Apparatus and method for preparing nanomaterials by supercritical-solvothermal combination

A nanomaterial and supercritical technology, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problem of difficult to obtain pure products, difficult to remove reaction aids, cumbersome post-treatment processes, etc. problems, to achieve the effect of broad industrialization prospects, high production efficiency, and huge application potential

Inactive Publication Date: 2016-04-06
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the solvothermal method is a preparation reaction in an ordinary liquid phase environment, which is limited by conditions such as reaction pressure and solvent solubility. Although the process is relatively mature, various organic solvents are used in some preparation processes, and the post-treatment process is relatively complex. cumbersome, reaction aids (such as surfactants, etc.) are difficult to remove, and it is difficult to obtain pure products, so researchers are still working hard to find more favorable preparation methods

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  • Apparatus and method for preparing nanomaterials by supercritical-solvothermal combination

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Embodiment 1

[0050] When the raw material is completely soluble in the entrainer. Nanomaterials can be prepared following an example method of supercritical-solvothermal combination.

[0051] (1) Before the operation starts, install the sintering disc with microporous structure on the bottom of the cylindrical metal basket, and put the cylindrical metal basket into the reaction kettle A2; put the raw materials into the entrainer container CS and dissolve them in the entrainer , to form a homogeneous solution; then connect the pipeline, test the air tightness, and carry out the preparation operation;

[0052] (2) Close the valves K1-K5, the high-purity carbon dioxide in the cylinder C is first cooled by the carbon dioxide cooler H, and after reaching the temperature range required for supercritical conditions, it enters the carbon dioxide pump B and pressurized by the pump to make the carbon dioxide reach a supercritical state , and then controlled by the valve K1 to enter the subsequent r...

Embodiment 2

[0059] If the raw material is not completely soluble in the entrainer, but the target substance components in the raw material are soluble in the entrainer, nanomaterials can be prepared according to the example method of supercritical-solvothermal combination as follows.

[0060] (1) Before the operation starts, put the raw materials into the cylindrical metal basket, install the sintering plate with microporous structure at the bottom of the cylindrical metal basket, put the metal basket into the reaction kettle A1; connect the pipeline, test the gas Tightness, for preparation operations;

[0061] (2) Close the valves K1-K5, the high-purity carbon dioxide in the cylinder C is first cooled by the carbon dioxide cooler H, and after reaching the temperature range required for supercritical conditions, it enters the carbon dioxide pump B and pressurized by the pump to make the carbon dioxide reach a supercritical state , and then controlled by the valve K1 to enter the subsequen...

Embodiment 3

[0068] If the raw material is not soluble in the entrainer, nanomaterials can be prepared according to the example method of supercritical-solvothermal combination as follows.

[0069] (1) Before the operation starts, put the raw materials into the cylindrical metal basket, install the sintering plate with microporous structure at the bottom of the cylindrical metal basket, put the metal basket into the reaction kettle A2; connect the pipeline, test the gas Tightness, for preparation operations;

[0070] (2) Close the valves K1-K5, the high-purity carbon dioxide in the cylinder C is first cooled by the carbon dioxide cooler H, and after reaching the temperature range required for supercritical conditions, it enters the carbon dioxide pump B and pressurized by the pump to make the carbon dioxide reach a supercritical state , and then controlled by the valve K1 to enter the subsequent reaction process;

[0071] (3) The entrainer in the entrainer container CS is pressurized by t...

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Abstract

The invention discloses a supercritical-solvent heat combined device and a method for preparing a nanometer material. The device comprises a carbon dioxide steel bottle, a carbon dioxide cooler, a carbon dioxide pump, an entrainer accommodator, an entrainer pump, a first valve, a second valve, a third valve, a secondary reactor, a fourth valve, a main reactor, a fifth valve and a separator. The device can realize a plurality of supercritical-solvent heat combined preparation methods, and can satisfy the preparation of the nanometer material and the demands of controlling such crystal growth behaviors as crystal transfer, grain size and morphology evolution of an inorganic nanometer material through splicing pipelines and modules and adjusting such conditions or parameters as valve switch combinations, raw material placing mode and entrainer entering mode. The device has such advantages as simplicity and convenience for operation, wide adjusting range of experimental parameters, strong stability and high productivity, has huge application potential in the research, preparation and application fields of the nanometer material, and has wider industrialization foreground.

Description

technical field [0001] The general idea and design of the present invention relate to a supercritical device and technology, and more specifically, relate to a device and method for preparing nanomaterials by combining supercritical and solvothermal. Background technique [0002] In recent decades, nanomaterials have attracted extensive attention from researchers from various countries. This is because it has been found that when the size of the material reaches the nanometer level, it will have surface interface effects, small size effects, and quantum dimensions that traditional materials do not have. effect, macroscopic quantum tunneling effect and other nano-effects. These nanomaterials exhibit strange or abnormal photoelectric, physical, chemical and even biological properties that are different from atoms or molecules, and different from macroscopic materials, so they have extremely high potential application value. [0003] In the field of nanomaterial preparation te...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J3/04B82Y30/00B82Y40/00
Inventor 赵斌陈超王蒙何丹农
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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