Preparation method of molybdenum disulfide-halloysite nano-tube composite material

A technology of halloysite nanotubes and molybdenum disulfide, which is applied in the field of composite materials, can solve the problems of complex preparation process, long reaction period and high energy consumption, and achieve the effects of good dispersion, improved morphology and large specific surface area.

Inactive Publication Date: 2018-09-21
HEBEI UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a preparation method of molybdenum disulfide-halloysite nanotube composite material, which uses molybdate, sulfide and halloysite nanotubes as raw materials to prepare molybdenum disulfide by using microwave hydrothermal method The molybdenum-hallosite nanotube composite material overcomes the existing technology of molybdenum disulfide composite material preparation, the molybdenum disulfide composite material is easy to re-aggregate or stack during the drying or annealing process, and the preparation process is complicated, the reaction cycle is long, and the energy consumption is low. High and costly defects

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  • Preparation method of molybdenum disulfide-halloysite nano-tube composite material

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Effect test

Embodiment 1

[0045] The first step is to prepare halloysite nanotubes:

[0046] Weigh the required amount of halloysite and 0.3mol / L HCl solution in a container according to the solid-liquid mass ratio of 1:3, mix them in a container, heat them in water at 60°C for 3 hours, then suction filter and wash with deionized water for 5 hours. Secondary to neutral, put the filter cake in an oven at 60°C to dry, then grind and pass through a 200-mesh sieve to obtain purified halloysite powder, add 0.3mol / L NaOH solution to the purified angstromite obtained above In the rockite powder, the mass ratio of solid to liquid was 1:10, ultrasonic treatment was carried out at a temperature of 50°C for 1 hour, and then suction filtration and washing were performed for 5 times until the pH value was neutral, and the obtained filter cake was placed in 60 Dry in an oven at ℃ for 10 hours, take out and grind and pass through a 200-mesh sieve to obtain halloysite nanotubes, which are set aside;

[0047] The seco...

Embodiment 2

[0054] The first step is to prepare halloysite nanotubes:

[0055] Weigh the required amount of halloysite and 2.6mol / L HCl solution in a container according to the solid-liquid mass ratio of 1:4, mix them in a container, heat them in water for 4 hours at a temperature of 70°C, and then filter them with suction and wash them with deionized water for 6 hours. Secondary to neutral, put the filter cake in an oven at 70°C to dry, then grind and pass through a 200-mesh sieve to obtain purified halloysite powder, add 3mol / L NaOH solution to the purified halloysite obtained above In the stone powder, the mass ratio of solid to liquid was 1:30, ultrasonic treatment was carried out at 60°C for 1.5h, and then suction filtration and washing 6 times until the pH value was neutral, and the obtained filter cake was placed in 70 Dry in an oven at ℃ for 11 hours, take out and grind and pass through a 200-mesh sieve to obtain halloysite nanotubes, which are set aside;

[0056] The second step...

Embodiment 3

[0063] The first step is to prepare halloysite nanotubes:

[0064] Weigh the required amount of halloysite and 5mol / L HCl solution according to the solid-liquid mass ratio of 1:5, mix them in a container, heat them in water at 80°C for 6 hours, then suction filter and wash with deionized water for 7 times To neutrality, place the filter cake in an oven at 80°C to dry, then grind and pass through a 200-mesh sieve to obtain purified halloysite powder, add 6mol / L NaOH solution to the purified halloysite obtained above In the powder, the mass ratio of solid to liquid is 1:50, ultrasonic treatment is carried out at a temperature of 70°C for 2 hours, then suction filtration and washing are carried out 7 times until the pH value is neutral, and the obtained filter cake is placed in an oven at 80°C Dry in medium for 12h, take out and grind and pass through a 200 mesh sieve to obtain halloysite nanotubes for subsequent use;

[0065] The second step is to prepare the reactant raw mater...

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Abstract

The invention provides a preparation method of a molybdenum disulfide-halloysite nano-tube composite material and relates to a composite material. The molybdenum disulfide-halloysite nano-tube composite material is prepared by a microwave hydrothermal method. The preparation method comprises the following steps: preparing a halloysite nano-tube; preparing a reactant raw material mixed liquid of molybdate, sulfide and the halloysite nano-tube; pouring the reactant raw material mixed liquid into a polytetrafluoroethylene reaction kettle, placing the polytetrafluoroethylene reaction kettle into microwave hydrothermal equipment and completing microwave hydrothermal effective composition of the reactants; and washing and drying the product obtained by the microwave hydrothermal method to prepare the molybdenum disulfide-halloysite nano-tube composite material. The defects in the prior art for preparing the molybdenum disulfide composite material that the molybdenum disulfide composite material is liable to gather or stack again in the drying or annealing process as well as the defects of complex preparation process, long reaction cycle, high energy consumption and high cost are overcome.

Description

technical field [0001] The technical solution of the invention relates to composite materials, specifically a method for preparing molybdenum disulfide-halloysite nanotube composite materials. Background technique [0002] Molybdenum disulfide is a typical layered transition metal sulfide. Every two layers of sulfur atoms sandwich a layer of molybdenum atoms, forming a typical sandwich structure. The molybdenum atom and the sulfur atom are covalently bonded, adjacent The two molecular layers are connected by relatively weak van der Waals force, and the intralayer interaction is strong while the interlayer interaction is relatively weak. Due to this special layered structure, molybdenum disulfide has good catalytic, lubricating and photoelectric properties, and is widely used in lithium ion battery electrodes and photocatalysis, solid lubrication, sensors, and field effect transistors. [0003] Molybdenum disulfide has high reactivity due to the unsaturation at the edge of i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06C01B33/40B82Y40/00
CPCB82Y40/00C01B33/40C01G39/06C01P2002/01C01P2004/13C01P2004/80
Inventor 王菲朱毛毛梁金生汤庆国崔丽
Owner HEBEI UNIV OF TECH
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