A kind of preparation method and application of dithiocarbamate iron complex catalyst

A technology of dithiocarbamate and dimethyldithiocarbamate is applied in the field of preparation of iron dithiocarbamate complex catalysts, which can solve problems such as poor recycling performance and achieve low pollution and high catalytic activity. , the effect of high yield

Active Publication Date: 2022-03-04
陕西中杰科仪化学科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a catalyst, under the condition of neutral solution, ferric chloride is prone to be hydrolyzed to form precipitates and inactivated, and the recycling performance is poor.

Method used

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  • A kind of preparation method and application of dithiocarbamate iron complex catalyst
  • A kind of preparation method and application of dithiocarbamate iron complex catalyst
  • A kind of preparation method and application of dithiocarbamate iron complex catalyst

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Experimental program
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Effect test

Embodiment 1

[0019] Take by weighing 1.0mmol, the ferrous ammonium sulfate (NH 4 ) 2 Fe(SO 4 ) 2 ·6H 2 O and 3.0mmol, 0.363g of N,N-dimethyldithiocarbamate, placed in a round bottom flask, add 10mL of distilled water, 5.0mL of ethanol and 1.0mL of DMF, stir at room temperature for 10min, adjust the pH of the solution with ammonia water The value is 5, and the mixture solution is obtained. The mixture solution is transferred to a stainless steel reactor at 130 ° C for 72 hours, naturally cooled to room temperature, and separated by filtration to obtain a reddish-brown block crystal, which is an iron dithiocarbamate complex. Yield 93%. The prepared iron complex was used as the catalyst for the Hantzsch reaction, and the reaction raw materials of ethyl acetoacetate, 3-cyanobenzaldehyde and ammonium acetate were carried out in a mixed solvent with a volume ratio of ethanol and water of 1:1, and the catalytic reaction experiment was carried out And catalyst recycling experiment test.

Embodiment 2

[0021] Take by weighing 1.0mmol, the ferrous ammonium sulfate (NH 4 ) 2 Fe(SO 4 ) 2 ·6H 2 O and 3.0mmol, 0.363g of N,N-dimethyldithiocarbamate, placed in a round bottom flask, add 10mL of distilled water, 5.0mL of ethanol and 1.0mL of DMF, stir at room temperature for 10min, adjust the pH of the solution with ammonia water The value is 6, and the mixture solution is obtained. The mixture solution is transferred to a stainless steel reactor at 160 ° C for 24 hours, naturally cooled to room temperature, and separated by filtration to obtain a reddish-brown block crystal, which is an iron dithiocarbamate complex. Yield 90.5%. The prepared iron complex was used as the catalyst for the Hantzsch reaction, and the reaction raw materials of ethyl acetoacetate, 3-cyanobenzaldehyde and ammonium acetate were carried out in a mixed solvent with a volume ratio of ethanol and water of 1:1, and the catalytic reaction experiment was carried out And catalyst recycling experiment test.

Embodiment 3

[0023] Take by weighing 1.0mmol, the ferrous ammonium sulfate (NH 4 ) 2 Fe(SO 4 ) 2 ·6H 2 O and 3.0mmol, 0.363g of N,N-dimethyldithiocarbamate, placed in a round bottom flask, add 10mL of distilled water, 5.0mL of ethanol and 1.0mL of DMF, stir at room temperature for 10min, adjust the pH of the solution with ammonia water The value was 5.5, and the mixture solution was obtained. The mixture solution was transferred to a stainless steel reactor at 140 ° C for 48 hours, cooled to room temperature naturally, filtered and separated to obtain a reddish-brown block crystal, which was an iron dithiocarbamate complex. Yield 92%.

[0024] Select the reddish-brown block crystal that makes in the above-mentioned embodiment that size is suitable to carry out X-ray single-crystal diffraction test analysis, after determination asymmetric structure unit is by an Fe (III) ion and three dithiocarbamate radicals (L - ) composition, its structural formula is [Fe(L) 3 ], the crystal system...

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Abstract

The invention discloses a preparation method and application of an iron dithiocarbamate complex catalyst. The iron dithiocarbamate complex comprises ferrous ammonium sulfate and N,N-dimethyldithiocarbamate ligands. As raw material, distilled water, ethanol and DMF are used as solvents, and it is prepared by solvothermal reaction; the prepared iron complex is used as a catalyst of Hantzsch, with high catalytic activity and can be recycled for many times; the solvent of the catalytic reaction is water and ethanol, which pollutes The iron complex has broad application prospects in the fields of biomedical synthesis and catalytic materials as a catalyst. The invention has mild reaction conditions, low cost, low equipment investment, and is suitable for mass production.

Description

technical field [0001] The invention belongs to the field of coordination chemistry, and in particular relates to a preparation method and application of an iron dithiocarbamate complex catalyst. Background technique [0002] Complexes generally refer to a class of compounds formed by atoms or ions of transition metals and ligand molecules containing lone pairs of electrons through coordination bonds. Complexes are widely used in daily life, industrial production and life sciences, and the development has been particularly rapid in recent years. In industrial production, the complex can be used for coordination catalysis, for example, copper diammonium acetate is used to remove CO in the ammonia synthesis industry, and organometallic catalysts catalyze the polymerization or oligomerization of olefins. [0003] N,N-Dimethyldithiocarbamate has strong coordination ability and can form structurally stable complexes with many transition metals. N,N-Dimethyl dithiocarbamate iron...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C333/16B01J31/22C07D211/02C07D211/90
CPCC07C333/16B01J31/226C07D211/02C07D211/90B01J2531/842B01J2531/0238Y02P20/584
Inventor 李星宫士超
Owner 陕西中杰科仪化学科技有限公司
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