Industrial production and detection method of excellent migration-resistant heat-resistant pigment red PR-48: 2

Abstract

The invention discloses an industrial production and detection method of excellent migration-resistant heat-resistant pigment red PR-48: 2 and belongs to the technical field of pigment synthesis and detection. The method comprises carrying out an acidification reaction process on sodium 2-amino-4-chloro-5-methylbenzenesulfonate to obtain a suspending liquid, adding a sodium nitrite aqueous solution into the suspending liquid, carrying out diazotization to obtain a diazotized solution, carrying out coupling on the diazotized solution and 3-hydroxy-2-naphthoic acid in the presence of a dispersant to obtain a product, carrying out lake treatment on the product to obtain pigment red, drying and crushing the pigment red to obtain toner particles, mixing the toner particles, PU resin and a solvent DMF according to a certain ratio, carrying out high-rate beating homogenization, coating a release paper with the slurry through a scraper, carrying out high temperature baking, tearing the coating to obtain a coloured release paper and comparing a migration degree through a color measurement instrument. The method has mild reaction conditions, low equipment requirements and short reaction time, is convenient for operation and utilizes a common dispersant. The product paratonere has good performances and migration resistance of 5 level and resists a temperature of 210-220 DEG C.

Description

technical field

[0001] The invention belongs to the technical field of fine chemical synthesis and detection, and in particular relates to a method of using sodium 2-amino-4-chloro-5-methylbenzenesulfonate as a raw material, dissolving acid at high temperature to form a salt, and undergoing acid and low temperature treatment under acidic and low temperature conditions. The diazotization reaction is carried out with 2-hydroxy-3-naphthoic acid to carry out the reaction of coating while coupling, and then adjust the crystal form in the post-treatment reaction stage, and synthesize Pigment Red PR-48:2 with excellent migration resistance and heat resistance. At the same time, the accompanying migration detection method and migration level judgment comparison table are formulated to accurately connect the application of downstream industry customers. Background technique

[0002] Migration of pigments: Pigments are mainly penetrated by plasticizers (dioctyl phthalate), polar solve...

Examples

Embodiment 1

[0034] 1) 175kg 2-amino-4-chloro-5-methylbenzene sodium sulfonate, 215kg / 30% concentrated hydrochloric acid stirring solution, add 250kg 30% sodium nitrite aqueous solution at 5℃~10℃ to carry out diazotization reaction, Stir for 1 hour to get the diazo liquid for use;

[0035]2) Add 1300kg of water, 250kg of liquid caustic soda and 140kg of 2,3 acid to the reaction kettle, stir at a temperature of 40 to 50°C to obtain a clear liquid, and add 100kg of water to the rosin liquid (30kg rosin + 15kg / 30% liquid caustic soda + 300kg) under stirring. water);

[0036] 3) Inject the diazo liquid into the reaction kettle at 10°C to 20°C for coupling reaction, and stir for 2 hours after adding the diazo liquid; after warming up to 35-45°C, adjust the pH of the system to 8-8.5 and stir for 30 minutes , then add the inorganic calcium compound, heat up to 80 ~ 85 ℃ for 30 minutes, then drop to room temperature for filtration, and dry the filter cake at 85 ~ 95 ℃ to obtain red pigment 48:2 Y...

Embodiment 2

[0039] 1) 175kg 2-amino-4-chloro-5-methylbenzene sodium sulfonate, 215kg / 30% concentrated hydrochloric acid stirring solution, add 250kg 30% sodium nitrite aqueous solution at 5℃~10℃ to carry out diazotization reaction, Stir for 1 hour to get the diazo liquid for use;

[0040] 2) Add 1300kg of water, 250kg of liquid caustic soda and 140kg of 2,3 acid to the reaction kettle, stir at a temperature of 40 to 50°C to obtain a clear liquid, and add 100kg of water under stirring and add S-rosin liquid (30kg S-rosin + 15kg / 30% liquid) alkali+300kg water);

[0041] 3) Inject the diazo liquid into the reaction kettle at 10°C to 20°C for coupling reaction, and stir for 2 hours after adding the diazo liquid; after warming up to 35-45°C, adjust the pH of the system to 8-8.5 and stir for 30 minutes , then add the inorganic calcium compound, heat up to 80 ~ 85 ℃ for 30 minutes, then drop to room temperature for filtration, and dry the filter cake at 85 ~ 95 ℃ to obtain red pigment 48:2 Yiel...

Embodiment 3

[0044] 1) 175kg 2-amino-4-chloro-5-methylbenzene sodium sulfonate, 215kg / 30% concentrated hydrochloric acid stirring solution, add 250kg 30% sodium nitrite aqueous solution at 5℃~10℃ to carry out diazotization reaction, Stir for 1 hour to get the diazo liquid for use;

[0045] 2) Add 1300kg of water, 250kg of liquid caustic soda and 140kg of 2,3 acid to the reaction kettle, stir at a temperature of 40 to 50°C to obtain a clear liquid, and add 100kg of water under stirring and add S-rosin liquid (30kg S-rosin + 15kg / 30% liquid) alkali+300kg water);

[0046] 3) Inject the diazo liquid into the reaction kettle at 10°C to 20°C for coupling reaction, and stir for 2 hours after adding the diazo liquid; after warming up to 35-45°C, adjust the pH of the system to 8-8.5 and stir for 30 minutes , then add the inorganic calcium compound, heat up to 80 ~ 85 ℃ for 30 minutes, then drop to room temperature for filtration, and dry the filter cake at 85 ~ 95 ℃ to obtain red pigment 48:2 Yiel...

technical field

[0001] The invention belongs to the technical field of fine chemical synthesis and detection, and in particular relates to a method of using sodium 2-amino-4-chloro-5-methylbenzenesulfonate as a raw material, dissolving acid at high temperature to form a salt, and undergoing acid and low temperature treatment under acidic and low temperature conditions. The diazotization reaction is carried out with 2-hydroxy-3-naphthoic acid to carry out the reaction of coating while coupling, and then adjust the crystal form in the post-treatment reaction stage, and synthesize Pigment Red PR-48:2 with excellent migration resistance and heat resistance. At the same time, the accompanying migration detection method and migration level judgment comparison table are formulated to accurately connect the application of downstream industry customers. Background technique

[0002] Migration of pigments: Pigments are mainly penetrated by plasticizers (dioctyl phthalate), polar solve...

Examples

Embodiment 1

[0034] 1) 175kg 2-amino-4-chloro-5-methylbenzene sodium sulfonate, 215kg / 30% concentrated hydrochloric acid stirring solution, add 250kg 30% sodium nitrite aqueous solution at 5℃~10℃ to carry out diazotization reaction, Stir for 1 hour to get the diazo liquid for use;

[0035]2) Add 1300kg of water, 250kg of liquid caustic soda and 140kg of 2,3 acid to the reaction kettle, stir at a temperature of 40 to 50°C to obtain a clear liquid, and add 100kg of water to the rosin liquid (30kg rosin + 15kg / 30% liquid caustic soda + 300kg) under stirring. water);

[0036] 3) Inject the diazo liquid into the reaction kettle at 10°C to 20°C for coupling reaction, and stir for 2 hours after adding the diazo liquid; after warming up to 35-45°C, adjust the pH of the system to 8-8.5 and stir for 30 minutes , then add the inorganic calcium compound, heat up to 80 ~ 85 ℃ for 30 minutes, then drop to room temperature for filtration, and dry the filter cake at 85 ~ 95 ℃ to obtain red pigment 48:2 Y...

Embodiment 2

[0039] 1) 175kg 2-amino-4-chloro-5-methylbenzene sodium sulfonate, 215kg / 30% concentrated hydrochloric acid stirring solution, add 250kg 30% sodium nitrite aqueous solution at 5℃~10℃ to carry out diazotization reaction, Stir for 1 hour to get the diazo liquid for use;

[0040] 2) Add 1300kg of water, 250kg of liquid caustic soda and 140kg of 2,3 acid to the reaction kettle, stir at a temperature of 40 to 50°C to obtain a clear liquid, and add 100kg of water under stirring and add S-rosin liquid (30kg S-rosin + 15kg / 30% liquid) alkali+300kg water);

[0041] 3) Inject the diazo liquid into the reaction kettle at 10°C to 20°C for coupling reaction, and stir for 2 hours after adding the diazo liquid; after warming up to 35-45°C, adjust the pH of the system to 8-8.5 and stir for 30 minutes , then add the inorganic calcium compound, heat up to 80 ~ 85 ℃ for 30 minutes, then drop to room temperature for filtration, and dry the filter cake at 85 ~ 95 ℃ to obtain red pigment 48:2 Yiel...

Embodiment 3

[0044] 1) 175kg 2-amino-4-chloro-5-methylbenzene sodium sulfonate, 215kg / 30% concentrated hydrochloric acid stirring solution, add 250kg 30% sodium nitrite aqueous solution at 5℃~10℃ to carry out diazotization reaction, Stir for 1 hour to get the diazo liquid for use;

[0045] 2) Add 1300kg of water, 250kg of liquid caustic soda and 140kg of 2,3 acid to the reaction kettle, stir at a temperature of 40 to 50°C to obtain a clear liquid, and add 100kg of water under stirring and add S-rosin liquid (30kg S-rosin + 15kg / 30% liquid) alkali+300kg water);

[0046] 3) Inject the diazo liquid into the reaction kettle at 10°C to 20°C for coupling reaction, and stir for 2 hours after adding the diazo liquid; after warming up to 35-45°C, adjust the pH of the system to 8-8.5 and stir for 30 minutes , then add the inorganic calcium compound, heat up to 80 ~ 85 ℃ for 30 minutes, then drop to room temperature for filtration, and dry the filter cake at 85 ~ 95 ℃ to obtain red pigment 48:2 Yiel...

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