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Modified aluminium oxide microsphere, and preparation method and application thereof

A kind of alumina, modification technology, applied in the field of chemistry, can solve the problem of difficult to access research results and so on

Active Publication Date: 2016-02-17
NUCLEAR POWER INSTITUTE OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The separation of element molybdenum in the element core after irradiation has not been studied in China before, and it is difficult to find foreign research results in this area in public literature reports

Method used

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  • Modified aluminium oxide microsphere, and preparation method and application thereof
  • Modified aluminium oxide microsphere, and preparation method and application thereof
  • Modified aluminium oxide microsphere, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A preparation method of modified alumina microspheres, adding 1~3mLtween-80, 1~3mLspan-80 and 1~3mL n-heptanol to 15-20mL n-heptane successively under stirring and heating conditions, and then adding 100 -120mL of 2.5-4.5mol / L aluminum nitrate solution, stirred at 50-70°C for a period of time, then added 180-200mL of 1mol / L ammonia water dropwise, and continued to stir at 50-70°C for 1-3h Cool and filter to obtain colloidal precipitation, wash, dry, burn, cool, vibrate, and then filter and dry.

Embodiment 2

[0022] A preparation method of modified alumina microspheres, adding 1~3mLtween-80, 1~3mLspan-80 and 1~3mL n-heptanol to 15-20mL n-heptane successively under stirring and heating conditions, and then adding 100 -120mL of 2.5-4.5mol / L aluminum nitrate solution, stirred at 50-70°C for a period of time, then added 180-200mL of 1mol / L ammonia water dropwise, and continued to stir at 50-70°C for 1-3h Cool and filter to obtain colloidal precipitates, wash the colloidal precipitates with petroleum ether, acetone, ethanol and high-purity water, then dry and burn (burning temperature is 300-800°C, burning time is 0.5-1h, cool, shake, Then filter and dry.

[0023] The general oscillation method can be used for oscillation, such as ultrasonic oscillation. If ultrasonic oscillation is used, a small amount of high-purity water should be added before operation. The function of the vibration is to completely disperse the alumina microspheres.

[0024] Table 1 shows the comparison of the sp...

Embodiment 3

[0027] The application of a modified alumina microsphere as a chromatographic column filler to separate, measure and recover molybdenum in the spent fuel element sample solution, specifically as a chromatographic column filler using reversed-phase chromatography, reversed-phase ion pair The three-column method combining chromatography and inorganic ion exchange method is used to separate, measure and recover molybdenum in spent fuel element sample solution.

[0028] The modified alumina microspheres are all injected into the chromatographic column in advance, and the sample is injected into the quantitative tube of the chromatographic sampling valve. After manual sampling, the eluent E 1 The sample flows into the first chromatographic column under the impetus of the chromatographic column. Due to the different interactions between the chromatographic column and the components in the sample, the retention time is significantly different. The rare earth and other fissile elements...

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Abstract

The invention discloses a modified aluminium oxide microsphere, and a preparation method and application thereof. The modified aluminium oxide microsphere possesses the specific surface area of 207.88 m<2> / g, and the adsorption accumulated total pore volume or desorption accumulated total pore volume of 0.51 cm<3> / g. The preparation method comprises successively adding tween-80, span-80 and heptan-1-ol into n-heptane under the conditions of stirring and heating, then adding an aluminium nitrate solution, stirring at a constant temperature of 50-70 DEG C for a period, adding ammonia water with the concentration of 1 mol / L drop by drop, continuing to stir at a constant temperature of 50-70 DEG C for 1-3 h, cooling and filtering to obtain a colloidal precipitate, and performing cleaning, drying, calcination, cooling and oscillation, and then performing filtering and drying, so as to obtain the modified aluminium oxide microsphere. Compared with an aluminium oxide microsphere prepared through a traditional method, the aluminium oxide microsphere prepared according to the disclosed preparation method possesses the specific surface area larger by about 18%, and possesses the total pore volume larger by about 25%, and is successfully applicable to separation of uranium, molybdenum and neodymium in spent fuel elements.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a modified alumina microsphere and a preparation method and application thereof. Background technique [0002] The traditional method of preparing alumina microspheres is the sol-gel method. The specific preparation process is to directly add aluminum nitrate solution, cool and filter after aging, and then wash several times with alcohol-water mixture, and then dry and burn. Finally, blocky and large and irregular granular alumina can be obtained, which can be ground and sieved to 60-100 meshes. The alumina microspheres obtained by this method are large and irregular in shape, so that their specific surface area and pore volume are relatively small. Even if they are barely used, they need to go through time-consuming and laborious processes such as grinding, which cannot meet actual needs. [0003] In addition, the current separation of molybdenum mainly includes α-benzoin-deficient pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/08B01J20/30B01J20/282B01J20/28G21F9/12G21F9/06
CPCB01J20/08B01J20/28002B01J20/28019B01J20/28021B01J20/28061B01J20/28073B01J20/282B01J20/305B01J20/3071B01J20/3078B01J20/3085B01J2220/52B01J2220/60B01J2220/86G21F9/06G21F9/12
Inventor 张劲松李兵陈云明黄立娟胡银李新政杨彬刘琢艺
Owner NUCLEAR POWER INSTITUTE OF CHINA
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