CN112053794B - Method for deeply purifying radioactive wastewater by utilizing nano composite adsorption material - Google Patents
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- 239000002354 radioactive wastewater Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 20
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 title claims abstract description 16
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000002244 precipitate Substances 0.000 claims abstract description 11
- 239000000084 colloidal system Substances 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 9
- 239000000941 radioactive substance Substances 0.000 claims abstract description 9
- 239000007790 solid phase Substances 0.000 claims abstract description 6
- 238000007599 discharging Methods 0.000 claims abstract description 4
- 230000000694 effects Effects 0.000 claims abstract description 4
- 239000007791 liquid phase Substances 0.000 claims abstract description 4
- 230000001737 promoting effect Effects 0.000 claims abstract description 4
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 19
- 238000000746 purification Methods 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 abstract description 10
- 238000004065 wastewater treatment Methods 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 4
- 239000007787 solid Substances 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 229910052742 iron Inorganic materials 0.000 description 9
- 239000007788 liquid Substances 0.000 description 7
- 230000007613 environmental effect Effects 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 6
- 230000002285 radioactive effect Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 239000002901 radioactive waste Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-NJFSPNSNSA-N Carbon-14 Chemical compound [14C] OKTJSMMVPCPJKN-NJFSPNSNSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052722 tritium Inorganic materials 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
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- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention belongs to the technical field of radioactive wastewater treatment. Aiming at the problem that the removal rate of the existing method for treating radioactive wastewater cannot meet the requirement of less than 10Bq/L or near zero emission, the method for deeply purifying the radioactive wastewater by utilizing the nano composite adsorption material is provided. The method comprises the following steps: mixing radioactive wastewater to be treated with H 2 SiO 3 Mixing the solutions at 70-80deg.C, adding NaSiO 3 Mixing the solutions, and reacting at 60-70 ℃ to generate polysilicic acid colloid; feCl is added 3 And FeSO 4 Adding the mixture into polysilicic acid colloid, adjusting the pH value to 8-9, and promoting the formation of ferric silicate complex precipitate; (3) And (3) centrifugally separating the ferric silicate complex precipitate, treating a solid phase by adopting the existing solid radioactive substance method, directly discharging the liquid phase with the total beta activity concentration of the wastewater of which the radionuclide is detected lower than 10Bq/L, and finally obtaining the precipitate with the radioactive substance content of more than 98%.
Description
Technical Field
The invention belongs to the technical field of radioactive wastewater treatment, and particularly relates to a method for deeply purifying radioactive wastewater by utilizing a nano composite adsorption material.
Background
After the radioactive wastewater of nuclear power plants and nuclear facilities is treated, the treated effluent is discharged and controlled strictly by each supervision department, which belongs to the important environmental protection field. With the improvement of public environmental awareness and the enhancement of government environmental protection supervision, the environmental emission standard requirements of various industrial facilities are higher and higher. The method actively develops the research of the advanced purification treatment technology of the radioactive waste liquid and has important practical significance for promoting the development and progress of the waste treatment technology.
The radioactive waste liquid is treated by setting a reasonable and feasible purification process according to the emission limit value. Currently, the implemented GB6249-2011 standard of environmental radiation protection regulations of nuclear power plants, for coastal plant sites, the concentration of other radionuclides except tritium and carbon-14 in radioactive effluent at a tank discharge outlet should not exceed 1000Bq/L; for inland sites, the concentration of other radionuclides in the radioactive effluent at the tank drain outlet, except for tritium and carbon-14, should not exceed 100Bq/L. With the improvement of environmental protection requirements, the existing emission standard is replaced by a stricter standard, and the emission concentration of radioactive wastewater is less than 10Bq/L or near zero emission is a necessary requirement. The existing radioactive waste liquid treatment process cannot meet the emission requirements in the future, and research on deep purification treatment technology and equipment of the radioactive waste liquid is urgently needed.
The radioactive waste water treatment at home and abroad mainly adopts the technologies of chemical flocculation method, ion exchange method, evaporation concentration method, membrane separation method and the like. At present, various adsorption technologies have been developed for purifying radioactive sewage, such as activated carbon adsorption, zeolite adsorption or other combined-type adsorption to remove radionuclides. The chemical flocculation method has the advantage of simple process, but the flocculant type needs to be reasonably selected according to the characteristics of the wastewater, the dosage of the flocculant also needs to be adjusted according to the change of the characteristics of the wastewater, and the method has the defects that only radionuclides existing in a colloid state in the wastewater can be removed and the purification efficiency is low. The ion exchange method is mainly suitable for treating wastewater with low salt content. If an ion exchange system is used for treating wastewater with higher salt content, a great amount of salt in the water can quickly consume the exchange capacity of the ion exchange resin, the consumption of the resin can be great, and the secondary waste amount can also be obviously increased. The evaporation concentration method treatment system has complex equipment composition, high energy consumption and large workload of operation, use and operation maintenance. If the high-salt-content waste water is treated by an evaporation method, the high-salt-content radioactive waste water generally contains high-concentration chloride ions, and if the high-chloride-ion-content waste water directly enters an evaporation system for treatment, the concentration of the chloride ions in the residual liquid can reach tens of thousands of mg/L, so that the risks of intergranular corrosion and stress corrosion cracking of the equipment pipelines of the evaporation system can be greatly increased. The membrane separation method has the advantages of simple equipment, small occupied area, simple and convenient system operation control and the like, but the common membrane separation treatment system can only perform primary concentration treatment on radioactive wastewater, and the residual concentrated solution after treatment can meet the requirement of solidification after further treatment by adopting methods such as evaporation and the like. The existing method for treating the wastewater has low removal rate, cannot meet the increasingly strict discharge requirements, and cannot achieve near zero discharge. The prior method is used for treating radioactive wastewater, and the radionuclide removal rate is mostly between 70% and 90%.
Disclosure of Invention
Aiming at the problems that the prior method for treating radioactive wastewater has low removal rate and can not meet the requirement of less than 10Bq/L or near zero emission, the invention provides a method for deeply purifying radioactive wastewater by utilizing a nano composite adsorption material.
The invention is realized by the following technical scheme:
a method for deeply purifying radioactive wastewater by utilizing nano composite adsorption materials comprises the following steps:
(1) Mixing radioactive wastewater to be treated with H 2 SiO 3 Mixing the solutions at 70-80deg.C, and adding NaSiO 3 Mixing the solutions, and reacting at 60-70 ℃ to generate polysilicic acid colloid;
(2) FeCl is added 3 Solution and FeSO 4 Mixing the solutions, adding the mixed solution into polysilicic acid colloid, regulating the pH value to 8-9, and promoting the formation of ferric silicate complex precipitate, wherein nuclides are adsorbed on the surface of the ferric silicate complex;
(3) And (3) centrifugally separating ferric silicate complex precipitate, wherein a solid phase contains radioactive substances, treating the solid phase by adopting the existing solid-state radioactive substance method, and directly discharging the liquid phase after detecting the total beta activity concentration of the radionuclide in the drainage is lower than 10 Bq/L.
Further, the step (1) H 2 SiO 3 The concentration of the solution is 15-25mg/mL, and the NaSiO 3 The concentration of the solution is in the range of 4-10mg/mL.
Further toIn said step (2) FeCl 3 Solution and FeSO 4 The concentration of the mixed solution is in the range of 35-60mg/mL.
Further, the H 2 SiO 3 The concentration of the solution is 19.3mg/mL, and the addition amount is 30mL; naSiO (NaSiO) 3 The concentration of the solution is 6.7mg/mL, and the addition amount is 12mL; feCl 3 And FeSO 4 The concentration of the mixed solution was 55.1mg/mL and the amount added was 20mL.
Further, the concentration range of the radioactive wastewater to be treated is 1-400Bq/L.
Further, the concentration range of the radioactive wastewater to be treated is 386Bq/L.
Further, the radioactive wastewater to be treated contains 60 Co、 90 Sr、 137 Cs、 90 Y, etc.
The invention provides a method for deeply purifying radioactive wastewater by utilizing nano composite adsorption material, which synthesizes polysilicic acid colloid nano particles with the size not more than 10nm, and uses a discrete magnet with positive charges in the same volume as an additional adsorbent to efficiently and selectively adsorb the radioactive wastewater under the action of electromagnetic field 60 Co、 90 Sr and 137 the Cs and other main nuclides are not influenced by the organic matters and other surface active substances contained in the waste liquid; the precipitation synthesized by complexing the nuclide cations and the nanocomposite is convenient for separation and collection treatment; the method has the advantages of purification efficiency, simple process operation and short time.
Drawings
FIG. 1 is a diagram of a physical-chemical process for the purification of radioactive wastewater using the nanocomposite.
Fig. 2 is a photograph of iron silicate complex observed by an electron microscope, which shows, from left to right, a sample of iron silicate complex in dry air, a sample of iron silicate complex at 250 c, and a sample of iron silicate complex at 1000 c in this order.
FIG. 3 is an X-ray diffraction pattern of an iron silicate complex.
Fig. 4 is a schematic diagram of a nanomaterial adsorption nuclide of the present application.
Detailed Description
The invention will be described in further detail with reference to specific embodiments and drawings.
Example 1
The method for deeply purifying the radioactive wastewater by utilizing the nano composite adsorption material comprises the following steps of:
(1) The concentration of 386Bq/L is contained 60 Co、 90 Sr and 137 radioactive waste water to be treated of Cs and other nuclides and H 2 SiO 3 Mixing the solutions, heating to 70-80 ℃, and then adding NaSiO 3 Mixing the solutions, and reacting at 60-70 ℃ for about 1h to obtain polysilicic acid colloid.
(2) FeCl is added 3 Solution and FeSO 4 Mixing the solutions, adding the mixed solution into polysilicic acid colloid, regulating the pH value to 8-9, reacting for 1h to generate iron silicate crystals, and stirring for 24h by adopting an ultrasonic stirrer to enable the surface of the iron silicate complex to adsorb nuclides;
(3) Centrifugally separating ferric silicate complex precipitate (figure 2 and figure 3), wherein the solid phase contains radioactive substances, treating by adopting the existing solid state radioactive substance method, detecting the total beta activity concentration of the radionuclide in the liquid phase to be lower than 10Bq/L, and directly discharging.
The preparation materials required by the preparation method provided by the invention are common chemical reagents in laboratories; the experimental reaction temperature is 70-80 ℃, and the operation is not high; the obtained colloidal precipitate can be separated by centrifugation, and the whole experimental process is simple to operate, and has shorter time consumption and higher preparation rate of the nanocomposite.
As can be seen from FIGS. 2 and 3, the nanocomposite prepared by this method has a diameter of between 4 and 8 nm.
It was determined that 20g of iron silicate crystals were consumed per 2L of radioactive waste water to be treated.
The nanometer composite material is used for describing the existence of radioactive elements in water during the radioactive wastewater treatment process.
TABLE 1 morphology of radioactive elements in Water during treatment of radioactive wastewater Using the nanocomposite
Therefore, the method provided by the invention can simultaneously remove 60 Co、 90 Sr、 90 Y and 137 cs are a number of major species.
The separated ferric silicate complex precipitate is taken as a sample, and the composition of the sample is analyzed. The results are shown in Table 2.
TABLE 2 precipitation composition and content of iron silicate complexes
The results show that the ferric silicate complex has better precipitation stability. The nano composite material obtained through laboratory tests is reacted with radioactive wastewater through a wastewater treatment device, so that the content of radioactive substances in the precipitate is up to more than 98% (the radioactive concentration of the original treatment waste liquid is 386Bq/L, and the concentration of the treated wastewater after being discharged is 6.4+/-0.8 Bq/L), thereby meeting the requirements of the radioactive wastewater discharge concentration of less than 10Bq/L or near zero discharge.
The above examples are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solution of the present invention should fall within the scope of protection defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (6)
1. The method for deeply purifying the radioactive wastewater by utilizing the nano composite adsorption material is characterized by comprising the following steps of:
(1) The radioactive wastewater to be treated is mixed with 30mL of H with the concentration of 19.3mg/mL 2 SiO 3 The solution was mixed at 70-80℃and then 12mL of NaSiO at a concentration of 6.7mg/mL was added 3 Mixing the solutions, and reacting at 60-70 ℃ to generate polysilicic acid colloid with the size not more than 10 nm;
(2) FeCl is added 3 Solution and FeSO 4 Mixing the solutions, adding the mixed solution into polysilicic acid colloid, regulating the pH value to 8-9, and promoting the formation of ferric silicate complex precipitate, wherein nuclides are adsorbed on the surface of the ferric silicate complex;
(3) And (3) centrifugally separating ferric silicate complex precipitate, wherein a solid phase contains radioactive substances, treating the solid phase by adopting the existing solid-state radioactive substance method, and directly discharging the liquid phase after detecting the total beta activity concentration of the radionuclide in the drainage is lower than 10 Bq/L.
2. The method for deep purification of radioactive wastewater by using nano-composite adsorption material according to claim 1, wherein in the step (2), feCl 3 And FeSO 4 The concentration of the mixed solution is in the range of 35-60mg/mL.
3. The method for deep purification of radioactive wastewater by using nano-composite adsorption material according to claim 1, wherein the feci 3 And FeSO 4 The concentration of the mixed solution was 55.1mg/mL, and the amount added was 20mL.
4. The method for deep purification of radioactive wastewater by using nano-composite adsorption material according to claim 1, wherein the concentration of the radioactive wastewater to be treated is 1-400Bq/L.
5. The method for deep purification of radioactive wastewater by using nano-composite adsorption material according to claim 4, wherein the concentration of the radioactive wastewater to be treated is 386Bq/L.
6. The method for deep purification of radioactive wastewater by using nano-composite adsorption material according to claim 1, wherein the radioactive wastewater to be treated contains 60 Co、 90 Sr and 137 Cs。
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