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A kind of method utilizing diazoamide hydrazone pyridine derivatives to adsorb and separate palladium

A technology for diazamide hydrazone pyridine and adsorption separation, applied in the direction of improving process efficiency, etc., can solve the problem of lack of simple and feasible methods for palladium recovery and separation, and achieve the effects of high selectivity, high separation efficiency and simple operation

Inactive Publication Date: 2018-02-23
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In the prior art, there is still a lack of simple and feasible methods for the recovery and separation of palladium

Method used

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  • A kind of method utilizing diazoamide hydrazone pyridine derivatives to adsorb and separate palladium
  • A kind of method utilizing diazoamide hydrazone pyridine derivatives to adsorb and separate palladium
  • A kind of method utilizing diazoamide hydrazone pyridine derivatives to adsorb and separate palladium

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Experimental program
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Effect test

Embodiment 1

[0033] The synthetic route of the present embodiment is as follows:

[0034]

[0035] The synthetic steps of the present embodiment include:

[0036] (1) Dissolve 2.6g of monopyridineamine hydrazone (i.e. compound 2) and 5.0mL of triethylamine in 300.0mL of ethanol, place in a 500.0mL three-necked flask to form a suspension and stir;

[0037] (2) Fully dissolve 5.0g camphorquinone (i.e. compound 1) in 50.0mL ethanol;

[0038] (3) Utilize the constant pressure funnel to drop the camphorquinone solution into the suspension in step (1) to react, the dropping process lasts 60 minutes, then stir and reflux for 8 days, utilize TLC (thin-layer chromatography analysis) to track the reaction until the raw material Stop when the reaction is complete.

[0039] (4) After the reaction stops, after the golden yellow reaction liquid is cooled to room temperature, filter through a sand core funnel to remove solid impurities, and the filtrate is rotary evaporated under reduced pressure to...

Embodiment 2

[0050]Dissolve 0.5g of the compound (CA-MTP) shown in structural formula II in 45.0mL of dichloromethane, mix uniformly to obtain a golden yellow solution; add 4.5g of ion exchange resin XAD-7 material to this golden yellow solution and stir evenly, And use a rotary evaporator to evaporate dichloromethane under reduced pressure to volatilize the material to a near-dry state, and then vacuum-dry the near-dry material at 55°C for 24 hours to obtain a CA-MTP / XAD-7 composite material , the adsorbent.

Embodiment 3

[0052] Dissolve 0.5g of the compound (CA-MTP) shown in structural formula II in 40.0mL of dichloromethane, mix well to obtain a golden yellow solution; add 4.0g of ion exchange resin XAD-7 material to this golden yellow solution and stir evenly, And use a rotary evaporator to evaporate dichloromethane under reduced pressure to volatilize the material to a near-dry state, and then vacuum-dry the near-dry material at 50°C for 24 hours to obtain a CA-MTP / XAD-7 composite material , the adsorbent.

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PUM

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Abstract

The invention discloses a method for adsorbing and separating palladium through dinitrogen amide hydrazone pyridine derivatives. The method includes the following steps that adsorbents and a nitric acid aqueous solution containing various kinds of metal ions are mixed; the palladium ions in the nitric acid aqueous solution are adsorbed and separated by the adsorbents, and the adsorbents are made by loading a chemical compound shown as the structural formula I on a carrier; every gram of adsorbents is mixed with 20-30 ml of the nitric acid aqueous solution; the carrier is weak-polar macroporous resin; according to the nitric acid aqueous solution, the concentration of nitric acid is 0.4-6 M; and the concentration of each kind of metal ions is 5.0*10<-4>-1.0*10<-3> M. By means of the method for adsorbing and separating the palladium through the dinitrogen amide hydrazone pyridine derivatives, the palladium can be separated from an acidic water phase, selectivity is high, operation is simple, separation efficiency is high, and the method is suitable for separating and recycling the precious metal palladium industrially.

Description

technical field [0001] The invention relates to the technical field of element separation, in particular to a method for adsorbing and separating palladium by using diazamide hydrazone pyridine derivatives. Background technique [0002] The precious metal palladium has a special structure and has a special adsorption capacity for hydrogen and oxygen, so it occupies an irreplaceable position in the field of industrial catalysis. [0003] In addition to its excellent catalytic activity, palladium can maintain chemical inertness in a wide temperature range and has the characteristics of high melting point, friction resistance, corrosion resistance, strong ductility, and strong thermoelectric stability. It is widely used in national industries. each field. [0004] At present, my country's palladium resource reserves are limited and the output is very low, which is far from meeting the needs of the modern chemical industry. Most of them rely on imports and are expensive. In th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B7/00C22B11/00
CPCC22B7/006C22B11/042Y02P10/20
Inventor 张安运徐雷
Owner ZHEJIANG UNIV