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Catalyst for synthesis of indoxacarb intermediate and preparation method thereof

The technology of a catalyst and an intermediate is applied in the field of a catalyst for synthesizing an indoxacarb intermediate and its preparation, which can solve the problems of slow reaction speed, difficult to apply mechanically, and dechlorination, etc., to reduce the rate of activity decline, save costs, and improve production efficiency. Effect

Active Publication Date: 2018-02-13
GANNAN NORMAL UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The invention provides a catalyst (aminated palladium-carbon catalyst) for the synthesis of an indoxacarb intermediate and a preparation method thereof, the main purpose of which is to prepare YCW- 6 In the process, there are problems such as high dechlorination, slow reaction speed, and difficulty in applying mechanically. A method for improving the catalytic activity of palladium-carbon catalysts is provided, so that hydrogenation activity is high, target product selectivity and recycling stability are good. features

Method used

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  • Catalyst for synthesis of indoxacarb intermediate and preparation method thereof
  • Catalyst for synthesis of indoxacarb intermediate and preparation method thereof

Examples

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Embodiment 1

[0016] Step 1, the activated carbon is heated and refluxed with HNO3 with a mass concentration of 5% at a temperature of 80° C. for 4 hours, and then the activated carbon after heating and reflux is washed with deionized water to neutrality;

[0017] Step 2, prepare the activated carbon after washing in step 1 into a slurry, slowly add palladium salt aqueous solution with corresponding palladium quality dropwise according to the palladium loading capacity of 10%, fully stir evenly; immerse for 8h, adjust the pH value of the solution with sodium hydroxide solution to 10. Filter, wash the filter cake with deionized water until it is neutral; then prepare the filter cake with deionized water to prepare the liquid, and perform reduction according to the molar ratio of formic acid and palladium as the reducing agent of 3:1, filter, and wash with deionized water To neutrality, the palladium carbon precursor catalyst is obtained.

Embodiment 2

[0019] In a stainless steel autoclave with a volume of 500 mL, add 20 g of the palladium-carbon precursor catalyst prepared in Example 1, 1 mL of ethylenediamine, and 200 mL of methanol, control the temperature at 30 ° C, fill with hydrogen to a pressure of 0.5 MPa, and start stirring , reacted for 8h, cooled down, washed with 200mL methanol, and filtered to obtain the aminated palladium carbon catalyst.

Embodiment 3

[0021] In a 500mL stainless steel autoclave with a volume of 500mL, add 20g of the palladium-carbon precursor catalyst prepared in Example 1, 1mL of ethylenediamine, and 200mL of methanol, control the temperature at 80°C, fill with hydrogen to a pressure of 0.5MPa, and start stirring. React for 8 hours, cool down, wash with 200 mL of methanol, and filter to obtain the aminated palladium carbon catalyst.

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Abstract

The invention discloses a preparation method of a catalyst for synthesis of an indoxacarb intermediate. The method comprises the following steps: (1) processing activated carbon in 5% nitric acid for 4 hours in a water bath at 80 DEG C, washing with water to be neutral, and drying for 8h at 110 DEG C; (2) preparing the activated carbon into slurry, slowly dropwise adding a palladium salt solution with the corresponding palladium loading amount being 10%, stirring thoroughly and mixing evenly, soaking for 8h, adjusting the pH to 10 by using a sodium hydroxide solution, filtering, washing filter cake with deionized water to be neutral, preparing a slurry with the filter cake and the deionized water, reducing with the ratio of a reducing agent to the deionized water being 3 to 5:1, filtering, and washing with the deionized water to be neutral, thus obtaining a palladium-carbon precursor catalyst; and (3) putting the palladium-carbon precursor catalyst, ethylenediamine and a solvent into a reaction kettle, adjusting the reaction temperature, inflating a gas until a set pressure is reached, stirring, reacting for 8h, cooling to reduce the temperature, washing and filtering the solvent to obtain the aminated palladium-carbon catalyst.

Description

technical field [0001] The invention belongs to the technical field of preparation of precious metal catalysts, and in particular relates to a catalyst (aminated palladium-carbon catalyst) for synthesizing an indoxacarb intermediate and a preparation method thereof. Background technique [0002] Indoxacarb (Indoxacarb) is a new type of oxadiazine insecticide developed by DuPont Company of the United States in 1992. It has high insecticidal activity, good environmental compatibility, low toxicity to mammals, and is safe to birds, fish and beneficial insects. The advantages. It is one of the ideal varieties to replace highly toxic organophosphorus insecticides, and has become a research hotspot and a product that has received widespread attention. Due to the outstanding efficacy of indoxacarb, the research on its production process has also attracted the attention of researchers. There are many synthetic routes for indoxacarb, and the indoxacarb intermediate 2-(benzyl)-7-chl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24C07D273/04
CPCB01J27/24C07D273/04
Inventor 卢新宁李阳明高艳妮谢永荣郁丰善李永敏何治鸿相亚波程龙
Owner GANNAN NORMAL UNIV
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