Preparing method of particle caesium removing inorganic ion adsorbent and product and application

An inorganic ion and adsorbent technology, which is applied in the field of material preparation and radioactive wastewater treatment, can solve the problems of reduced adsorbent performance, large particle size of silica gel balls, and difficulty in complete ferrocyanide, achieving stable structure and high adsorption performance. Effect

Inactive Publication Date: 2016-05-25
TSINGHUA UNIV
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Problems solved by technology

However, in practical applications, ferrocyanide generally has small particle size and poor hydraulic properties, so it cannot be operated on the column, and the separation of solid and liquid phases is very difficult; in addition, the internal mass transfer conditions of ferrocyanide particles are poor, and the inner layer adsorption Agents are often not fully utilized (Nuclear Chemistry and Radiation Chemistry, 23, 108-113, 2001)
In response to this problem, domestic and foreign counterparts usually use immobilization technology, one is to load ferrocyanide on the surface of carriers such as silica (Separation and Purification Technology 16, 147–158, 1999), and its disadvantages are: the loading of active components Low; the process of using transition metal ions to fix ferrocyanide is difficult to complete, and the active ferrocyanide component is easy to lose during use
The other is to combine the adsorbent with PAN to make inorganic / organic hybrid pellets (Chinese patent CN1319849A). The problem is that the binder is easy to block the surface area pores of the adsorbent and reduce the performance of the adsorbent.
In the in situ immobilization technique, SiO 2 As a binder, it is easy to wrap the active adsorbent ferrocyanide in the inner layer, and it is not easy to exert its adsorption effect; wrapping the adsorbent on the outer surface of the silica gel ball can make the adsorbent easy to combine with Cs + However, due to the large particle size of the silica gel balls (3ˉ4mm), it affects the adsorption of the adsorbent on the Cs + Ion Adsorption Efficiency and Adsorption Capacity

Method used

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  • Preparing method of particle caesium removing inorganic ion adsorbent and product and application
  • Preparing method of particle caesium removing inorganic ion adsorbent and product and application
  • Preparing method of particle caesium removing inorganic ion adsorbent and product and application

Examples

Experimental program
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Effect test

Embodiment 1

[0057] Embodiment 1: the laboratory preparation of five kinds of silica gel-loaded adsorbents

[0058] Two-step impregnation method to prepare silica-supported adsorbent:

[0059] 1) Add 4L of deionized water to five 10L beakers respectively, add: A—630g of Co(NO 3 ) 2 ·6H 2 O; B—790g of CuSO 4 ·5H 2 O; C—180g of (CH 3 COO) 2 Zn·2H 2 O; D—1020g of ZrO(NO 3 ) 2 ; E—430g of FeCl 3 ·6H 2 O. Heat and stir until completely dissolved, then pour the five solutions into five enamel trays each containing 1kg of silica gel particles, the solution is basically immersed in all the silica gel, and stand for 3 hours, stirring often during the process to make the particles impregnated evenly. Then put the 5 trays in a constant temperature oven and dry them at 120°C for 10 hours, then take them out and cool down naturally to obtain silica gel intermediates impregnated with different ions.

[0060] 2) Add 5L of deionized water to each of the five 10L beakers of A, B, C, D, and E, ...

Embodiment 2

[0066] Example 2: Trial production of a single batch of 500kg KCuHCF-S

[0067] Add 500L of water to a 1 ton reaction box, and add 395kg of CuSO 4 ·5H 2 O, heated to 80°C with continuous stirring to dissolve completely. Then add 500kg of silica gel carrier, impregnate at 80°C for 12 hours, and stir frequently during the process to make the adsorption process uniform. Afterwards, the material was filtered, placed in a tray, and dried in an electric blast drying room at 120°C for 24 hours. The filtrate was collected and the water uptake of the first maceration was determined by volume. Pour the filtrate back into the reaction box, and add water in it, so that the volume of the solution is equal to the amount of water absorbed for the first time. Put the dried material into the reaction box again, repeat the first impregnation process and operating conditions until the solution is basically absorbed. Place the material in a tray again, and dry it in an electric blast drying ...

Embodiment 3

[0070] Example 3: Trial production of 500kg KZnHCF-S in a single batch

[0071] Add 500L water in 1 ton of reaction box, add 92kg (CH 3 COO) 2 Zn·2H 2 O, heated to 40°C with continuous stirring to dissolve completely. Then add 500kg of silica gel carrier, impregnate at 40°C for 12 hours, and stir frequently during the process to make the adsorption process uniform. Afterwards, the material was filtered, placed in a tray, and dried in an electric blast drying room at 120°C for 24 hours. The filtrate was collected and the water uptake of the first maceration was determined by volume loss. Pour the filtrate back into the reaction box, add water to make the volume of the solution equal to the first water absorption. Put the dried material into the reaction box again, repeat the first impregnation process and operating conditions until the solution is basically absorbed. Place the material in the tray again, and dry it in an electric blast drying room at 120°C for 24 hours to...

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Abstract

The invention comprises the specific steps: according to a principle of monolayer dispersion of salts on an oxide carrier surface, adopting an X ray diffraction method to determine a monolayer dispersion value of Mn <+> ion salt on a silica gel surface and taking the value as an optimal Mn <+> ion salt capacity. In the preparing of the adsorbent, silica gel particles are fully dipped with Mn <+> ion salt of certain concentration to load the Mn <+> ions on the silica gel surface to form a dispersion monolayer, and higher binding force exists between the Mn<+> ions and the silica gel; then an intermediate M/SiO2 is fully soaked with a potassium ferrocyanide solution to react potassium ferrocyanide with the Mn<+> ions on the surface, so as to generate a layer of ferrocyanide with stable M ions and higher binding force at the silica gel surface. Through static Cs<+> adsorptive property determining, fixed bed reactor cooling experiment determining and verification of a fixed bed reactor 137Cs radioactivity tracer test, the silica gel-carrying ferrocyanide adsorbent prepared by the method has well adsorptive property for Cs<+>.

Description

technical field [0001] The invention relates to a method for removing radioactive waste liquid 134 Cs / 137 The invention relates to a granular inorganic ion adsorbent for Cs ions and an industrial preparation method thereof, in particular to a preparation method of a composite adsorption material. The material uses silica gel as a carrier, and uses a surface monolayer dispersion technology to load a series of metal ion-stabilized ferrocyanide active components, in which the stable metal ions include Fe 3+ 、Co 2+ 、Cu 2+ , Zn 2+ and Zr 4+ Wait. The formed granular adsorbent is suitable for filling in fixed-bed adsorption reactors and applied to the waste liquid treatment process of nuclear power plants and other nuclear facilities. The invention belongs to the technical field of material preparation and radioactive waste water treatment. Background technique [0002] As an important clean energy, nuclear power is gradually becoming an important part of my country's ene...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/10B01J20/30G21F9/12
CPCB01J20/0211B01J20/0225B01J20/0229B01J20/0237B01J20/0244B01J20/0274B01J20/103B01J2220/42B01J2220/4806G21F9/12B01J20/04B01J20/223B01J20/28064B01J20/28066B01J20/3085B01J20/3204B01J20/3236C02F1/281C02F1/288C02F2101/006
Inventor 赵璇尉继英成徐州
Owner TSINGHUA UNIV
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