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Process for producing solvent of red 135

A technology of solvent red and polar organic solvents, which is applied in chemical instruments and methods, organic dyes, organic chemistry, etc., can solve the problems of incomplete recycling, low production cost, and large amount of solvent usage, so as to avoid the relative brightness of products Low, promote the improvement of product grade, and the effect of high product brightness

Active Publication Date: 2009-08-19
NANTONG LONGXIANG NEW MATERIALS TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solvent method is a method of producing solvent red 135 with a polar organic solvent as the reaction medium. The product produced by this method has high vividness, but because solvent red 135 has a certain solubility in the organic solvent, it is relatively difficult to separate the product. The amount of solvent used is relatively large, and recycling requires a lot of energy. The recovery rate is generally about 85%, which cannot be completely recycled, so the production cost is relatively high.
The aqueous phase method is a method of producing Solvent Red 135 with hydrochloric acid aqueous solution as the reaction medium. This method only needs to be filtered to realize product separation, and the reaction medium does not need to be recycled, only needs to be neutralized. The production cost is relatively low, but the production The product quality and yield are relatively low, and the product quality is poor

Method used

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  • Process for producing solvent of red 135
  • Process for producing solvent of red 135

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] In a three-necked flask with stirring and reflux condenser, add 300g 13% hydrochloric acid solution, 60g alcohol, 28.6g tetrachlorophthalic anhydride, 15.8g 1,8-naphthalenediamine, 0.3g fatty alcohol polyoxyethylene ether, turn on the stirring and Heating, heating to reflux, reacting for 10 hours and then filtering, the filter cake is washed with water until the filtrate is neutral, and the product is dried to obtain 40.0 g (98% of the theoretical yield). Compared with the standard product, the product is similar in hue, slightly brighter, similar in depth (see Table 1 for details), and its strength is 101.2%.

[0018] Table 1

[0019] light source △E * △H * △C * △L * △a * △b * D65 / 10 0.86 0.27 0.81 0.15 0.64 0.56 A / 10 0.91 0.31 0.82 0.24 0.50 0.72 F2 / 10 0.94 0.24 0.89 0.20 0.65 0.66

[0020] (Among them: △E—color difference, △H—color difference, △L—lightness difference, △C—chromaticity difference,

[0021] △a—redness-g...

Embodiment 2

[0023] Add 2000kg of 10% hydrochloric acid solution, 150kg of acetic acid, 228kg of tetrachlorophthalic anhydride, 125kg of 1,8-naphthalenediamine, 2kg of nonylphenol polyoxyethylene ether into a 3000L enamel reactor with frame stirring and reflux condenser in sequence, and turn on Stir and heat, heat up to reflux, react for 15 hours and filter, wash the filter cake with clear water until the filtrate is neutral, and dry to obtain 317 kg of product (98.1% of the theoretical yield). Compared with the standard product, the color of the product is similar (see Table 2 for details), and the intensity is 99.1%.

[0024] Table 2

[0025] light source △E * △H * △C * △L * △a * △b * D65 / 10 0.25 0.00 0.21 0.15 0.19 0.08 A / 10 0.39 -0.05 0.34 0.19 0.31 0.15 F2 / 10 0.10 0.01 0.02 0.10 0.01 0.01

Embodiment 3

[0027] Add 3000kg of 13% hydrochloric acid solution, 200kg of dimethylformamide (DMF), 286kg of tetrachlorophthalic anhydride, 158kg of 1,8-naphthalene diamine, 2.5kg of fat in a 5000L enamel reactor with frame stirring and reflux condenser. The alcohol polyoxyethylene ether was stirred and heated, heated to reflux, and filtered after 12 hours of reaction. The filter cake was washed with clean water until the filtrate was neutral and dried to obtain 403 kg of product (98.8% of the theoretical yield). The hue of the product is similar to that of the standard product (see Table 3 for details), and the strength is 100.2%.

[0028] table 3

[0029] light source △E * △H * △C * △L * △a * △b * D65 / 10 0.34 0.07 0.26 0.21 0.21 0.16 A / 10 0.37 0.08 0.27 0.24 0.18 0.22 F2 / 10 0.35 0.07 0.26 0.23 0.19 0.19

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Abstract

The invention relates to a method for preparing solvent red 135, belonging to the field of chemical engineering. Tetrachlorophthalic anhydride and 1, 8-naphthylenediamine which have the substance amount ratio being 1:1, aqueous hydrochloric acid solution with the mass concentration of 10-15%, polar organic solvent that can be mixed and dissolved with the water and non-ionic surface activity catalyst are mixed in a reaction device provided with stirring and reflow equipment, and then the mixture is stirred and heated up to a reflow state to react for 8-15h; after being filtered, filter mass is washed by clear water until the filtrate is neutral; at last, the solvent red 135 is obtained after being dried; the dosage of the aqueous hydrochloric acid solution is 10-20 times more than that of the 1, 8-naphthylenediamine, the dosage of the polar organic solvent is 1-50% of the total content of reaction medium, and the dosage of the catalyst is 0.01-2% of the total content of reaction medium. The invention has the advantages of good product quality of a solvent method and low cost of an aqueous phase method.

Description

Technical field [0001] The invention relates to a preparation method of solvent red 135, which belongs to the field of chemical engineering. Background technique [0002] Solvent Red 135, English name Solvent Red135, molecular formula: C 18 H 6 Cl 4 N 2 O, molecular weight: 408.06, CAS number: 71902-17-5. The appearance is bright red powder. Insoluble in water, soluble in organic solvents such as ethanol, chloroform and acetone. It is mainly used for coloring polystyrene, ABS resin, polymethyl methacrylate resin, cellulose acetate, polyvinyl chloride, and also for coloring polyester fiber virgin pulp. Its structural formula is: [0003] [0004] At present, according to the different reaction medium used in the preparation of Solvent Red 135, it is divided into solvent method and water phase method. The solvent method is a method to produce solvent red 135 with polar organic solvent as the reaction medium. The product produced by this method has high brightness, but because sol...

Claims

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Application Information

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IPC IPC(8): C09B67/20C09B57/00C07D487/06C08J3/20
Inventor 杨连飞吴卫东杨彦青倪伟黄东升王思源
Owner NANTONG LONGXIANG NEW MATERIALS TECH CO LTD
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