CN110467190B - Device and method for recycling boron from radioactive boron-containing waste liquid - Google Patents
Device and method for recycling boron from radioactive boron-containing waste liquid Download PDFInfo
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- CN110467190B CN110467190B CN201810438815.6A CN201810438815A CN110467190B CN 110467190 B CN110467190 B CN 110467190B CN 201810438815 A CN201810438815 A CN 201810438815A CN 110467190 B CN110467190 B CN 110467190B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/023—Boron
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- 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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Abstract
The invention provides a device for recycling boron from radioactive boron-containing waste liquid, which comprises a raw water tank, a separation unit water inlet pump, a separation unit membrane assembly for separating boron and nuclides, an intermediate water tank, a concentration unit water inlet pump, a concentration unit membrane assembly and a water production tank, wherein the raw water tank is connected with the separation unit water inlet pump; the raw water tank, the separation unit water inlet pump, the separation unit membrane assembly, the intermediate water tank, the concentration unit water inlet pump, the concentration unit membrane assembly and the water production tank are sequentially connected. The device for recycling boron in the radioactive boron-containing waste liquid provided by the invention is simple and efficient, solves the problems that boron is concentrated and nuclides and impurities are concentrated in the traditional boron recycling process, improves the purity of the concentrated boron, reduces the radioactivity concentration of the concentrated boron, avoids the repeated concentration of nuclides, increases the solid waste production amount, and simply and flexibly controls the concentration of the recycled boron according to the actual requirements of projects.
Description
Technical Field
The invention relates to a device and a method for recycling boron from radioactive boron-containing waste liquid.
Background
In a conventional pressurized water reactor nuclear power plant, boron is used for reactive chemical compensation control. During the operation of the power plant, a large amount of boron-containing waste liquid is generated due to frequent discharging operation of the boron regulating and capacity dissolving system. Most of the discharged boron-containing waste liquid is concentrated and purified by a boron recovery system and then recycled in a power plant. But still about 0.4 tons of boron per stack year is discharged to the environment.
The reactivity control mode of the CAP series nuclear power plant is similar to that of a common pressurized water reactor nuclear power plant, but the CAP series nuclear power plant also adopts a mechanical compensation operation mode in the reactivity control, soluble boron is only used for compensating the reactivity change caused by the core burnup, and the control rod is utilized for rapid reactivity change control and load tracking, so that the generation of boron-containing waste liquid is reduced from the source. In order to simplify the system design, the prior boron recovery system of the pressurized water reactor power plant is omitted, and if the boron-containing waste liquid is not treated, about 1 ton of boron is discharged into the environment after being treated by the radioactive waste liquid treatment system every year.
The reviewer wishes to further control the boron emission concentration and the total boron emission of the nuclear power plant by design improvement. One solution to control the concentration and total amount of boron eventually discharged to the environment is to reuse this portion of the boron. In addition, based on the application characteristics of the enriched boric acid, more and more nuclear power plants may adopt the enriched boric acid in the future, and in view of the high value of the enriched boron, the enriched boric acid also needs to be recycled.
Currently available processes for recovering boron mainly include evaporation and reverse osmosis membrane processes. The boron removal process adopted by the nuclear power station without the boron recovery system at the present stage has the advantages of mature process, more engineering operation experience, large occupied area, high energy consumption, high activity of radioactive nuclide in concentrated solution, concentration of radioactive nuclide and non-radioactive impurities (including silicon) together with boron, increased solid waste production even if the nuclear power station is purified by a resin bed, and gradual rise of silicon dioxide in a loop due to low selectivity of resin to silicon in impurity ions. The membrane technology is a physical separation process, and no extra impurities are introduced, but the existing membrane treatment technology mainly has the advantages of simple process, high boron removal efficiency, low energy consumption and the like, but boron and nuclides can be concentrated simultaneously. The highest concentration of boron in coolant effluent of nuclear power plant may reach 2700ppm, the average boron concentration is about 1000ppm, the concentration of boron after concentration reaches 5000ppm, the concentration of nuclide ions in radioactive liquid is only ppb level or lower, the contrast between boron and nuclide concentration to be separated is too large, the traditional reverse osmosis membrane lacks application examples for treating boron-containing waste liquid with high boron concentration and low nuclide concentration, and the phenomenon that nuclide and boron are simultaneously concentrated also occurs, so that the concentrated boron cannot meet the recycling requirement.
The invention aims to solve the problems of avoiding concentration of nuclides and other impurity ions while concentrating boron, improving the application range of a membrane to the concentration of boron in water, and concentrating a solution with the average boron concentration of only about 1000ppm into a high-purity boron solution with the average boron concentration of about 5000 ppm. By adopting the combined application of the membrane product with high separation rate of boron and nuclides in the nuclear power plant and the membrane product with high rejection rate of boron, the efficient concentration of boron is carried out after the nuclides in the radioactive boron-containing waste liquid of the nuclear power plant are efficiently separated, and meanwhile, the concentration and purity requirements of engineering application recovery are met, so that the efficient and high-quality recovery and utilization of boron are realized.
Disclosure of Invention
The invention provides a device and a method for recycling boron from radioactive boron-containing waste liquid, aiming at the defects of the prior art.
The invention provides a device for recycling boron from radioactive boron-containing waste liquid, which is characterized by comprising a raw water tank, a separation unit water inlet pump, a separation unit membrane assembly for separating boron and nuclides, an intermediate water tank, a concentration unit water inlet pump, a concentration unit membrane assembly and a water production tank; the raw water tank, the separation unit water inlet pump, the separation unit membrane assembly, the intermediate water tank, the concentration unit water inlet pump, the concentration unit membrane assembly and the water production tank are connected in sequence; the separation unit membrane component is connected with the raw water tank; the concentration unit membrane component is connected with the intermediate water tank; wherein:
the permeability of the separation unit membrane component to boron is more than 90%, and the rejection rate to nuclides is more than 95%;
the rejection rate of the concentration unit membrane component to boron is more than 95 percent.
Preferably, the separation unit feed water pump is configured to pump the radioactive waste containing boron and nuclides in the raw water tank into the separation unit membrane module.
Preferably, the concentration unit water inlet pump is configured to pump the boron-containing waste liquid in the intermediate water tank into the concentration unit membrane module.
Preferably, the separation unit membrane assembly comprises a composite reverse osmosis membrane and is characterized by comprising a non-woven fabric, a support base layer, an active desalting layer and a separation layer, wherein the non-woven fabric, the support base layer, the active desalting layer and the separation layer are sequentially overlapped; the thickness of the non-woven fabric is 80-150 mu m, the supporting base layer is overlapped on the non-woven fabric, and the thickness is 20-50 mu m; the active desalting layer and the separating layer are sequentially attached to the support base layer, and the thickness of the active desalting layer and the separating layer is 0.1-0.5 mu m.
The invention provides a preparation method of a composite reverse osmosis membrane, which comprises the steps that a desalting layer is of a wholly aromatic compact cross-linked structure and is provided with a charged functional group to adjust the charge density of the surface of a polyamide layer; the support base layer is of a porous structure; the support base layer adopts polysulfone and a hydroxyl ethyl ester additive, wherein the polysulfone is used as a raw material, and the concentration of the hydroxyl ethyl ester additive is controlled to be 5-50%.
1-10% of aminobenzoyl piperazine is used as a water phase monomer, 2-8% of trimesoyl chloride is used as an oil-soluble monomer to carry out interfacial polymerization reaction, and the reaction time is controlled to be 30-90s. The compact active layer is ensured to be formed, meanwhile, reasonable flux is ensured, the surface charge density is optimized, the high-separation-rate membrane has high rejection rate for the nuclide with extremely low concentration, and meanwhile, the boric acid can be penetrated, so that an excellent separation effect is achieved.
Preferably, the concentration unit membrane assembly comprises a composite reverse osmosis membrane and is characterized by comprising a non-woven fabric, a support base layer, an active desalting layer and a boron-removing layer, wherein the non-woven fabric, the support base layer, the active desalting layer and the boron-removing layer are sequentially overlapped; the thickness of the non-woven fabric is 80-150 mu m, the supporting base layer is overlapped on the non-woven fabric, and the thickness is 20-50 mu m; the active desalting layer and the boron removing layer are sequentially attached to the support base layer, and the thickness of the active desalting layer and the boron removing layer is 0.1-0.5 mu m.
The desalination layer with the wholly aromatic compact cross-linked structure is constructed by design, and the charge density of the surface of the polyamide layer is adjusted by combining the charged functional groups in the desalination layer. The composite reverse osmosis membrane consists of a support base layer, an active desalting layer and a boron removing layer. The preparation method of the support base layer and the active desalting layer is basically consistent with the traditional membrane preparation method. The preparation method of the boron removal layer comprises the following steps:
adding 15-25% concentration of ethylene glycol methyl ether, 2-10% concentration of catalyst HCl and 2-10% concentration of cross-linking agent glutaraldehyde into deionized water, heating and stirring until the mixture is completely dissolved to obtain ethylene glycol methyl ether cross-linking solution;
and immersing the prepared composite reverse osmosis membrane into the ethylene glycol methyl ether crosslinking solution, and then placing the reverse osmosis membrane immersed in the ethylene glycol methyl ether solution in an oven for heat treatment to obtain the composite reverse osmosis membrane containing the boron removal layer.
The invention provides a method for recycling boron from radioactive boron-containing waste liquid, which comprises the following steps:
pumping the radioactive waste liquid containing boron and nuclides into a separation unit membrane assembly capable of separating boron and nuclides through a separation unit water inlet pump;
the nuclides and impurities in the waste liquid are intercepted by the membrane component of the separation unit and returned to the raw water tank, and boron in the waste liquid is discharged to the intermediate water tank after penetrating the membrane;
pumping the boron solution in the intermediate water tank into a membrane component of the concentration unit through a water inlet pump of the concentration unit, concentrating the boron in the boron solution, and returning to the intermediate water tank until the boron solution reaches a system set value.
Preferably, the raw water tank is used to store radioactive waste liquid containing boron and nuclides.
Compared with the prior art, the invention has the following beneficial effects:
1. the device for recycling boron in the radioactive boron-containing waste liquid provided by the invention is simple and efficient, solves the problems that boron is concentrated and nuclides and impurities are concentrated in the traditional boron recycling process, improves the purity of the concentrated boron, reduces the radioactivity concentration of the concentrated boron, avoids the repeated concentration of nuclides, increases the solid waste production amount, and simply and flexibly controls the concentration of the recycled boron according to the actual requirements of projects.
2. The device for recovering boron from the radioactive boron-containing waste liquid solves the problem that the nuclide is concentrated while the boron in the boron-containing waste liquid of the nuclear power plant is concentrated, reduces the nuclide concentration in the boron solution, and provides a scheme with high purity, low impurity concentration, small process waste production, simple system operation and small occupied area for the recycling of the boron.
3. The device for recycling boron in the radioactive boron-containing waste liquid solves the different requirements of different types of nuclear power plants on the concentration of recycled boron, and can adjust the concentration of the final concentrated boron of the system according to practical engineering application and the type of boron; providing a solution for the nuclear power plant to reduce the total emission amount and concentration of boron in the nuclear power plant; according to the total amount of the boron-containing waste liquid generated by the nuclear power plant, the process requirements can be realized by adjusting the combination mode and the number of the membrane elements, and the flexibility of process application is improved.
Drawings
FIG. 1 is a schematic flow diagram of an apparatus for recovering boron from radioactive boron-containing waste liquid in accordance with a preferred embodiment of the present invention.
Wherein, 1, raw water tank 2: separation unit intake pump 3: separation unit membrane module 4: intermediate water tank 5: concentration unit intake pump 6: concentration unit membrane module 7: water producing tank
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more readily apparent, a more particular description of the invention will be rendered by reference to the appended drawings and appended detailed description.
As shown in FIG. 1, an embodiment of the present invention provides a membrane treatment device for separating boron and nuclides from radioactive waste liquid, which comprises a raw water tank, a separation unit water inlet pump, a separation unit membrane module with high separation rate for boron and nuclides, an intermediate water tank, a concentration unit water inlet pump, a concentration unit membrane module, a water production tank, and related pipelines, valves and meters. The radioactive waste liquid containing boron and nuclides enters a boron and nuclide separation membrane assembly through a separation unit water inlet pump, nuclides and impurities are intercepted by a membrane and then return to an original water tank, boron is discharged to a middle water tank after penetrating through the membrane, high-purity low-concentration boron solution in the middle water tank enters a concentration unit membrane assembly through a concentration unit water inlet pump, boron is continuously concentrated and returns to the middle water tank until reaching a system set value, and water produced by a concentration membrane unit is discharged to a water production tank for waiting discharge.
The membrane treatment method for recycling boron in the radioactive waste liquid is characterized by comprising the following steps:
1. the invention relates to a membrane product with high separation rate for boron, cesium, strontium and other nuclides for a nuclear power plant, which can realize the high-efficiency separation of boron and nuclides, and aims at the boron concentration of 100-5000ppm in water, when the pH value of a solution is not regulated and the recovery rate of a single membrane original is 10%, the transmittance of the boron is more than 90%, and the rejection rate of the nuclides and impurities is more than 95%;
wherein: the main technical means for developing the film product are as follows:
1) Control and optimization of the base film structure:
the base film of the composite film mainly plays a supporting role, and the high-performance supporting film is a necessary condition for preparing the high-performance composite film. In order to obtain a composite membrane having high performance, the support base membrane is required to have appropriate porosity, pore size and pore size distribution. Meanwhile, the supporting layer material should have good chemical stability, thermal stability and mechanical properties. The invention adopts polysulfone which is cheap and easy to obtain, has simple membrane preparation, good mechanical strength and compression tightness, good chemical stability and biodegradation resistance as the raw material of the porous support membrane, controls the concentration of the hydroxyethyl additive to 25%, ensures that the base membrane has no obvious paper-shaped holes, ensures that the developed membrane product has uniform base membrane hole type structure, complete skin layer and higher mechanical property, and prolongs the service life of the membrane product.
2) Control and optimization of active desalination layer structure
Interfacial polymerization is the key to preparing the active desalination layer of the composite membrane. The main factors affecting interfacial polymerization are: the monomer concentration of the aqueous and organic phases, the impregnation time of the base film in both phases, the temperature and time during the heat treatment, etc. In order to improve the better separation effect on the membrane and nuclides, 6% of aminobenzoyl piperazine is used as a water phase monomer, 3% of trimesoyl chloride is used as an oil-soluble monomer, the interfacial polymerization reaction time is controlled in a reasonable range (30-90 s), a compact active layer is ensured to be formed, meanwhile, reasonable flux is ensured, the surface charge density is optimized, the high-separation-rate membrane is ensured to have high rejection rate on the very low-concentration nuclides, and meanwhile, boric acid can be permeated, so that the excellent separation effect is achieved.
2. The concentration of boron in the separated produced water, the total amount of boron and raw water are close to each other, and the total amount of boron emission is reduced to the greatest extent. When 1000ppm B of water is fed and the system recovery rate reaches 50-95%, the concentration of boron in the produced water is 925-980ppm, and the total recovery rate of boron reaches 46-93%;
3. the concentration of nuclides in the separated produced water is obviously reduced, and the purity of the recycled boron is greatly improved. When the water inlet radioactivity concentration is 1000Bq/L and the system recovery rate reaches 50-95%, the nuclide concentration in the produced water is 76-134Bq/L, and the total amount of nuclides and impurities is reduced by 96-88%;
4. after separating nuclide, the boron solution passes through a boron concentration unit, the concentration of the finally concentrated boron can reach any value higher than the concentration of the boron in water, when the concentration of the concentrated boron reaches 4000-7000ppm, the recovery rate of system boron can reach more than 80%, and the activity concentration of radionuclide in the concentrated boron solution can meet the low-level requirement of less than 1000 Bq/L;
in addition, the concentration unit mainly relies on developing a membrane product with high rejection rate for high-concentration boron for a nuclear power plant, and the rejection rate for boron is more than 95% when the pH value of a solution is not regulated and the recovery rate of a single membrane element is 10% aiming at the concentration of boron which is 100-5000 ppm. The main technical means for developing the film product are as follows: the desalination layer with the wholly aromatic compact cross-linked structure is constructed by design, and the charge density of the surface of the polyamide layer is adjusted by combining the charged functional groups in the desalination layer.
Preferably, the composite reverse osmosis membrane in the invention consists of a support base layer, an active desalting layer and a boron-removing layer. The preparation method of the support base layer and the active desalting layer is basically consistent with the traditional membrane preparation method. The preparation method of the boron removal layer comprises the following steps: adding a certain amount (15-25%) of ethylene glycol methyl ether, a catalyst HCl and a cross-linking agent glutaraldehyde (2-10%) into a proper amount of deionized water, heating and stirring until the mixture is completely dissolved, and obtaining the ethylene glycol methyl ether cross-linking solution. And immersing the preliminarily prepared composite reverse osmosis membrane into the ethylene glycol methyl ether crosslinking solution for a certain time, and placing the reverse osmosis membrane immersed in the ethylene glycol methyl ether solution in an oven for heat treatment for a certain time to obtain the composite reverse osmosis membrane containing the boron removal layer.
5. The batch separation treatment is adopted, so that the number of membranes adopted by the system can be reduced to the greatest extent;
6. the number of membrane elements in the membrane component of the separation unit and the combination mode can be flexibly adjusted according to the flow requirement to be treated;
7. the separation end point can be flexibly controlled, and can be controlled by the recovery rate or the water quality index end point which needs to be controlled.
Those skilled in the art may implement the described functionality using different approaches for each particular application, but such implementation is not intended to be limiting.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (5)
1. An apparatus for recovering boron from radioactive boron-containing waste liquid, comprising: raw water tank, separation unit water inlet pump, separation unit membrane module for separating boron and nuclides, intermediate water tank, concentration unit water inlet pump, concentration unit membrane module and water producing tank; the raw water tank, the separation unit water inlet pump, the separation unit membrane assembly, the intermediate water tank, the concentration unit water inlet pump, the concentration unit membrane assembly and the water production tank are connected in sequence; the separation unit membrane component is connected with the raw water tank; the concentration unit membrane component is connected with the intermediate water tank;
the separation unit membrane component comprises a composite reverse osmosis membrane and comprises non-woven fabrics, a support base layer, an active desalting layer and a separation layer, wherein the non-woven fabrics, the support base layer, the active desalting layer and the separation layer are sequentially overlapped; the support base layer is overlapped on the non-woven fabric, and the active desalting layer and the separating layer are sequentially attached to the support base layer; the active desalting layer is of a wholly aromatic compact cross-linked structure, 6% of aminobenzoyl piperazine is adopted as a water phase monomer, 3% of trimesoyl chloride is adopted as an oil-soluble monomer, the interfacial polymerization reaction time is controlled to be 30-90s, and the active desalting layer has a charged functional group to adjust the charge density of the surface of the polyamide layer; the support base layer is of a porous structure; the support base layer adopts polysulfone and a hydroxyl ethyl ester additive, wherein the polysulfone is used as a raw material, and the concentration of the hydroxyl ethyl ester additive is controlled to be 5-50%;
the concentration unit membrane component comprises a composite reverse osmosis membrane, and comprises a non-woven fabric, a support base layer, an active desalting layer and a boron-removing layer, wherein the non-woven fabric, the support base layer, the active desalting layer and the boron-removing layer are sequentially overlapped; the support base layer is overlapped on the non-woven fabric, and the active desalting layer and the boron-removing layer are sequentially attached to the support base layer; the preparation method of the boron removal layer comprises the following steps: adding 15-25% concentration of ethylene glycol methyl ether, 2-10% concentration of catalyst HCl and 2-10% concentration of cross-linking agent glutaraldehyde into deionized water, heating and stirring until the mixture is completely dissolved to obtain ethylene glycol methyl ether cross-linking solution; immersing the prepared composite reverse osmosis membrane into ethylene glycol methyl ether crosslinking solution, and then placing the reverse osmosis membrane immersed in the ethylene glycol methyl ether solution in an oven for heat treatment to obtain the composite reverse osmosis membrane containing the boron removal layer;
the permeability of the separation unit membrane component to boron is more than 90%, and the rejection rate to nuclides is more than 95%; the rejection rate of the concentration unit membrane component to boron is more than 95 percent.
2. The apparatus for recovering boron from a radioactive boron-containing waste liquid of claim 1, wherein said separation unit feed water pump is configured to pump the radioactive waste liquid containing boron and nuclides in said raw water tank into said separation unit membrane module.
3. The apparatus for recovering boron from a radioactive boron-containing waste liquid of claim 1, wherein said concentrating unit water inlet pump is configured to pump boron-containing waste liquid in said intermediate water tank into said concentrating unit membrane module.
4. A method for recovering boron of an apparatus for recovering boron from radioactive boron-containing waste liquid as claimed in claim 1, comprising the steps of:
pumping the radioactive waste liquid containing boron and nuclides into a separation unit membrane assembly capable of separating boron and nuclides through a separation unit water inlet pump;
the nuclides and impurities in the waste liquid are intercepted by the membrane component of the separation unit and returned to the raw water tank, and boron in the waste liquid is discharged to the intermediate water tank after penetrating the membrane;
pumping the boron solution in the intermediate water tank into a membrane component of the concentration unit through a water inlet pump of the concentration unit, concentrating the boron in the boron solution, and returning to the intermediate water tank until the boron solution reaches a system set value.
5. The method for recovering boron according to claim 4, wherein said raw water tank is used for storing radioactive waste liquid containing boron and nuclides.
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