Synthetic method for halogenated aniline
一种合成方法、卤代苯胺的技术,应用在催化领域,能够解决易发生团聚、降低产品收率与品质、易被洗脱等问题,达到高活性及高选择性、提高收率与品质、适合保存与运输的效果
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[0072] The invention provides a kind of synthetic method of haloaniline, comprising:
[0073] The carbon-coated nickel nanocomposite is used as a catalyst to catalyze the hydrogenation reduction reaction of halonitrobenzene under a hydrogen atmosphere; the chemical reaction equation is illustrated as follows, wherein R represents one or more substituents on the benzene ring, and the At least one of the substituents is halogen:
[0074]
[0075] Wherein, the nanocomposite material contains a core-shell structure with a shell and an inner core, the shell layer is a graphitized carbon layer doped with nitrogen and oxygen, the inner core is nickel nanoparticles, and the nanocomposite material has at least A mesoporous material with a mesoporous distribution peak. That is to say, the nanocomposite material has at least one mesopore distribution peak on the pore distribution curve obtained by calculating the desorption curve according to the Barrett-Joyner-Halenda (BJH) method. ...
preparation example 1
[0108] (1) Weigh 10g of nickel acetate, 10g of citric acid, and 20g of hexamethylenetetramine, add them to a beaker containing 30mL of deionized water, stir at 70°C to obtain a homogeneous solution, and continue heating and evaporating to dryness Obtain a solid precursor. Tests have proved that the solid precursor obtained in this step is soluble in water.
[0109] (2) Put the precursor obtained in step (1) in the porcelain boat, then place the porcelain boat in the constant temperature zone of the tube furnace, feed nitrogen gas with a flow rate of 100mL / min, and raise the temperature at a rate of 5°C / min to 650°C, keep the temperature for 2 hours, stop heating, and cool to room temperature under nitrogen atmosphere to obtain a carbon-coated nickel nanocomposite material. The mass percentages of the elements contained in the nanocomposite are listed in Table 1 as measured by an elemental analyzer and an X-ray fluorescence spectrometer (XRF).
[0110] Characterization of the...
preparation example 2
[0115] (1) Weigh 10g of nickel acetate, 20g of citric acid, and 20g of hexamethylenetetramine, add them into a beaker containing 100mL of deionized water, stir at 80°C to obtain a homogeneous solution, and continue heating and evaporating to dryness to obtain solid precursor.
[0116] (2) Put the precursor obtained in step (1) in the porcelain boat, then place the porcelain boat in the constant temperature zone of the tube furnace, feed nitrogen gas with a flow rate of 150mL / min, and raise the temperature at a rate of 5°C / min to 600° C., keep the temperature for 2 hours, stop heating, and cool to room temperature under a nitrogen atmosphere to obtain carbon-coated nanomaterials. After being measured by an elemental analyzer and an X-ray fluorescence spectrometer (XRF), the mass percentages of the elements contained in the nanocomposite are listed in Table 1.
[0117] Material characterization: The nanocomposite material contains a core-shell structure with nano-metallic nicke...
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