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Preparation method of pigment yellow 138

A pigment yellow and crude product technology, applied in the field of preparation of pigment yellow 138, can solve the problems of difficult recycling and incompleteness, and achieve the effects of low environmental pollution, high raw material utilization rate, and high product quality

Active Publication Date: 2013-05-08
南通龙翊新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN1918244A proposes a pigmentation method for preparing transparent Pigment Yellow 138. This method grinds Pigment Yellow 138 in the presence of an abrasive, and uses 5-10 parts of salt in the process (the quality of the pigment is calculated as 1 part, the same below). , 2 parts of organic solvent, 100 parts of water, the grinding medium is 100 parts of grinding balls, the salt and organic solvent used are difficult to recover
In a word, the above-mentioned preparation methods disclosed at home and abroad about Pigment Yellow 138 are incomplete or insufficient, therefore, a new technical solution should be provided to solve the above problems

Method used

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  • Preparation method of pigment yellow 138

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Effect test

Embodiment 1

[0020] The preparation method of Pigment Yellow 138 comprises synthesis steps and pigmentation steps:

[0021] The synthesis steps are as follows: add 480g of benzoic acid into a reactor with heating and stirring, heat up to 125°C to melt it, start stirring, add 87g of tetrachlorophthalic anhydride and 16g of 8-aminoquinaldine in sequence, and react at 160°C for 3 hours , then heated up to 220°C for 2 hours, cooled the reactant to 130°C, poured it into 840g of 20% sodium hydroxide solution within 0.5h, reacted for 20min, filtered, washed, and dried to obtain 63.8g of crude pigment yellow 138 , The filtrate recovered 478.3 g of benzoic acid and unreacted tetrachlorophthalic anhydride after acid analysis.

[0022] The pigmentation step is: add 300 g of DMF to a reactor with heating and stirring and a reflux condenser, start stirring, add 20 g of the crude product of Pigment Yellow 138 and 1 g of sodium dodecylbenzene sulfonate, and after dispersing evenly, in 0.5 Add 10g of 30%...

Embodiment 2

[0025] The preparation method of Pigment Yellow 138 comprises synthesis steps and pigmentation steps:

[0026] The synthesis steps are as follows: add 320g of benzoic acid into a reactor with heating and stirring, heat up to 127°C to melt, start stirring, add 60g of tetrachlorophthalic anhydride and 16g of 8-aminoquinaldine in sequence, and react at 140°C for 2 hours , then raised the temperature to 180°C for 3 hours, cooled the reactant to 130°C, poured it into 960g of 10% sodium hydroxide solution within 40min, reacted for 10min, filtered, washed and dried to obtain 65.7g of crude pigment yellow 138, The filtrate recovered 303.4 g of benzoic acid and unreacted tetrachlorophthalic anhydride after acid analysis.

[0027] The pigmentation step is as follows: add 600 g of o-dichlorobenzene into a reactor with heating and stirring and a reflux condenser, start stirring, add 20 g of the above-mentioned crude product of Pigment Yellow 138, and after the dispersion is uniform, add 6...

Embodiment 3

[0030] The preparation method of Pigment Yellow 138 comprises synthesis steps and pigmentation steps:

[0031] The synthesis steps are as follows: add 160g of benzoic acid to a reactor with heating and stirring, heat up to 130°C to melt it, start stirring, add 70g of tetrachlorophthalic anhydride and 16g of 8-aminoquinaldine in sequence, and react at 180°C for 1 hour , then heated up to 200°C to react for 4h, cooled the reactant to 130°C, poured it into 1200g 5% sodium hydroxide solution within 1h, reacted for 1h, filtered, washed and dried to obtain 66.9g of crude pigment yellow 138, The filtrate recovered 154.8 g of benzoic acid and unreacted tetrachlorophthalic anhydride after acid analysis.

[0032] The pigmentation step is as follows: add 100 g of N-methylpyrrolidone into a reactor with heating and stirring and a reflux condenser, start stirring, add 20 g of the above-mentioned crude product of Pigment Yellow 138, and after dispersing evenly, add 30% sodium methoxide with...

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Abstract

The invention discloses a preparation method of pigment yellow 138, which comprises the following steps: synthesis: adding benzoic acid into a reactor, sequentially adding tetrachlorophthalic anhydride and 8-aminoquinaldine, heating to 140-160 DEG C, reacting for 1-3 hours, heating to 180-220 DEG C, reacting for 2-4 hours, cooling the reaction product to 130 DEG C, pouring into a previously prepared sodium hydroxide solution, reacting for 10-60 minutes, filtering, washing and drying to obtain a crude pigment yellow 138 product; and preparation of pigment: adding an organic solvent and the crude pigment yellow 138 product into a reactor, adding sodium methoxide or methanol solution thereof, heating to 40-80 DEG C, carrying out salification reaction for 1-3 hours, neutralizing by adding acid, precipitating the pigment in the form of molecules, distilling out low-boiling-point substances, heating to 80-150 DEG C, keeping the temperature for 1-6 hours to obtain slurry, filtering the slurry, washing, drying and pulverizing to obtain the pigment yellow 138. The invention has the advantages of high utilization ratio of raw materials, low environmental pollution, high product quality and favorable economic benefit.

Description

technical field [0001] The invention relates to a preparation method of Pigment Yellow 138, which belongs to the field of chemical industry. Background technique [0002] Pigment Yellow 138 (C.I. Pigment Yellow 138, C.I. 56300) is a high-grade yellow organic pigment, belonging to quinophthalone pigments, CAS number: 30125–47–4, molecular formula: C 26 h 6 Cl 8 N 2 o 4 , molecular weight: 693.97, structural formula: [0003] [0004] Pigment Yellow 138 is a bright green light yellow powder with strong tinting strength, high heat resistance, excellent heat resistance, acid resistance, alkali resistance, and no migration. It is mainly used for the coloring of plastics, paints, and paints, and is also used for synthetic fibers. Dope coloring. [0005] There are few domestic and foreign reports on the preparation of Pigment Yellow 138. U.S. Patent No. 3,622,583A proposes a method for preparing quinophthalone pigments, with 8-aminoquinaldine and tetrachlorophthalic anhyd...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B25/00
Inventor 倪伟黄东升薛冬杰杨连飞
Owner 南通龙翊新材料科技有限公司
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