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A kind of solid catalyst, its preparation method and application

A solid catalyst, catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve problems such as high cost and inability to mass production, and achieve cost Low, mild reaction conditions, high yield

Active Publication Date: 2017-11-07
JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Precious metals such as platinum, rhodium, palladium are mostly used in the existing technology to catalyze the reaction, and the cost is too high to be produced on a large scale. The yield and selectivity of -3-pyrazolyloxymethyl]aniline

Method used

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  • A kind of solid catalyst, its preparation method and application
  • A kind of solid catalyst, its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Weigh 2.42 grams of Cu(NO 3 ) 2 ·3H 2 O and 2.97 g of Zn(NO 3 ) 2 ·6H 2 Add O to a 50mL beaker, add 15mL deionized water to make a solution, add 5 grams of 40 mesh γ-Al 2 o 3 Carrier, magnetic stirring for 10 hours, suction filtration, filter residue vacuum drying for 12 hours, reduction and activation treatment at 500°C for 4 hours in a tube furnace with a mixed gas of 2g hydrogen and 1g nitrogen to prepare Cu-Zn / γ-Al 2 o 3 catalyst.

[0031] (2) 2.46 grams of Cu-Zn / γ-Al prepared in step 1 2 o 3 Add the catalyst to 150mL of 1,2-dichloroethane solution, stir at room temperature and slowly introduce 1.0g of hydrogen gas, stir and add 49.28g of compound I at 50°C, react for 5 hours and filter with suction, and the filtrate is passed through anhydrous sodium sulfate After drying, the solvent was distilled off under reduced pressure, and the obtained product was recrystallized to obtain 47.51 g of a light yellow solid, which was Compound II, with a yield of 98...

Embodiment 2

[0034] (1) Weigh 2.42 grams of Cu(NO 3 ) 2 ·3H 2 O and 5.94 g of Zn(NO 3 ) 2 ·6H 2 Add O to a 50mL beaker, add 20mL deionized water to make a solution, add 5 grams of 40 mesh γ-Al 2 o 3 Carrier, magnetically stirred for 15 hours, suction filtered, and the filter residue was vacuum-dried for 12 hours. Cu-Zn / γ-Al was prepared by reducing and activating at 500°C for 4 hours in a tube furnace with a mixed gas of 3g hydrogen and 1g nitrogen. 2 o 3 catalyst.

[0035] (2) 4.92 grams of Cu-Zn / γ-Al prepared in step 1 2 o 3 The catalyst was added to 150mL of 1,2-dichloroethane solution, stirred at room temperature and slowly introduced 6.8g of ammonia gas, stirred and added 49.28g of compound I at 50°C, reacted for 5 hours and filtered with suction, and the filtrate was passed through anhydrous sulfuric acid After sodium drying, the solvent was distilled off under reduced pressure, and the obtained product was recrystallized to obtain 47.56 g of light yellow solid, which was Com...

Embodiment 3

[0037] (1) Weigh 2.42 grams of Cu(NO 3 ) 2 ·3H 2 O and 8.91 g of Zn(NO 3 ) 2 ·6H 2 Add O into a 50mL beaker, add 25mL deionized water to make a solution, add 5 grams of 40 mesh γ-Al 2 o 3 Carrier, magnetically stirred for 20 hours, suction filtered, and the filter residue was vacuum-dried for 12 hours. Cu-Zn / γ-Al was prepared by reduction and activation treatment at 400°C for 4 hours in a tube furnace with a mixed gas of 1g hydrogen and 1g nitrogen. 2 o 3 catalyst.

[0038] (2) 7.38 grams of Cu-Zn / γ-Al prepared in step 1 2 o 3 Add the catalyst to 150mL of 1,2-dichloroethane solution, stir and add 49.28g of compound I and 7.5g of hydrazine hydrate at 50°C, react for 5 hours and then filter with suction, and the filtrate is dried over anhydrous sodium sulfate and distilled under reduced pressure The solvent was removed, and the obtained product was recrystallized to obtain 46.93 g of a light yellow solid, which was Compound II, with a yield of 97.5% and a purity of 98....

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Abstract

The present invention relates to a solid catalyst, its preparation method and the synthesis of pyraclostrobin intermediate N-hydroxyl-N-2-[(N-p-chlorophenyl)-3-pyrazolyloxymethyl]aniline For application in the method, the solid catalyst includes an active component and a carrier, the active component is copper and zinc, the carrier is γ-Al2O3, and the molar ratio of copper to zinc is 1:1-3. The self-made Cu-Zn / γ-Al2O3 catalyst is used to catalyze the reaction, the reaction conditions are mild, the yield of the product is about 98%, the cost is low, the three wastes are less, and it is suitable for industrial production.

Description

technical field [0001] The present invention relates to a solid catalyst, its preparation method and application, in particular to a pyraclostrobin intermediate N-hydroxyl-N-2-[(N-p-chlorophenyl)-3-pyrazolyloxymethyl Catalytic preparation method of base] aniline. Background technique [0002] Pyraclostrobin is a methoxyacrylate fungicide with a pyrazole structure. It has the advantages of high efficiency and low toxicity, wide bactericidal spectrum, and stable chemical properties. It has become a hot spot for domestic and foreign pesticide companies. It can be widely used in wheat, Peanuts, rice, fruit trees and other crops have strong control effects on powdery mildew, sheath blight, brown spot, gray mold, etc. [0003] N-Hydroxy-N-2-[(N-p-chlorophenyl)-3-pyrazolyloxymethyl]aniline is the key intermediate for the synthesis of pyraclostrobin, and its efficient synthesis is also The key steps of the whole synthetic route. Its structure is as follows: [0004] [0005] ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/80C07D231/22
Inventor 周炜陶亚春吴天宇何永利褚小静
Owner JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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