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A kind of method for preparing 1,5-diaminodecalin by catalytic hydrogenation of 1,5-diaminonaphthalene

A technology of diaminodecalin and diaminonaphthalene, which is applied in the field of preparing 1,5-diaminodecalin by catalytic hydrogenation of 1,5-diaminonaphthalene, can solve the problem of low nickel effective utilization rate, narrow activation temperature, Dispersion is not high, to achieve good activity and product selectivity, high reuse rate, simple preparation process

Inactive Publication Date: 2016-02-10
武汉椿岭科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the active temperature of nickel-aluminum catalysts currently used in industry is narrow (generally 130-180°C), and even under the best conditions, the yield of the target product cyclohexylamine is only 30-50%, and Accompanied by a large number of side reaction products, such as dicyclohexylamine, N-cyclohexylaniline, benzene and ammonia, in addition to unconverted aniline, these disadvantages are generally considered to be largely due to the higher nickel content, which in the support Accumulated on the surface, the degree of dispersion is not high, resulting in low effective utilization of nickel

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0018] The preparation method of the supported nickel-based hydrogenation catalyst is as follows: the active component nickel is loaded on the oxide or zeolite molecular sieve carrier by impregnation method. The impregnation method generally first impregnates the nickel salt solution on the oxide or molecular sieve carrier, and after drying Calcined at 400°C for 3-5h, then reduced at 400°C for 2-4h under a hydrogen atmosphere to obtain a supported nickel-based hydrogenation catalyst.

[0019] For example, weigh 1.37g to 4.11g of cobalt nitrate (the value here is based on the metal nickel loading mass accounting for 10 to 30% of the hydrogenation catalyst and the selection of Al 2 o 3 The mass is calculated at 2.5g, and the load is calculated as the nickel metal load to calculate the amount of metal salt nickel nitrate, the amount of nickel metal is 0.28~0.83g), dissolved in 100mL of water, and then added 2.5gAl 2 o 3 , impregnation reaction at 80°C for 10h, rotary evaporatio...

Embodiment 1

[0023] In a stirred pressure reactor, add a hydrogenation catalyst Ni / Al with a nickel loading mass fraction of 10% 2 o 3 100mg, 1.0g of 1,5-diaminonaphthalene (NDA), 9.0ml of tetrahydrofuran, replace the air in the reactor with hydrogen three times, then fill in hydrogen to make the reaction pressure of the reactor reach 4.0MPa, start stirring, and the stirring speed is 300r / min, and heating the reactor to make the reaction temperature reach 220 ° C, supplementing and maintaining the reaction pressure is 7.0MPa, constant temperature reaction 6h, take out the reaction product, filter the catalyst after cooling, and obtain 1,5-diaminodecalin ( h 10 NDAs). Using gas chromatography analysis, the conversion rate of 1,5-diaminonaphthalene (NDA) was 100%, and the conversion rate of 1,5-diaminodecalin (H 10 NDA) selectivity was 95.4%.

Embodiment 2

[0025] In a stirred pressure reactor, add a hydrogenation catalyst Ni / Al with a nickel loading mass fraction of 10% 2 o 3 100mg, 2.0g of 1,5-diaminonaphthalene (NDA), 8.0ml of tetrahydrofuran, replace the air in the reactor with hydrogen three times, then fill in hydrogen to make the reaction pressure of the reactor reach 4.0MPa, start stirring, and the stirring speed is 300r / min, and heating the reactor to make the reaction temperature reach 220 ° C, supplementing and maintaining the reaction pressure is 7.0MPa, constant temperature reaction 6h, take out the reaction product, filter the catalyst after cooling, and obtain 1,5-diaminodecalin ( h 10 NDAs). Using gas chromatography analysis, the conversion rate of 1,5-diaminonaphthalene (NDA) was 100%, and the conversion rate of 1,5-diaminodecalin (H 10 NDA) selectivity was 95.8%.

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Abstract

The invention relates to a method for preparing 1,5-diaminodecalin by catalytic hydrogenation of 1,5-diaminonaphthalene, which is characterized in that: adding 1,5-diaminonaphthalene and a solvent into a pressure reactor, adding Type nickel-based hydrogenation catalyst, the amount of the catalyst is 2.5-10% of the added amount of the reaction substrate 1,5-diaminonaphthalene in terms of mass, and the air in the reactor is replaced with hydrogen for three times, and then filled with hydrogen to make the reactor When the reaction pressure reaches 4.0MPa, start stirring, and heat the reactor to make the temperature 190-230°C. Supplement hydrogen and maintain the reaction pressure of the reactor to 6-8MPa. React at constant temperature for 5-8 hours. After cooling, filter out the catalyst to obtain 1 ,5-Diaminodecalin. The invention can significantly improve the conversion rate of 1,5-diaminonaphthalene, and at the same time, the catalyst has low cost, simple preparation and long service life, and exhibits good application prospects.

Description

technical field [0001] The invention relates to a kind of catalytic hydrogenation of 1,5-diaminonaphthalene (NDA) to prepare 1,5-diaminodecalin (H 10 NDA), specifically relates to a supported nickel-based hydrogenation catalyst to catalyze 1,5-diaminonaphthalene (NDA) hydrogenation to prepare 1,5-diaminodecalin (H 10 NDA) approach. Background technique [0002] In recent years, 1,5-diaminonaphthalene (NDA) has gradually increased in the application of organic synthesis, pigments, dyes, pharmaceuticals, pesticides, rubber additives, resins, photosensitive materials and other fine chemical products, especially the main raw material of advanced polyurethane The demand for 1,5-diisocyanate has greatly increased, and the research on its synthesis has been increasing in various countries. However, the hydrogenation reaction of 1,5-diaminonaphthalene and the full hydrogenation product 1,5-diaminodecalin (H 10 NDA) research and application, there are few reports. [0003] The re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/38C07C209/72B01J23/755B01J29/14B01J29/46B01J29/035B01J29/76B01J29/85
Inventor 刘新泰夏清华鲁新环
Owner 武汉椿岭科技有限公司
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