Preparation method for C.I. pigment red 53:1

A pigment red and amino technology, applied in the field of organic pigments, can solve the problems of reduced heat resistance, excessive heavy metals in products, adverse effects on the environment and human body, etc. Effect

Inactive Publication Date: 2012-07-18
宇虹颜料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the adverse effects on the environment and human body caused by the existing production process, the heavy metals in the product exceed the standard and the heat resistance is reduced, and at the same time meet the requirements for the shade, tinting strength and vividness of the pigment, the present invention provides a new preparation C. I. Pigment Red 53:1 Method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Preparation of diazo solution

[0025] Add 200g of water to a 500ml beaker, then add 23g of 30% hydrochloric acid, 32.5g of 2-amino-5-chloro-4-methylbenzenesulfonic acid, 0.6g of 2-amino-1-naphthalenesulfonic acid, add dodecyl Stir 0.4 g of sodium benzenesulfonate for 30 minutes, cool down to 5°C, then add 30% sodium nitrite (30% aqueous solution prepared with 10.5 g of sodium nitrite), the addition time is 10 minutes, and the diazotization reaction takes 90 minutes Finally, add sulfamic acid until the KI test paper is slightly blue to obtain a diazo solution.

[0026] (2) Preparation of coupling solution

[0027] Add 150 g of water, 10 g of sodium hydroxide, and 22 g of 2-naphthol into a 500 ml beaker, and stir for 30 minutes to cool down to 20° C. after completely dissolving.

[0028] (3) Coupling

[0029] Put the coupling solution into a 3000ml beaker, then add diazonium solution for coupling reaction. The time is 60 minutes, the temperature is lower than 30°...

Embodiment 2

[0043] The preparation of step (1) diazo solution and step (2) coupling solution is the same as in Example 1.

[0044] (3) Coupling

[0045] Put the coupling solution into a 3000ml beaker, then add diazonium solution for coupling reaction. The time is 60 minutes, the temperature is less than 30°C, the pH value is adjusted to 9.5 with diluted sodium hydroxide solution, stirred for 30 minutes, and the pH is adjusted to 7.5 with diluted hydrochloric acid solution, and stirred for 15 minutes.

[0046] (4) Lake reaction

[0047] Add 14.96 g of the laking agent barium chloride and 1.58 g of the second laking agent calcium chloride in 15 minutes, stir for 5 minutes, raise the temperature to 100° C., and keep the temperature for 60 minutes.

[0048] (5) Post-processing

[0049] Cool down and press filter, fully wash with pure water, dry at 80°C, and ultrafinely pulverize to obtain the finished product.

[0050] In this example, the molar ratio of barium chloride to 2-amino-5-chlor...

Embodiment 3

[0054] (1) Preparation of diazo solution

[0055] Add 200g of water into a 500ml beaker, then add 23g of 30% hydrochloric acid, 32.5g of 2-amino-5-chloro-4-methylbenzenesulfonic acid, 0.6g of 2-amino-1-naphthalenesulfonic acid, add fatty alcohol polyoxygen Stir 0.5 g of ethylene (20) ether for 30 minutes, cool down to 5°C, and then add 30% sodium nitrite (30% aqueous solution prepared with 10.5 g of sodium nitrite), the addition time is 20 minutes, and the diazotization reaction is 90 Minutes later, add sulfamic acid until the KI test paper is slightly blue to obtain a diazo solution.

[0056] (2) Preparation of coupling solution

[0057] Add 150 g of water, 10 g of sodium hydroxide, and 22 g of 2-naphthol into a 500 ml beaker, and stir for 30 minutes to cool down to 20° C. after completely dissolving.

[0058] (3) Coupling

[0059]Put the coupling solution into a 3000ml beaker, then add diazonium solution for coupling reaction. The time is 60 minutes, the temperature is l...

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PUM

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Abstract

The invention discloses a preparation method for a C.I. pigment red 53:1. The preparation method comprises the following steps of: the preparation of diazo liquid, the preparation of coupling liquid, coupling, laking reaction and post treatment. By the preparation method, the adverse effect on environment and human bodies when the component of the diazo liquid, namely 2-amino-5-chlorin-4-methyl benzene sulfonic acid is dissolved is effectively avoided; the problems that the heavy metal barium in the product exceeds the standard due to the addition of excess barium chloride in the laking reaction, and the heat resistance of the product is reduced due to the use of rosin are effectively solved; simultaneously, the pigment prepared by the method is bright in color, easy to disperse, and floppy in pigment particles; and moreover, the content of the soluble heavy metal barium in the product is below 80 mg/kg.

Description

technical field [0001] The invention belongs to the field of organic pigments, in particular to a C. I. Preparation of Pigment Red 53:1. Background technique [0002] C. I. Pigment Red 53:1 is yellowish red, widely used in printing inks, plastics, cultural and educational supplies, etc. for its bright shade, high tinting strength, excellent solvent resistance, heat resistance and stability. C. I. The existing preparation method of Pigment Red 53:1 is to dissolve 2-amino-5-chloro-4-methylbenzenesulfonic acid in ammonia water, then add hydrochloric acid for acid analysis, add ice to cool down, and put in sodium nitrite solution for diazotization Reaction, and then with 2-naphthol coupling reaction under certain conditions, and finally using barium chloride for color lake in the system. Existing technology uses volatile ammoniacal liquor to dissolve 2-amino-5-chloro-4-methylbenzenesulfonic acid in the diazotization reaction, so environment and human body are all caused a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B63/00C09B29/15C09B67/02
Inventor 吕东军陈都方李秀景赵翠平詹秀涛
Owner 宇虹颜料股份有限公司
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