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Method for anhydrously preparing isoindoline pigment

A technology of isoindoline and pigments, which is applied in the production process field of isoindoline yellow pigments, can solve the problems of difficult recycling, many by-products, and low product yields, and achieve industrial production convenience, low environmental pollution, The effect of high product yield

Inactive Publication Date: 2013-04-03
CINIC CHEM SHANGHAI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN200810139252.7 reports a synthesis of PY139 using an organic acid as a base-binding agent and a solvent. No water is introduced during the synthesis process. Oxidation and light resistance have been improved, but this patent uses a large amount of organic acid, which will be a great test for the corrosion resistance of the equipment
[0004] The patent documents introduced above all use a large amount of organic acids. This type of organic acid has a large amount of use, strong corrosion, high price, high recovery cost and is difficult to fully recycle. The product yield is 70-80%, and the product yield is low. There are many by-products, which bring great difficulties to wastewater treatment

Method used

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  • Method for anhydrously preparing isoindoline pigment
  • Method for anhydrously preparing isoindoline pigment

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Add 800ml of N,N-dimethylformamide and 37.5g (0.293 moles) of barbituric acid into the reaction kettle, heat up to 55°C to dissolve, add 19.2g (0.132 moles) of 1,3-bis The iminoisoindoline was dissolved in a solution of 200ml N,N-dimethylformamide, and reacted for 30 hours, during which the ammonia gas produced was decompressed and fractionated. Cool down to 20-30°C, filter, wash with methanol, and dry in vacuum to obtain 46g of pigment with a yield of 95%.

Embodiment 2

[0023] Add 800ml of N,N-dimethylacetamide and 37.5g (0.293 moles) of barbituric acid into the reaction kettle, heat up to 140°C to dissolve, add 19.2g (0.132 moles) of 1,3-di The iminoisoindoline was dissolved in a solution of 200ml N,N-dimethylacetamide, and reacted for 15 hours. During the reaction, the ammonia gas produced was fractionally distilled off under reduced pressure. Cool down to 20-30°C, filter, wash with methanol, and dry in vacuum to obtain 45g of pigment with a yield of 94%.

Embodiment 3

[0025] Add 800ml of ethylene glycol and 37.5g (0.293 moles) of barbituric acid into the reaction kettle, heat up to 110°C to dissolve, add 19.2g (0.132 moles) of 1,3-diiminoisoindoline dropwise within 30 minutes Dissolved in 200ml of ethylene glycol, reacted for 25 hours, during the reaction process, the ammonia gas produced was decompressed and fractionated. Cool down to 20-30°C, filter, wash with methanol, and dry in vacuum to obtain 45g of pigment with a yield of 94%.

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Abstract

The invention provides a method for anhydrously preparing an isoindoline pigment, comprising the following steps of: dissolving or suspending barbituric acid into an organic solvent A; adding an organic solvent B containing 1,3-diimino isoindoline to react; in a reaction process, fractionating generated ammonia gas; and then, collecting the isoindoline pigment from a reaction product. The method disclosed by the invention has the beneficial effects are very obvious; a pure organic solvent reaction system is adopted and a product yield is high; only the organic solvents need to be recycled; the production cost is low and the environmental pollution is small; and the method is convenient for industrial production.

Description

technical field [0001] The invention relates to a production process of isoindoline yellow pigment. Background technique [0002] Isoindoline pigments have good solvent resistance, migration resistance, acid and alkali resistance, redox resistance and heat resistance due to the existence of intermolecular and intramolecular hydrogen bonds and the formation of three-dimensional network stacking. Widely used in plastics, coatings and inks. Since the pigments of this type are synthesized from 1,3-diiminoisoindoline, barbituric acid and its derivatives except for a few documents, the main intermediate 1,3-diiminoisoindoline is Indoline can be synthesized from phthalonitrile or phthalic anhydride with substituents on the benzene ring. [0003] DE2041999 reported the preparation of pigments by low-temperature reaction followed by heat treatment in DMF / HOAc. Although the patent used DMF as a solvent, an organic acid was used in the reaction process. US4166179 reports the use of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B57/04
Inventor 李秀娟
Owner CINIC CHEM SHANGHAI
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