Method for one-step synthesis of diamino decalin by catalytic hydrogenation of dinitro naphthalene
A technology of dinitronaphthalene catalysis and diaminodecalin, applied in chemical instruments and methods, preparation of organic compounds, molecular sieve catalysts, etc., can solve problems such as narrow activation temperature, low effective utilization rate of nickel, and low dispersion , to achieve the effect of improving conversion rate, good activity and product selectivity, and good selectivity
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Examples
preparation example Construction
[0023] The preparation method of the supported nickel-based hydrogenation catalyst is as follows: Under the condition of ultrasonic assisted oscillation, the active component nickel is loaded on the oxide or zeolite molecular sieve carrier by impregnation method. Generally, the nickel-containing salt solution is first impregnated into the oxide Or on a zeolite molecular sieve carrier, after drying, calcinate at 300-500°C for 3-5h, and then reduce at 250-500°C for 2-4h under a hydrogen atmosphere to obtain a supported nickel-based hydrogenation catalyst.
[0024] For example, take nickel nitrate 0.68 ~ 4.11g (the value here is 5 ~ 30wt% and SiO 2 Calculated from 2.5g, the load is based on the nickel metal load to calculate the amount of metal salt nickel nitrate, the amount of nickel metal is 0.14 ~ 0.83g), dissolved in 100mL of water, and then added 2.5g of SiO under the condition of ultrasonic assisted oscillation 2 , ultrasonically oscillating and impregnating at 70°C for 4h...
Embodiment 1
[0028] In a stirred pressure reactor, add Ni / SiO with a nickel loading mass fraction of 10% 2 Hydrogenation catalyst 100mg, 1,5-dinitronaphthalene 1.0g, tetrahydrofuran 9.0g, replace the air in the reactor with hydrogen three times, then fill in hydrogen to make the reaction pressure of the reactor reach 5.0MPa, start stirring, and the stirring speed is 250r / min, and heat the reaction kettle to make the reaction temperature reach 220°C, supplement and maintain the reaction pressure at 7.5MPa, keep the constant temperature for 6 hours, take out the reaction product, filter the catalyst after cooling, and obtain 1,5-diaminodecalin. Gas chromatography analysis showed that the conversion rate of 1,5-dinitronaphthalene was 99.1%, and the selectivity of 1,5-diaminodecalin was 96.2%.
Embodiment 2
[0030] In a stirred pressure reactor, add nickel loading mass fraction of 5% Ni / SiO 2 Hydrogenation catalyst 100mg, 1,8-dinitronaphthalene 1.0g, tetrahydrofuran 9.0g, replace the air in the reactor with hydrogen three times, then fill in hydrogen to make the reaction pressure of the reactor reach 5.5MPa, start stirring, and the stirring speed is 300r / min, and heat the reaction kettle to make the reaction temperature reach 200°C, replenish and maintain the reaction pressure at 8.0MPa, keep the constant temperature for 4 hours, take out the reaction product, filter the catalyst after cooling, and obtain 1,8-diaminodecalin. Gas chromatography analysis showed that the conversion rate of 1,8-dinitronaphthalene was 99.6%, and the selectivity of 1,8-diaminodecalin was 93.1%.
PUM
Abstract
Description
Claims
Application Information
- R&D Engineer
- R&D Manager
- IP Professional
- Industry Leading Data Capabilities
- Powerful AI technology
- Patent DNA Extraction
Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.
© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com