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Synthetic method of amino-anisole compound

An aminoanisole and a synthesis method technology, applied in the field of catalysis, can solve the problems of easy agglomeration, great environmental damage, easy to be eluted, etc., and achieve the effects of being suitable for storage and transportation, good catalytic performance, and good repeatability

Inactive Publication Date: 2020-07-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Pt and Pd noble metal catalysts have the advantages of high catalytic activity and mild reaction conditions, but the price and cost of noble metal catalysts are too high, and the loss of noble metals is harmful to the environment, so their application in industrial production is limited.
Non-precious metal catalysts, such as nickel, also have a series of problems in actual production and application, for example, they are prone to agglomeration during the preparation process, easy to be eluted during the catalytic hydrogenation process, poor stability, and greater safety hazards, etc.

Method used

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  • Synthetic method of amino-anisole compound
  • Synthetic method of amino-anisole compound
  • Synthetic method of amino-anisole compound

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preparation example Construction

[0055] The invention provides a method for synthesizing aminoanisole compounds, comprising: using carbon-coated nickel nanocomposites containing alkaline earth metals as a catalyst, and catalyzing nitroanisole compounds for hydrogenation reduction reaction in a hydrogen atmosphere ; The chemical reaction equation is illustrated as follows,

[0056]

[0057] Wherein, the nanocomposite material has a core-shell structure with a shell and an inner core, the shell is a graphitized carbon layer containing alkaline earth metals, nitrogen and oxygen, and the inner core is nickel nanoparticles.

[0058] In some embodiments, the benzene ring of the nitroanisole compound also contains a substituent, and the substituent R is selected from C 1-20 One or more of the alkyl, cycloalkyl and aryl groups, the above-mentioned substitutions can be mono-substituted or multi-substituted, such as p-nitroanisole, m-nitroanisole or 3-methyl -4-Nitroanisole.

[0059] In some embodiments, the catal...

preparation example 1

[0095] (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.

[0096] (2) Place the solid precursor obtained in step (1) in a 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 set the temperature at a rate of 5°C / min. Raise the temperature to 650°C, stop the heating after keeping the temperature for 2 hours, and cool to room temperature under a nitrogen atmosphere to obtain a carbon-coated nickel material.

[0097] (3) Weigh 2g of the carbon-coated nickel material obtained in step (2), add 4mL of an aqueous solution containing 0.5128g of magnesium nitrate, soak for 24h, and then dry...

preparation example 2

[0104] (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.

[0105] (2) Place the solid precursor obtained in step (1) in a porcelain boat, then place the porcelain boat in the constant temperature zone of the tube furnace, feed in nitrogen gas with a flow rate of 150mL / min, and heat at a rate of 5°C / min. The temperature was raised to 600°C, the temperature was kept constant for 2 hours, the heating was stopped, and the carbon-coated nickel material was obtained by cooling to room temperature under a nitrogen atmosphere.

[0106] (3) Weigh 2 g of the carbon-coated nickel material obtained in step (2), add 4 mL of an aqueous magnesium nitrate solution containing 0.8589 g, impregnate for 24 h, and then dry at 120° C.

[0107] (4) The dried material obtained in ste...

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Abstract

The invention provides a synthesis method of an amino-anisole compound. The synthesis method comprises the following steps: taking a carbon-coated nickel nano composite material containing alkaline-earth metals as a catalyst, and catalyzing a hydrogenation reduction reaction of a nitro-anisole compound in a hydrogen atmosphere; wherein the nano composite material contains a core-shell structure with a shell layer and an inner core, the shell layer is a graphitized carbon layer containing alkaline-earth metals, nitrogen and oxygen, and the inner core is nickel nano particles. According to the method, the nano composite material is used as a catalyst; a carbon material and the nickel nano particles generate a synergistic effect and a good catalytic effect, the alkaline-earth metals of the shell layer further synergistically improve the catalytic performance of the nano composite material, and the catalyst is used for hydrogenation reduction of nitro-anisole compounds to synthesize amino-anisole compounds and has excellent activity, selectivity and safety.

Description

technical field [0001] The invention relates to the field of catalysis, in particular to a method for synthesizing aminoanisole compounds. Background technique [0002] Aminoanisole compounds can be widely used in the dye industry, pharmaceutical industry and perfume intermediates. Its traditional industrial production method is chemical reduction method, which is usually obtained by reducing nitroanisole with iron powder or sodium sulfide. The method is simple in process, but has the disadvantages of heavy pollution of three wastes, high cost and poor quality. Compared with the chemical reduction method, the catalytic hydrogenation reduction method has attracted much attention due to its advantages of good product quality, high yield, and simple process, and is an environmentally friendly green process. [0003] The catalysts currently used to catalyze the hydrogenation of nitroanisole are mainly noble metal catalysts such as platinum (Pt), palladium (Pd) and rhodium (Rh)...

Claims

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Application Information

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IPC IPC(8): C07C217/84C07C213/02B01J27/24B01J35/10
CPCC07C213/02B01J27/24B01J35/398B01J35/33B01J35/615B01J35/633B01J35/69B01J35/647C07C217/84
Inventor 宗明生谢婧新荣峻峰于鹏吴耿煌林伟国纪洪波
Owner CHINA PETROLEUM & CHEM CORP
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