iodine were added to the reactor L, will enter Cl from the upper and lower ends of the reactor 2 The volume was adjusted to 2.8 L / min, and then the Cl was again passed through the gas flow meter 2 The volume was adjusted to 4.2 L / min.

[0038] The weight of the phthalocyanine green finally obtained by embodiment two is 43.5kg.

Embodiment 3

[0039] Embodiment three: The difference from Example 1 is the acquisition of phthalonitrile (4) copper phthalocyanine in step (4): 50 kg of phthalonitrile prepared in step (1) was added to the reaction kettle, and phthalonitrile prepared in step (2) The obtained copper source is 16kg, ethylene glycol is 100L, and the Cl 2 The amount is controlled at 0.8 / min by a gas flow meter, and 40g molybdic anhydride is added;

[0040] (5) Preparation of crude phthalocyanine green product: Next, the temperature in the reactor was lowered to 120°C at a rate of 2°C per minute, and three catalysts, 6L of chlorosulfonic acid, 3L of liquid sulfur chloride and 3L of iodine were added to the reactor, and the Enter Cl from the upper and lower ends of the reactor 2 The amount is adjusted to 3.2 L / min, and then the Cl is again passed through the gas flow meter 2 The volume was adjusted to 4.5 L / min.

[0041] The weight of the phthalocyanine green finally obtained by embodiment three is 54.5kg. ...

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Abstract

The invention discloses a fine clean production process of a phthalocyanine green pigment. The fine clean production process comprises the following steps: (1) phthalonitrile preparation; (2) copper source preparation; (3) solvent selection; (4) copper phthalocyanine obtaining; (5) phthalocyanine green crude product preparation; (6) phthalocyanine green refining; (7) finished phthalocyanine green preparation; (8) finished phthalocyanine green crystal form change. The phthalocyanine green pigment produced by the production process is clean, environment-friendly and less in side reaction; the coloring power, the brightness, the dispersibility, the transparence and other properties are finally improved; the production process is strong in operability, close in step combination and short in process time.

Description

technical field [0001] The invention relates to the technical field of chemical pigment production, in particular to a refined and clean production process of phthalocyanine green pigment. Background technique [0002] Phthalocyanine pigments are known as the leader of organic pigments for their excellent light fastness, heat resistance, acid and alkali resistance and bright color. Phthalocyanine green is a large category of this series of pigments, and it is the best green pigment. It is the product of chlorination or chlorination of phthalocyanine blue (ie, copper phthalocyanine) and mixed halogenation. Depending on the number of halogen atoms substituted on the benzene ring, the color is different. Usually chlorinated products 1 2 to 16 chlorine atom substitutions are bright green. The synthesis of phthalocyanine green is divided into two categories in terms of technological process: direct halogenation and direct condensation. In terms of raw materials, it is divided i...

Claims

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Application Information

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IPC IPC(8): C09B47/10C07D487/22
Inventor 杨汉洲朱骥
Owner 双乐颜料泰兴市有限公司
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