Method for manufacturing pigment red 3BL condensation intermediate

A production method and intermediate technology, applied in the preparation of sulfonate, organic chemistry, etc., can solve the problems of large energy consumption, environmental pollution, high processing cost, etc., and achieve faster reaction speed, good chemical stability, and no corrosion of equipment Effect

Active Publication Date: 2010-09-15
南通市埃唯卡新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the process of synthesizing Pigment Red 3BL, due to the use of a large amount of sulfuric acid, a large amount of acid-containing and dark-colored wastewater is discharged into the environm...

Method used

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  • Method for manufacturing pigment red 3BL condensation intermediate

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Effect test

Embodiment 1

[0017] A kind of production method of pigment red 3BL condensation intermediate, in the 500mL four-necked bottle that thermometer, agitator and reflux condenser are equipped with, add bromine 25g, copper powder 13g, diethylene glycol ethyl ether 350mL and laurylamine 1.5g , stirred and reacted at 68-72°C for 150 minutes, then filtered while it was hot, transferred the filtrate to a distillation flask to distill and recover diethylene glycol ethyl ether, after the distillation of diethylene glycol ethyl ether was completed, add 320ml of hot water and heat to boiling, then Add 50g of sodium chloride at 70-80°C for salting out and filter, wash the filter cake with 10% sodium chloride solution, and then dry it in a drying oven to obtain the pigment red 3BL condensation intermediate. The yield can reach 67.2%.

Embodiment 2

[0019] A kind of production method of pigment red 3BL condensation intermediate, in the 500mL four-neck bottle that is equipped with thermometer, agitator and reflux condenser tube, add 25g of bromine, 12.5g of copper powder, 380mL of N,N~dimethylformamide and octadecylamine 1.7g, stirred and reacted at 68-72°C for 150min, then filtered while hot, transferred the filtrate to a distillation flask to recover N,N-dimethylformamide, and waited for N,N-dimethylformamide After the distillation is completed, add 300ml of hot water and heat to boiling, add 50g of sodium chloride at 70-80°C for salting out and filter, wash the filter cake with 10% sodium chloride solution, and then place it in a drying oven to dry to obtain Pigment Red 3BL condensation intermediate. The yield can reach 73.2%.

Embodiment 3

[0021] A kind of production method of pigment red 3BL condensation intermediate, in the 500mL four-necked bottle that thermometer, stirrer and reflux condenser tube are housed, add bromine 25g, copper powder 13.2g, propylene glycol ether 380mL and stearylamine 1.7g, Stir and react at 68-72°C for 150 minutes, then filter while it is hot, transfer the filtrate to a distillation flask to recover propylene glycol ether, and after the distillation of propylene glycol ether is completed, add 350ml of hot water and heat to boiling, then add 50g at 70-80°C Sodium chloride was salted out and filtered, the filter cake was washed with 10% sodium chloride solution, and then dried in a drying oven to obtain the pigment red 3BL condensation intermediate. The yield can reach 73.2%.

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Abstract

The invention relates to a method for manufacturing a pigment red 3BL condensation intermediate, which is characterized by comprising the following steps of: adding 25 parts by weight of bromamine acid and 280 to 450 parts by weight of catalysts consisting of an organic solvent, a surface active agent and copper powder into to a 500-mL four-neck bottle provided with a thermometer, a stirrer and a reflux condensing tube; stirring the mixture for reacting for 150 min at 68-72 DEG C, filtering when the mixture is hot , moving the filtrate to a distilling bottle for distilling and recycling the organic solvent; after the organic solvent is distilled, adding 300 to 350 parts by weight of hot water, heating to boiling, adding 50 parts by weight of sodium chloride at 70 to 80 DEG C, salting out and filtering; washing a filter cake washed by 10% sodium chloride solution, and then, drying the washed filter cake in a drying box to obtain the pigment red 3BL condensation intermediate. The invention has the advantages of having high activity and good chemical stability, improving the reaction speed and productivity, having no corrosion to equipment and low cost, and realizing zero discharge of acid containing waste water.

Description

technical field [0001] The invention relates to a production method of a chemical pigment intermediate, in particular to a production method of a pigment red 3BL intermediate. Background technique [0002] Pigment Red 3BL is an organic pigment with excellent weather resistance, solvent resistance, chemical resistance, migration resistance, and plastic molding temperature resistance. It is the main red organic pigment variety for synthetic resin and plastic coloring. It has bright colors and various fastnesses. With excellent performance and other advantages, it is widely used in the coloring of inks, paints, cosmetics, printing and dyeing, paints, plastics, synthetic fibers, etc., and is considered by the market as one of the high-grade red organic pigments. However, during the condensation reaction during the synthesis of Pigment Red 3BL, there is the problem of inorganic acid sulfuric acid polluting the environment. [0003] Currently, synthetic Pigment Red 3BL reacts in ...

Claims

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Application Information

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IPC IPC(8): C07C309/53C07C303/32
Inventor 徐立群赵觉新
Owner 南通市埃唯卡新材料有限公司
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