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A kind of method that p-nitroanisole catalytic hydrogenation prepares p-aminoanisole

A technology for p-nitroanisole and p-aminoanisole is applied in the field of catalytic hydrogenation of p-nitroanisole to prepare p-aminoanisole, and can solve the problem of complex catalyst preparation process, high production cost and high equipment requirements problem, to achieve the effect of non-toxic and non-corrosive separation and reuse, low cost and simple post-processing

Active Publication Date: 2020-06-30
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The performance of the catalyst is excellent, and the yield of the product reaches 99%, but the catalyst is mainly composed of noble metal ruthenium, and the production cost is high; meanwhile, the preparation process of the catalyst is complicated, requires high equipment, and requires a large investment, making it difficult for industrial application
[0006] Throughout the above various reports, the prior art has not been able to realize the method for preparing p-aminoanisole with high selectivity and high yield on the scale of industrial production so far.

Method used

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  • A kind of method that p-nitroanisole catalytic hydrogenation prepares p-aminoanisole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1 (Ni-Cr / C-SiO 2 )

[0020] Weigh 20 g SiO 2 Add to 150 mL deionized water, stir for 2 h, and disperse evenly; weigh 0.37 g (0.9 mmol) of chromium nitrate nonahydrate, 0.26 g (0.9 mmol) of nickel nitrate hexahydrate, and 2.2 g (20 mmol) of resorcinol, Add 3.25 g (37wt.%) formaldehyde aqueous solution to the above solution, heat and stir in a water bath at 80 °C. Slowly add 1.7 mol / L Na 2 CO 3 50 mL of aqueous solution, stirred for 3 h, centrifuged the mixture, washed to neutral, moved to a drying oven for 4 h at 100 °C, and then dried under N 2 Calcination was carried out at 450 °C for 4 h under protective conditions, and finally the temperature was raised to 450 °C using a temperature-programmed reduction furnace at a hydrogen flow rate of 20 mL / min and a heating rate of 10 °C / min, and then lowered to room temperature after holding for 2 h to obtain catalyst A.

Embodiment 2

[0021] Embodiment 2 (Ni-Fe / C-Al 2 o 3 )

[0022] Weigh 20 g Al 2 o 3 Add to 150 mL deionized water, stir for 2 h, and disperse evenly; weigh 0.6 g (2 mmol) of nickel nitrate hexahydrate, 0.81 g (2 mmol) of iron nitrate nonahydrate, and 0.7 g (6.5 mmol) of resorcinol, 1.1 g (37 wt.%) formaldehyde aqueous solution was added to the above solution, heated and stirred in a water bath at 80 °C. Slowly add 1.7 mol / L Na 2 CO 3 50 mL of aqueous solution, stirred for 3 h, centrifuged the mixture, washed to neutral, moved to a drying oven for 4 h at 100 °C, and then dried under N 2 Calcination was carried out at 450 °C for 4 h under protective conditions, and finally the temperature was raised to 450 °C using a temperature-programmed reduction furnace at a hydrogen flow rate of 20 mL / min and a heating rate of 10 °C / min.

Embodiment 3

[0023] Embodiment 3 (Ni-Zn / C-Al 2 o 3 )

[0024] Weigh 20 g Al 2 o 3 Add to 150 mL deionized water, stir for 2 h, and disperse evenly; weigh 0.3 g (1 mmol) of nickel nitrate hexahydrate, 0.3 g (1 mmol) of zinc nitrate hexahydrate, and 2.2 g (20 mmol) of resorcinol, 3.25 g (37 wt.%) formaldehyde aqueous solution was added to the above solution, heated and stirred in a water bath at 80 °C. Slowly add 1.7 mol / L Na 2 CO 3 50 mL of aqueous solution, stirred for 3 h, centrifuged the mixture, washed to neutral, moved to a drying oven for 4 h at 100 °C, and then dried under N 2 Calcination was carried out at 450 °C for 4 h under protected conditions, and finally the temperature was raised to 450 °C using a temperature-programmed reduction furnace at a hydrogen flow rate of 20 mL / min and a heating rate of 10 °C / min, and then lowered to room temperature after holding for 2 h to obtain catalyst C.

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Abstract

The invention discloses a method for preparing p-anisidine through catalytic hydrogenation of p-nitroanisole. According to the method, p-nitroanisole is used as a reaction raw material and subjected to a reaction in an enclosed reactor with a mechanical stirring function under the conditions of usage of a composite catalyst, no usage of a solvent, a reaction temperature of 80 to 150 DEG C and hydrogen pressure of 0.3 to 1 MPa so as to obtain p-anisidine, wherein the composite catalyst is composed of active components metal M and a carrier; the active components metal M are composed of two or more selected from a group consisting of Cu, Ni, Fe, Zn, Co, Cr and Mo, and the content of the active components metal M accounts for 0.3 to 25 wt% of the mass of the composite catalyst; and the carrier is prepared by compounding a carbon-containing organic matter and an inorganic oxide, a mass ratio of the carbon-containing organic matter to the inorganic oxide is 1: 50 to 1: 10, and the inorganicoxide is any one selected from a group consisting of SiO2, Al2O3, MgO, TiO2, CeO2 and a 4A molecular sieve. The composite catalyst used in the invention has high catalytic activity, stable performance and high selectivity and conversion rate.

Description

technical field [0001] The invention relates to a method for preparing p-aminoanisole by heterogeneous catalytic hydrogenation of p-nitroanisole. Background technique [0002] P-aminoanisole, also known as p-methoxyaniline or p-anisidine, is a traditional fine chemical widely used in pharmaceutical intermediates, photographic materials, agricultural chemicals, polymers, dyes and other fields. According to incomplete statistics, my country is the main producer and supplier of p-aminoanisole in the world, and the output of p-aminoanisole accounts for about 80% of the global output. At present, the traditional industrial production method of producing p-aminoanisole through p-nitroanisole in China is to adopt the soda sulfide method or the iron powder reduction method. However, the above two methods have many problems such as high energy consumption, high input cost, low conversion rate and selectivity, a large amount of waste residue, and serious environmental pollution by wa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/02C07C217/84B01J23/755B01J23/78B01J23/80B01J23/83B01J23/86B01J23/883B01J23/887B01J29/72B01J37/03B01J37/08B01J37/18
CPCB01J23/755B01J23/78B01J23/80B01J23/83B01J23/866B01J23/868B01J23/883B01J23/8872B01J23/8878B01J29/7207B01J37/031B01J37/084B01J37/18C07C213/02C07C217/84
Inventor 黄永吉袁航空王红利石峰
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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