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Core-shell structure thionazin composite microspheres and preparation method thereof

A core-shell structure and composite technology, which is applied in the field of synthesis of new catalytic materials, can solve the problems of sulfur loss of sulfide catalysts, and achieve the effects of good shape, reduced risk, and improved recycling rate

Pending Publication Date: 2017-04-26
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome the problem of high temperature required for the preparation of phosphide catalysts by traditional methods and the serious loss of sulfur faced by sulfide catalysts, the purpose of the present invention is to provide a method for preparing sulfur-phosphorus composite microspheres with a core-shell structure, which is mild and easy OK, the prepared core-shell structure sulfur-phosphorus composite microspheres (AS x @BP y ) show some potential application in catalysis

Method used

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  • Core-shell structure thionazin composite microspheres and preparation method thereof
  • Core-shell structure thionazin composite microspheres and preparation method thereof
  • Core-shell structure thionazin composite microspheres and preparation method thereof

Examples

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Embodiment 1

[0036] ZnS@Ni 2 Preparation of P-complex microspheres:

[0037] Step 1, prepare ZnS microspheres: 0.876g Zn(CH 3COO) 2 2H 2 O was dissolved in 60mL of deionized water. While stirring, 1.8mL of acetic acid and 6mmol of thiourea were added successively, and the stirring was continued until the solution was transparent and colorless. Then, the mixture solution was transferred to a hydrothermal reaction kettle and treated at 170°C for 8h. The resulting white precipitate was centrifuged with absolute ethanol and distilled water, washed several times, and dried in a vacuum oven at 60° C. for 6 hours to obtain white ZnS powder.

[0038] Step 2: Preparation of core-shell structure ZnS@Ni 2 P composite microspheres: Disperse 0.0585 g of the zinc sulfide powder prepared in step 1 into 18 mL of deionized water, and ultrasonically treat it for 20 min. Under magnetic stirring, sequentially add 0.0891g NiCl 2 ·6H 2 O, 0.0788g citric acid and 0.15g sodium dodecyl sulfate (SDS), after ...

Embodiment 2

[0041] ZnS@Ni 2 Preparation of P-complex microspheres:

[0042] In Example 1, the hydrothermal treatment temperature in step 1 was changed to 100°C, and the hydrothermal treatment time was changed to 2h; the hydrothermal treatment temperature in step 2 was changed to 100°C, and the hydrothermal treatment time was changed to 2h, and the obtained product was ZnS@Ni with inhomogeneous morphology. 2 P Composite Microspheres.

Embodiment 3

[0044] ZnS@Ni 2 Preparation of P-complex microspheres:

[0045] In Example 1, the hydrothermal treatment temperature in step 1 was changed to 220°C, and the hydrothermal treatment time was changed to 16h; the hydrothermal treatment temperature in step 2 was changed to 220°C, and the hydrothermal treatment time was changed to 20h, and the obtained product was ZnS@Ni with uniform morphology 2 P composite microspheres.

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Abstract

The invention discloses core-shell structure thionazin composite microspheres and a preparation method thereof. The structural formula is shown by ASx@BPy, wherein 0.3<=x<=2, and 0.3<=y<=4. The method comprises the steps that firstly, powdery sulfide microspheres ASx are prepared, then, ASx powder, soluble salt of B and nontoxic red phosphorus are adopted as main raw materials, the core-shell structure thionazin composite microspheres are prepared by adopting a hydrothermal synthesis method under the effect of a surface active agent sodium dodecyl sulfonate (SDS), and the preparation method adopts nontoxic red phosphorus as a phosphorus source to replace a traditional raw material, namely, highly toxic, inflammable and explosive white phosphorus. The preparation method is simple and easy to implement, conditions are easy to control, the repeatability is good, and no later-period thermal treatment is needed. The prepared core-shell structure thionazin composite is better in catalytic performance compared with a single sulfide and phosphide, and can be used for lignin hydrogenation catalysis and photocatalytic degradation of dye wastewater.

Description

technical field [0001] The invention belongs to the technical field of synthesis of novel catalytic materials, and in particular relates to a sulfur-phosphorus composite microsphere with a core-shell structure and a preparation method thereof. Background technique [0002] In recent years, transition metal phosphides, as a new type of catalytic material with high activity, high stability and resistance to sulfur poisoning, have attracted extensive attention due to their applications in many fields. Transition metal phosphides are a general term for covalent compounds formed by phosphorus and transition metals Fe, Co, Ni, Mo, and W. In 1996, Robinson et al. (J.Catal., 1996,161:539-550) first reported Ni 2 P is used for the hydrogenation reaction of quinoline. Li et al. (Chem. Lett., 1998, 3:207) prepared molybdenum phosphide in 1998 by a temperature-programmed reduction method, and found that it had good hydrodenitrogenation performance and stability. The temperature-progr...

Claims

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Application Information

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IPC IPC(8): B01J27/19B01J27/188B01J27/185B01J35/08B01J13/22B01J13/02
CPCB01J13/02B01J13/22B01J27/1853B01J27/188B01J27/19B01J35/51
Inventor 纪娜张晴黄艺博刁新勇王琪琪宋春风刘庆岭
Owner TIANJIN UNIV
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