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Ni-Cu/Al2O3 bimetal catalyst and preparation method thereof, and application of Ni-Cu/Al2O3 bimetal catalyst in preparation of (tert-butylaminoethoxy)ethanol (TBEE)

A bimetallic catalyst, nickel salt technology, applied in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, etc., can solve the loss of active species, waste, increase in reaction cost, etc. problems, to achieve the effect of solving pollution problems, high reactivity, and high product yield

Inactive Publication Date: 2019-11-29
JILIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the reaction process, the loss of active species causes great waste, and the utilization rate of active components is low; (3) U.S. Patent US453452 uses halogenated alkanols and primary amines as raw materials for amination reaction, and there will be more halides, etc. in this reaction By-product formation, halides can seriously affect the service life of equipment
In the post-processing process, it is necessary to use lye to absorb halides to achieve the purpose of purification, and the reaction cost is significantly increased; (4) Chinese patent CN108906061A uses diethylene glycol and tert-butylamine as the reaction raw materials, and monometallic Ni is the active component to explore different carriers. Effect on reactivity
where Al 2 o 3 When used as a carrier, in a batch tank reactor, the best yield of the reaction can only reach 54.3%

Method used

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  • Ni-Cu/Al2O3 bimetal catalyst and preparation method thereof, and application of Ni-Cu/Al2O3 bimetal catalyst in preparation of (tert-butylaminoethoxy)ethanol (TBEE)
  • Ni-Cu/Al2O3 bimetal catalyst and preparation method thereof, and application of Ni-Cu/Al2O3 bimetal catalyst in preparation of (tert-butylaminoethoxy)ethanol (TBEE)
  • Ni-Cu/Al2O3 bimetal catalyst and preparation method thereof, and application of Ni-Cu/Al2O3 bimetal catalyst in preparation of (tert-butylaminoethoxy)ethanol (TBEE)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh 0.991g Ni(NO 3 ) 2 ·6H 2 O and 0.38g Cu(NO 3 ) 2 ·3H 2 O was dissolved in 40 mL of distilled water, and the mixed solution was placed on a rotary stirrer and stirred for 30 min to fully dissolve the solid. Weigh 2g of Al purchased from commercial channels 2 o 3 Carrier (amphoteric metaacid) was added to the above mixed solution, fully immersed for 2h. Afterwards, the excess impregnation solution was heated to 90° C., stirred and evaporated to dryness. The evaporated samples were dried in an oven at 100 °C for 12 h, and then calcined at 500 °C for 4 h in an air atmosphere in a muffle furnace to obtain the precursor of the catalyst. The catalyst precursor that takes by weighing 0.25g is in quartz tube, in 10% (volume fraction) H 2 10wt%Ni-5wt%Cu / Al was obtained by reduction at 500℃ for 2h in Ar atmosphere 2 o 3 catalyst. The catalyst after the reduction is lowered to room temperature, and used in a batch tank reactor to catalyze the reaction of diethylen...

Embodiment 2

[0019] Weigh 1.486g Ni(NO 3 ) 2 ·6H 2 O and 0.38g Cu(NO 3 ) 2 ·3H 2 O was dissolved in 40 mL of distilled water, and the mixed solution was placed on a rotary stirrer and stirred for 30 min to fully dissolve the solid. Weigh 2g of Al purchased from commercial channels 2 o 3 Carrier (amphoteric metaacid) was added to the above mixed solution, fully immersed for 2h. Afterwards, the excess impregnation solution was heated to 90° C., stirred and evaporated to dryness. The evaporated samples were dried in an oven at 100 °C for 12 h, and then calcined at 500 °C for 4 h in an air atmosphere in a muffle furnace to obtain the precursor of the catalyst. The catalyst precursor powder that takes 0.25g is in quartz tube, in 10% (volume fraction) H 2 15wt%Ni-5wt%Cu / Al was obtained by reduction at 500℃ for 2h in / Ar atmosphere 2 o 3 catalyst. The catalyst after the reduction is lowered to room temperature, and used in a batch tank reactor to catalyze the reaction of diethylene gl...

Embodiment 3

[0021] Weigh 0.495g Ni(NO 3 ) 2 ·6H 2 O and 1.14g Cu(NO 3 ) 2 ·3H 2 O was dissolved in 40 mL of distilled water, and the mixed solution was placed on a rotary stirrer and stirred for 30 min to fully dissolve the solid. Weigh 2g of Al purchased from commercial channels 2 o 3 The carrier (amphoteric metaacid) was added to the above mixed solution, fully immersed for 2h. Afterwards, the excess impregnating solution was heated to 90° C., stirred and evaporated to dryness. The evaporated samples were dried in an oven at 100 °C for 12 h, and then calcined at 500 °C for 4 h in an air atmosphere in a muffle furnace to obtain the precursor of the catalyst. The catalyst precursor powder that takes 0.25g is in quartz tube, in 10% (volume fraction) H 2 Reduction at 500℃ for 2h in / Ar atmosphere to obtain 5wt%Ni-15wt%Cu / Al 2 o3 catalyst. The catalyst after the reduction is lowered to room temperature, and used in a batch tank reactor to catalyze the reaction of diethylene glycol...

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Abstract

The invention provides a Ni-Cu / Al2O3 bimetal catalyst and a preparation method thereof, and application of the Ni-Cu / Al2O3 bimetal catalyst to catalysis of an amination reaction of diethylene glycol (DEG) with tert-butylamine (TBA) for preparation of the desulphurization solvent TBEE with severe steric-hinerance effect, belonging to the field of heterogeneous catalysis. The catalyst is composed ofa Ni-Cu bimetal active component and an Al2O3 carrier, wherein the loading amount of Ni accounts for 5 wt%-30 wt% of the mass of the carrier, and the loading amount of Cu accounts for 5 wt%-20 wt% ofthe mass of the carrier. The Ni-Cu / Al2O3 bimetal catalyst described in the invention has high reactivity and product yield in the synthesis of TBEE through the amination reaction of DEG with TBA; thepreparation cost of the catalyst is low; the catalyst can be produced on a large scale; in addition, the by-product DEG produced during the production of ethanol from ethylene oxide can be effectively used as a reaction raw material; meanwhile, the preparation method is of great significance to solving of environmental pollution caused by H2S emissions.

Description

technical field [0001] The invention belongs to the field of heterogeneous catalytic amination, in particular to a Ni-Cu / Al 2 o 3 Bimetallic catalyst, preparation method and application thereof in catalyzing the amination reaction of diethylene glycol and tert-butylamine to prepare desulfurization solvent tert-butylaminoethoxyethanol with serious steric hindrance effect. Background technique [0002] Tert-butylaminoethoxyethanol (TBEE) is a secondary aminoether alcohol with a strong steric hindrance effect, and is a particularly effective selective desulfurization solvent, widely used in petroleum, natural gas, oilfield associated gas, liquid hydrocarbons and synthesis gas selective desulfurization, especially in the treatment of highly acidic CO 2 / H 2 The desulfurization effect of S mixed gas is remarkable. TBEE vs H 2 The relative selectivity of S is methyldiethanolamine (MDEA) to H 2 3 times the relative selectivity of S. In the gas purification process, the energ...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J37/02B01J37/08B01J37/18C07C213/02C07C217/08
CPCB01J23/755B01J37/0201B01J37/088B01J37/18C07C213/02C07C217/08
Inventor 王振旅吴依凡张文祥朱万春
Owner JILIN UNIV
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