Nitration catalyst and preparation method and application thereof

A catalyst, liquid-phase nitration technology, applied in the preparation of nitro compounds, catalysts for physical/chemical processes, chemical instruments and methods, etc., can solve the problems of high reaction cost, expensive fluorophosphate, catalyst deactivation, etc., and achieve simplification Process, improve resource utilization, simple effect of separation

Inactive Publication Date: 2011-09-07
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Olah G.A. et al. (Proc.Natl.Acad.Sci.USA1997,94:11783-11785) found that methane, ethane, propane, butane, neopentane in dichloromethane or nitroethane solvent Electrophilic nitration reaction occurs in the presence of fluorophosphate nitrate to obtain the corresponding nitro compound, but fluorophosphate is expensive, which makes the reaction cost higher
Ishii et al. (J.Org.Chem.2002, 67:5663-5668) have shown that N-hydroxyphthalimide can be used as a catalyst to catalyze the nitration of aliphatic hydrocarbons, but the catalyst loses its strength soon after the reaction. live

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  • Nitration catalyst and preparation method and application thereof

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Comparison scheme
Effect test

Embodiment 1

[0031] 16 g of ZrOCl 2 ·8H 2 O and 20g Al(NO 3 ) 3 ·9H 2 O was dissolved in distilled water to prepare a solution with a concentration of 1mol / L, and then a certain amount of 6mol / L ammonia water was added under the condition of rapid stirring to control the pH value of the solution to 9.0 to obtain Zr(OH) 4 Precipitation and Al(OH) 3 , the precipitate was aged at 30 °C for 24 hours, filtered, and then washed repeatedly with deionized water to remove chloride ions until the AgNO 3 Solution test filtrate free of chloride ions. The resulting precipitate was dried at 110°C for 12 hours to obtain a solid powder, which was ground and impregnated with 200ml of 1.0mol / L sulfuric acid solution for 24 hours, then filtered off excess sulfuric acid, dried at 110°C and placed in a muffle furnace The temperature was raised to 550° C. at a heating rate of 5° C. per minute, and the calcination was continued at this temperature for 3 hours to obtain the catalyst for catalyzing the liqui...

Embodiment 2

[0033] 16 g of ZrOCl 2 ·8H 2 O and 5 g Al(NO 3 ) 3 ·9H 2 O was dissolved in distilled water to prepare a solution with a concentration of 1mol / L, and then a certain amount of 6mol / L ammonia water was added under the condition of rapid stirring to control the pH value of the solution to 9.0 to obtain Zr(OH) 4 Precipitation and Al(OH) 3 , the precipitate was aged at 10°C for 24 hours, then filtered, and then washed repeatedly with deionized water to remove chloride ions until the AgNO 3Solution test filtrate free of chloride ions. The obtained precipitate was dried at 110°C for 12 hours to obtain a solid powder, which was ground and impregnated with 150ml of 1.0mol / L sulfuric acid solution for 24 hours, then filtered off excess sulfuric acid, dried at 110°C and placed in a muffle In the furnace, the temperature was raised to 650° C. at a rate of 5° C. per minute, and the calcination was continued at this temperature for 3 hours to obtain the catalyst for catalyzing the liq...

Embodiment 3

[0035] 16 g of ZrOCl 2 ·8H 2 O and 5 g Al(NO 3 ) 3 9H 2 O was dissolved in distilled water to prepare a solution with a concentration of 1mol / L, and then a certain amount of 6mol / L ammonia water was added under the condition of rapid stirring to control the pH value of the solution to 9.0 to obtain Zr(OH) 4 Precipitation and Al(OH) 3 , the precipitate was aged at 10°C for 24 hours, then filtered, and then washed repeatedly with deionized water to remove chloride ions until the AgNO 3 Solution test filtrate free of chloride ions. The obtained precipitate was dried at 110°C for 12 hours to obtain a solid powder, which was ground and impregnated with 150ml of 1.0mol / L sulfuric acid solution for 24 hours, then filtered off excess sulfuric acid, dried at 110°C and placed in a muffle In the furnace, the temperature was raised to 650° C. at a rate of 5° C. per minute, and the calcination was continued at this temperature for 3 hours to obtain the catalyst for catalyzing the liq...

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Abstract

The invention relates to a catalyst used in synthesis of nitrocyclohexane by nitrifying a cyclohexane liquid phase, a preparation method and application thereof. In the catalyst, a zirconium-aluminum composite oxide is taken as a carrier, and sulfuric acid is loaded on the carrier by taking an immersion method to form solid acid. The catalyst is used for catalyzing a liquid-phase nitration reaction between cyclohexane serving as a raw material and nitric acid under a certain condition to synthesize nitrocyclohexane. By adopting the method disclosed by the invention, the process can be simplified greatly, the cost is lowered, the catalyst is very easy to separate after the reaction, the problems of a large quantity of byproducts caused by mixed acid nitration in the conventional nitration,difficulty in treating waste acid and environmental pollution are solved, and the resource utilization ratio can be effectively increased.

Description

technical field [0001] The invention relates to a catalyst for liquid-phase nitration of cyclohexane to synthesize nitrocyclohexane, a preparation method and application thereof. Background technique [0002] Nitroalkane is a fine chemical intermediate with a wide range of uses, and nearly 2,000 derivatives can be produced. Nitroalkanes can be partially catalytically reduced to nitroso compounds and oximes, among which oximes can be rearranged into amide products or synthetic pesticides; the principle of complete reduction can be used to prepare amine compounds, which are used in fuels, pigments and medicines, etc. An important class of synthetic raw materials for chemical products. Nitroalkane has become an important raw material in the field of fine chemicals such as drugs, solvents, surfactants, emulsifiers and lubricants due to its unique physical and chemical properties and reactivity, and its derivatives will definitely be used for the creation of new functional produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053C07C205/05C07C201/08
Inventor 罗和安刘平乐庄明晨刘四化游奎一艾秋红
Owner XIANGTAN UNIV
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