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Pigment yellow 139 synthesis process

A synthesis process and a technology for pigment yellow, applied in the field of pigment production, can solve the problems of complex production process route of phthalonitrile, environmental protection, large safety impact, insufficient product supply, etc., to avoid a large amount of waste acid water and save a lot of The effect of energy consumption and shortening of process time

Pending Publication Date: 2022-06-03
山东世纪连泓新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] However, the domestic phthalonitrile production process is complicated, the production cost is high, and the pollution produced is relatively large, so there are relatively few manufacturers. In recent years, environmental protection and safety have greatly affected the supply of products.

Method used

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  • Pigment yellow 139 synthesis process

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Pigment Yellow 139 synthesis process, including the following steps:

[0031] (1) The use of solid melting method to use batch or continuous or batch and continuous combination of phthalic anhydride and urea, under the action of the catalyst to synthesize 1,3-diiminoisoindoleline,

[0032] (2) The crude pigment Yellow 139 was synthesized by the reaction of 1,3-diiminoisoindoleline with barbiturate acid.

[0033] The steps described (1) are specifically:

[0034] Urea, ammonium salts were added to the reactor, heated to melt and then a catalyst was added, dehydrated at 120-135 °C for 2 to 3 hours, phthalic anhydride was added after dehydration, and the iminoline reaction was carried out at 130 ~150 °C for 3 hours, and the heating was continued to 160 ~ 180 ° C for 5 to 7 hours for condensation, and after the condensation was completed, the cooling was reduced to 60 ° C or less, and the water was added to add sodium hydroxide, until the material dissolution was dissolved and d...

Embodiment 2

[0042] Pigment Yellow 139 synthesis process, including the following steps:

[0043] (1) The use of solid melting method to use batch or continuous or batch and continuous combination of phthalic anhydride and urea, under the action of the catalyst to synthesize 1,3-diiminoisoindoleline,

[0044](2) The crude pigment Yellow 139 was synthesized by the reaction of 1,3-diiminoisoindoleline with barbiturate acid.

[0045] The steps described (1) are specifically:

[0046] Urea, ammonium salts were added to the reactor, heated to molten after the catalyst was added, dehydrated at 120-135 ° C for 2 to 3 hours, phthalic anhydride was slowly added to the above reactor after dehydration, and the iminoidation reaction was carried out at 130 ~ 150 ° C for 3 hours, and the heating was continued to 160 ~ 180 ° C for 5 to 7 hours of condensation, and after the condensation was completed, the vacuum was evacuated and cooled below 60 ° C, and the 1,3-diiminoisoindoline was adhered to the molten c...

Embodiment 1 and comparative example 1

[0081] (2) Example 1 compared to the counter-proportional 1:

[0082]Example 1: 1,3-Diiminoisoindole is dissolved in an alkaline methanol solution, facilitating the reaction; In particular, the reaction system is methanol and a large number of anhydrous solvents are added, with the distillation of methanol, the residual acidic wastewater is very small, and after separation by pressure filtration, the amount of waste liquid produced is small and easy to treat.

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PUM

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Abstract

The invention discloses a pigment yellow 139 synthesis process, which belongs to the technical field of pigment production, and comprises the following steps: synthesizing 1, 3-diimino isoindoline from phthalic anhydride and urea under the action of a catalyst by using a solid-state melting method in an intermittent or continuous or intermittent and continuous combined manner, and synthesizing the 1, 3-diimino isoindoline from the 1, 3-diimino isoindoline to obtain the pigment yellow 139. The preparation method comprises the following steps: reacting 2, 3-diimino isoindoline with barbituric acid to synthesize a crude product pigment yellow 139; the method has the beneficial effects that the phthalic anhydride and the urea are used in the solid melting method, so that the problem of phthalonitrile is avoided, and large-scale production of the pigment yellow 139 is facilitated; the dehydration and drying process in the refining process of the 1, 3-diimino isoindoline is omitted, the process time is shortened, and a large amount of energy consumption is saved; and a high-temperature filtering means is adopted, so that the content of cyanuric acid can be maintained below 30ppm, meanwhile, the loss of the pigment yellow 139 along with a large amount of hot water can be avoided, and the yield of the pigment yellow 139 is ensured.

Description

Technical fields: [0001] The present invention belongs to the field of pigment production technology, more specifically relates to the pigment yellow 139 synthesis process. Background: [0002] Pigment Yellow 139, as one of the isoindoleline pigments, because its molecules contain carbonyl, imino, cyano and amide groups, etc., thereby forming intramolecular and intermolecular hydrogen bonds, resulting in a more planar molecular structure. Therefore, pigment yellow 139 is an organic pigment with excellent heat resistance and solvent resistance. [0003] The preparation method of pigment yellow 139 is mainly: under the condition of alkali presence, the phthalonitrile is first reacted in an alcohol, and then the resulting intermediate is reacted with a barbiturate acid compound to obtain the target. [0004] For example, the national invention patent number 201110447652.6 discloses a method for preparing C.I. pigment yellow 139. The method comprises [0005] (1) the steps of prepari...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B57/04C07D403/14
CPCC09B57/04C07D403/14Y02P20/584
Inventor 王庆刚范文锋高卫
Owner 山东世纪连泓新材料有限公司
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