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Method for preparing tantalum (Ta)-doped wolfram (W)-oxide adsorption nano-material

A nano-tungsten oxide, adsorption material technology, applied in chemical instruments and methods, radioactive purification, other chemical processes, etc., can solve the problems of easy extraction, difficult introduction of transition metal ions, difficult control and improvement of pore channels and pore shapes, etc. To achieve the effect of smooth pores, stable physical and chemical properties, and maintaining stability

Inactive Publication Date: 2015-03-04
INST OF NUCLEAR PHYSICS & CHEM CHINA ACADEMY OF
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The interconnected channels and cavities in the skeleton make the zeolite have a large internal surface area, especially when the "zeolite water" escapes, the channels and voids are more open, and the corresponding internal surface area is even larger (the porosity can reach more than 50%, and the pores or voids Cavity diameter is generally between 0.6-1.5nm), however, in the traditional tetrahedral framework molecular sieve, there are shortcomings of transition metal ions difficult to introduce and easy to extract, and it is difficult to control and improve its channel and pore type

Method used

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  • Method for preparing tantalum (Ta)-doped wolfram (W)-oxide adsorption nano-material

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Weigh 7 parts of sodium tungstate (NaWO 4 2H 2 O) Place in a polytetrafluoroethylene reactor, add 7 parts of double distilled water, stir to make it fully dissolved, add 7 parts of tantalum pentachloride ethanol solution with a concentration of 0.05mol / L, and make the solution Ta / W molar ratio 0.01 Continue stirring to make it fully mixed, then add 7 parts of 3mol / L hydrochloric acid solution and 7 parts of 0.5mol / L ammonium sulfate solution, stir for 0.5h, seal the polytetrafluoroethylene reaction kettle, place it in a programmed oven, and set the temperature to rise And the cooling rate is 1°C / min, hydrothermal treatment at a temperature of 170°C for 48h. Take out the reactor and cool to room temperature. Wash the reaction products with distilled water until neutral, and then freeze-dry them in a freeze dryer at a temperature of -40°C. Obtain tantalum doped hex-WO3 nanomaterials.

Embodiment 2

[0044] Weigh 10 parts of sodium tungstate (NaWO 4 2H 2 O) Put it in a polytetrafluoroethylene reactor, add 10 parts of secondary distillation, stir to make it fully dissolved, add 10 parts of tantalum pentachloride ethanol solution with a concentration of 0.05mol / L, and make the mole of Ta / W in the solution The ratio is 0.18, continue stirring to make it fully mixed, then add 10 parts of 2mol / L hydrochloric acid solution and 10 parts of 0.4mol / L ammonium sulfate solution, stir for 1h, seal the polytetrafluoroethylene reaction kettle, and place it in a programmed oven. Set the heating and cooling rate to 1°C / min, and conduct hydrothermal treatment at 200°C for 24 hours. After the reaction is completed, take out the reactor and cool to room temperature. Wash the reaction products with distilled water until neutral, and then freeze at -40°C Freeze drying in a dryer to obtain tantalum doped hex-WO 3 nanomaterials.

Embodiment 3

[0046] Weigh 8 parts of sodium tungstate (NaWO 4 2H 2 O) Put it in a polytetrafluoroethylene reaction kettle, add 8 parts of double distilled water, stir to make it fully dissolved, add 8 parts of tantalum pentachloride ethanol solution with a concentration of 0.05mol / L, and make the mole of Ta / W in the solution The ratio is 0.05, continue to stir to make it fully mixed, then add 8 parts of 3mol / L hydrochloric acid solution and 0.5mol L -1 8 parts of ammonium sulfate solution, stirred for 0.8h, sealed the polytetrafluoroethylene reaction kettle, placed in a programmed oven, set the heating and cooling rate to 1°C / min, and hydrothermally treated at a temperature of 175°C for 40h. After the reaction was completed, the reaction kettle was taken out , cooled to room temperature. The reaction products were washed with distilled water until neutral, and then placed in a freeze-dryer at a temperature of -40°C to obtain tantalum-doped hex-WO 3 nanomaterials.

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Abstract

The invention discloses a method for preparing a tantalum (Ta)-doped wolfram (W)-oxide adsorption nano-material. The method is characterized by comprising the following steps: weighing 7-10 parts by weight of sodium wolframate, putting the sodium wolframate into a polytetrafluoroethylene (PTFE) reaction kettle, and adding 7-10 parts of secondary distilled water so as to thoroughly dissolve the sodium wolframate; adding different volumes of tantalum-pentachloride ethanol solutions with the concentration of 0.05mol / L, so as to enable the Ta / W molar ratio of a solution to be 0.01-0.18, and mixing thoroughly; adding 7-10 parts of hydrochloric solution with the concentration of 2-3mol / L and 7-10 parts of ammonium sulfate solution with the concentration of 0.4-0.5mol / L into the PTFE reaction kettle, and stirring for 0.5-1 hour; sealing the PTFE reaction kettle, putting the PTFE reaction kettle into a programmed baking oven, respectively controlling the heating and cooling rates to be 1-2 DEG C / min, carrying out hydrothermal treatment for 24-48 hours at the temperature of 170-200 DEG C, taking out the reaction kettle, cooling to room temperature, washing a reaction product by using distilled water until the reaction product is neutral, putting the reaction product in a freeze drier with the temperature of -40 DEG C, and carrying out freeze drying for 24-48 hours, thereby obtaining the Ta-doped hexagonal-phase wolfram-oxide nano-material.

Description

technical field [0001] The invention relates to a preparation method of a tantalum-doped nano-tungsten oxide adsorption material, belonging to the technical field of inorganic functional materials. Background technique [0002] 90 Sr is an important heat-releasing nuclide in the split solution. If it can be separated, the cost of subsequent treatment of radioactive waste can be greatly reduced. 90 Sr is a very challenging work (Zhang et al. in Isotope, 2009, 22(4): 237-246). Inorganic materials are often used in the treatment of radioactive waste liquid due to their advantages of high temperature resistance, radiation resistance, easy column packing, and relatively simple operation process. Among them, zeolite porous inorganic materials are widely used low-level waste liquid treatment materials. From the structural point of view, zeolite is a kind of [SiO 4 ] 4- and [AlO 4 ] 5- Aluminosilicate skeleton compound composed of tetrahedrons. The interconnected channels and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/06B01J20/30B01J39/10G21F9/12
Inventor 牟婉君李兴亮唐惠马宗平周官宏魏洪源蹇源罗顺忠
Owner INST OF NUCLEAR PHYSICS & CHEM CHINA ACADEMY OF
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