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Method for preparing 1,5-diaminonaphthalene through naphthalene in one step and application of catalysts

A diaminonaphthalene and catalyst technology, applied in molecular sieve catalysts, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem that the intermediate process is not easy to control, the synthesis process route is complicated, the process is complicated, etc. problem, to achieve the effect of simple operation, simple preparation process and mild reaction conditions

Active Publication Date: 2013-12-04
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process avoids the formation of isomer 1,8-diaminonaphthalene through ring closure, but the synthesis process is complicated and the intermediate process is not easy to control
As can be seen from the above, existing methods for synthesizing 1,5-diaminonaphthalene with naphthalene as a raw material all need to go through multiple steps, and the process is complicated; and the obtained product often contains other impurities In addition, its preparation process causes great pollution to the environment, causing environmental protection burden.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 2.04g (NH 4 ) 6 Mo 7 o 24 4H 2 O, 5.51gNi(NO) 2 ·6H 2 O, 7.24g mass concentration is 50% Mn(NO 3 ) 2 solution. Take an appropriate amount of water to dissolve and impregnate 10g of γ-Al 2 o 3 ; After impregnating for 24 hours, the resulting solution was dried under vacuum, calcined, and finally reduced by hydrogen to obtain γ-Al 2 o 3 Catalyst supporting Mo, Ni, Mn.

[0021] The preparation method of the Ni, Mn, and Mo-based catalyst supported by the titanium-silicon molecular sieve is the same as above.

[0022] Weigh 0.50g of naphthalene into a 100ml three-neck flask, add 20.00g of N,N-dimethylformamide (hereinafter referred to as DMF), and add 0.08g of Ni / titanium silicate molecular sieve with a mass fraction of 20%. Start the constant flow pump, heat and stir at 50°C for 20 minutes, then add 5.00 g of ammonia water with a mass fraction of 25% to the three-necked flask, and slowly add 5.11 g of hydrogen peroxide with a mass fraction of 30% by const...

Embodiment 2

[0024] Weigh 0.50g of naphthalene into a 100ml three-neck flask, add 20.00g of DMF, and add 0.11g of Mo / γ-Al with a mass fraction of 10% 2 o 3 . Start the constant flow pump, heat and stir at 50°C for 20 minutes, then add 5.03g of ammonia water with a mass fraction of 25% to the three-necked flask, and slowly add 5.01g of 30% hydrogen peroxide dropwise with the constant flow pump. After reacting for 2 hours under the conditions of 65° C., normal pressure, and condensing reflux, the sample solution was obtained by suction filtration. The 1,5-diaminonaphthalene obtained by liquid phase analysis and calculation was 11.65 mg.

Embodiment 3

[0026] Weigh 0.50g of naphthalene into a 100ml three-neck flask, add 20.01g of DMF, and add 0.11g of Mo / γ-Al with a mass fraction of 10% at the same time 2 o 3 . Start the constant flow pump, heat and stir at 50°C for 20 minutes, then add 5.05 g of ammonia water with a mass fraction of 25% to the three-necked flask, and slowly add 10.03 g of hydrogen peroxide with a mass fraction of 30% by constant flow pump. After reacting for 2 hours under the conditions of 65° C., normal pressure, and condensing reflux, the sample solution was obtained by suction filtration. The 1,5-diaminonaphthalene obtained by liquid phase analysis and calculation was 21.42mg.

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Abstract

The invention relates to a method for preparing 1,5-diaminonaphthalene through naphthalene in one step and application of catalysts. The naphthalene generates the 1,5-diaminonaphthalene in one step in an organic solvent under the action of ammonia water, hydrogen peroxide and the catalysts, and the used catalysts are obtained in a manner that one type or several types of Ni, Mn and Mo are loaded on gamma-Al2O3 or a titanium silicon molecular sieve. Under the action of the catalysts, the naphthalene reacts with the ammonia water and the hydrogen peroxide in the solvent to compound the 1,5-diaminonaphthalene in one step. The method is simple in technological process, mild in reaction condition, easy and convenient to operate, and friendly to the environment.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and specifically relates to a method for preparing 1,5-diaminonaphthalene from naphthalene in one step and an application of a catalyst. Background technique [0002] In recent years, the application of 1,5-diaminonaphthalene in various fine chemical products such as organic synthesis, pigments, dyes, medicines, pesticides, rubber additives, resins, and photosensitive materials has gradually increased. The demand for 1,5-naphthalene diisocyanate has greatly increased, and the research on its synthesis method continues to increase. [0003] The literature reports on the preparation methods of 1,5-diaminonaphthalene mainly include: naphthalene nitration reduction method, ring method, ammonification method, electrochemical hydrolysis method, etc. The naphthalene nitration reduction method is a traditional method to produce 1,5-diaminonaphthalene. Naphthalene is nitrated with mixed acid to generate ...

Claims

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Application Information

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IPC IPC(8): C07C211/58C07C209/02B01J29/89B01J23/889
Inventor 刘平乐胡征宇罗和安郝芳游奎一
Owner XIANGTAN UNIV
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