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A kind of preparation method of diaminonaphthalene

A technology of diaminonaphthalene and dinitronaphthalene is applied in the field of pigments and dyes, which can solve the problems of increasing product cost and failing to take advantage of the hydrazine hydrate reduction method, and achieves lowering treatment costs, improving market competitiveness, and reducing the generation of three wastes. amount of effect

Active Publication Date: 2018-07-31
XIAN CAIJING OPTO ELECTRICAL SCI & TECH
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Problems solved by technology

[0006] For example, the Chinese patents CN103664645A and CN101823968B describe in detail a method for reducing 1,8-dinitronaphthalene with hydrazine hydrate to prepare 1,8-diaminonaphthalene. The above two methods all need to separate mixed dinitronaphthalene Purification, separation of mixed dinitronaphthalene increases product cost, does not give play to the advantages of hydrazine hydrate reduction method; this method is not suitable for industrial production of 1,8-diaminonaphthalene and 1,5-diaminonaphthalene

Method used

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Embodiment 1

[0038] The present embodiment provides a kind of preparation method of diaminonaphthalene, and this method comprises the following steps:

[0039] Step 1, the synthesis of mixed dinitronaphthalene:

[0040] Add 246kg of sulfuric acid with a mass concentration of 76% to a 500L reactor with a stirrer, a thermometer, a reflux condenser, and a high-level dripping tank, start stirring, keep the temperature at 15-30°C, and then add dropwise a mass concentration of 98% 56.5kg of fuming nitric acid was added dropwise in 0.5h, and after mixing evenly, 45kg of naphthalene was added in batches, and the addition was completed in 2 hours. React to obtain the first reaction solution;

[0041] The first reaction liquid is lowered to normal temperature, filtered to obtain the first filtrate and the first filter cake, the first filtrate is recovered, the first filter cake is washed with water, and the crude product is beaten and purified with 200kg of toluene to obtain 76kg of mixed dinitrona...

Embodiment 2

[0049] The present embodiment provides a kind of preparation method of diaminonaphthalene, and other processes of this method are identical with embodiment 1, and difference is only in:

[0050] In this embodiment, the first organic solvent is replaced by methanol from toluene.

[0051] In the second organic solvent, methanol was replaced by ethanol, and toluene was replaced by dichloroethane.

[0052] The reflux reaction time in step 2 was 9 hours.

[0053] The characterization results of 1,8-diaminonaphthalene are the same as in Example 1, and the characterization results of 1,5-diaminonaphthalene are the same as in Example 1.

[0054] Based on mixed dinitronaphthalene, the yield of 1,8-diaminonaphthalene: 53%, the yield of 1,5-diaminonaphthalene: 32%, the total yield is 85%.

Embodiment 3

[0056] The present embodiment provides a kind of preparation method of diaminonaphthalene, and other processes of this method are identical with embodiment 1, and difference is only in:

[0057] In this embodiment, the first organic solvent is replaced by dichloroethane from toluene.

[0058] In the second organic solvent, change from methanol and toluene to acetone.

[0059] The reflux reaction time in step 2 is 4 hours.

[0060] The characterization results of 1,8-diaminonaphthalene are the same as in Example 1, and the characterization results of 1,5-diaminonaphthalene are the same as in Example 1.

[0061] Based on mixed dinitronaphthalene, the yield of 1,8-diaminonaphthalene: 51%, the yield of 1,5-diaminonaphthalene: 31%, the total yield is 82%.

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Abstract

The invention provides a method for preparing diaminonaphthalene. The method comprises the following steps: carrying out a nitration reaction by adopting sulfuric acid, fuming nitric acid and naphthalene so as to obtain mixed dinitronaphthalene; adding a second organic solvent, the mixed dinitronaphthalene, a catalyst and activated carbon into a reaction kettle, raising the temperature to 60-65 DEG C, adding hydrazine hydrate, and reacting and separating so as to obtain second filtrate and second filter cake; separating and purifying the second filtrate so as to obtain a solid, namely 1,8-diaminonaphthalene; and separating and purifying the second filter cake so as to obtain 1,5-diaminonaphthalene. According to the preparation of the mixed dinitronaphthalene, the nitratlon reaction is carried out by adopting an organic solvent free method, the waste acid can be recycled, and the yield and treatment cost of the three wastes can be reduced. The mixed dinitronaphthalene is directly reduced, the separation cost is reduced, and the market competitiveness is improved for industrial production. By utilizing different physical properties of the mixed dinitronaphthalene in different organic solvents, 1,8-diaminonaphthalene and 1,5-diaminonaphthalene with high purity are separated.

Description

technical field [0001] The invention belongs to the field of pigments and dyes, and relates to intermediates of pigments and dyes, in particular to a preparation method of diaminonaphthalene. Background technique [0002] 1,8-diaminonaphthalene is an important intermediate for the manufacture of oil-soluble pigments, mainly used in the synthesis of C.1. Oil-soluble orange 60 gas oil-soluble red 135#, etc. These two pigments are widely used in PS, AS, ABS, Coloring of various substances such as MMA, rigid PVC, PET, etc. Especially in recent years, the successive development of black oil-soluble pigments, such as ballpoint pen ink, has increased the demand for 1,8-diaminonaphthalene. 1,5-diaminonaphthalene and 1,8-diaminonaphthalene are two important compounds among the isomers of diaminonaphthalene. They are mainly used as intermediates of dyes (pigments) and also as raw materials for resins and pesticides. [0003] The preparation of dinitronaphthalene, an intermediate of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/36C07C209/84C07C211/58
CPCC07C201/08C07C209/36C07C209/84C07C211/58C07C205/06
Inventor 杜渭松高嫒嫒林岩柏赵群星李涛张胜军海啸别国军徐磊郭计化张伟杰张旺财
Owner XIAN CAIJING OPTO ELECTRICAL SCI & TECH
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