CN106927539B - UF (ultra filtration factor)6Treatment method of production tail gas leacheate - Google Patents
UF (ultra filtration factor)6Treatment method of production tail gas leacheate Download PDFInfo
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- CN106927539B CN106927539B CN201511025774.0A CN201511025774A CN106927539B CN 106927539 B CN106927539 B CN 106927539B CN 201511025774 A CN201511025774 A CN 201511025774A CN 106927539 B CN106927539 B CN 106927539B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/18—Nature of the water, waste water, sewage or sludge to be treated from the purification of gaseous effluents
Abstract
The invention belongs to the technical field of uranium conversion, and particularly relates to UF6A method for treating production tail gas leacheate. Selecting UF6Wastewater generated in the process of leaching the process tail gas is taken as a treatment object; preparing 15-20% sodium hydroxide solution for neutralizing bicarbonate ions in the process wastewater, converting the bicarbonate ions into carbonate ions and reducing HCO3 ‑Competitive adsorption of metallic uranium; adding the prepared sodium hydroxide solution into a process wastewater tank, and uniformly stirring by using compressed air; the prepared alkaline uranium-containing waste liquid is sent to a filter by a magnetic driving centrifugal pump for filtering and removing suspended particle impurities; pressing the waste liquid into an ion exchange column by using compressed air for adsorption treatment, wherein the ion exchange column is filled with strong-base anion exchange resin; after the ion exchange resin is adsorbed and saturated, desorbing the ion exchange resin by using a mixed solution of 2mol/L sodium chloride and 5% sodium carbonate as a desorbent; and precipitating the desorption solution by using solid sodium hydroxide, and recovering the metal uranium in the desorption solution.
Description
Technical Field
The invention belongs to the technical field of uranium conversion, and particularly relates to UF6A method for treating production tail gas leacheate.
Background
At present, UF is treated at home and abroad6The treatment measures of the alkaline uranium-containing waste liquid generated in the production process mainly include two measures: firstly, the ion exchange method is adopted for the exchange adsorption treatment. Secondly, adopt Ca (OH)2Alkalization, FeSO4Neutralizing, and finally adding a precipitator for treatment, so that the standard discharge of the wastewater can be realized after the treatment. From the uranium conversion process itself, the UO2Hydrofluorination to prepare UF4Techniques and UF4Preparation of UF by fluorination6The technology is at the leading level in China, but indexes such as three-waste emission and the like have larger gap with foreign advanced uranium conversion production plants, especially UF6CO in alkaline uranium-containing waste liquid generated in production tail gas leaching procedure3 2-、HCO3 -、F-、Cl-Coexisting, the prior art has poor uranium removal effect, and the maximum allowable limit value of wastewater discharge of 0.05mg/L is difficult to achieve. At present, domestic UF6The main problems in the treatment process of the alkaline uranium-containing wastewater generated in the production process are as follows: (1) the content of the bicarbonate ions in the alkaline uranium-containing waste liquid is high, and the adsorption effect of the resin on uranium in the waste liquid during ion exchange is obviously influenced by the content of the bicarbonate ions in the waste liquid; (2) the concentration of metallic uranium in the waste liquid after the ion exchange adsorption treatment can not reach the discharge standard.
Disclosure of Invention
The invention aims to provide UF6A method for treating a production tail gas leacheate, which overcomes the defects in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
UF (ultra filtration factor)6The treatment method of the production tail gas leacheate comprises the following steps:
the method comprises the following steps: putting strongly basic styrene quaternary ammonium I type anion exchange resin into an ion exchange column, and fixing the upper end and the lower end of the ion exchange column by sieve plates;
step two: preparing a sodium carbonate solution with the mass percentage of 5% in a transformation liquid preparation tank; opening the inlet and outlet control valves of the ion exchange column; opening an inlet control valve of a transformation liquid preparation tank to ensure that transformation liquid enters from the top of the ion exchange column at a flow rate of 900L/h; sampling from a sampling port at the bottom of the ion exchange column, sampling once every 3h, and analyzing the content of chloride ions in the transformation liquid; when the content of chloride ions is reduced to 3g/L, the flow rate of the transformation liquid is adjusted to 300L/h for continuous transformation, and sampling is carried out according to the same frequency until the content of the chloride ions in the transformation effluent liquid is reduced to below 1g/L, and the transformation is finished;
step three: transferring the alkaline uranium-containing waste liquid into a waste liquid storage tank, and sampling and analyzing the content and pH value of uranium, fluorine ions, chloride ions, carbonate ions and bicarbonate ions; adding 50kg of sodium hydroxide into a sodium hydroxide lye preparation tank, and then adding water into the sodium hydroxide lye preparation tank to prepare 15-20% of sodium hydroxide solution; starting a sodium hydroxide alkali liquor preparation tank to stir compressed air, accelerating the dissolution of sodium hydroxide, and stopping stirring after stirring for 10 min; opening a compressed air stirring control valve to stir the compressed air stirring control valve; opening an outlet valve at the bottom of the sodium hydroxide preparation tank, and conveying the sodium hydroxide lye into a waste liquid storage tank; stirring for about 1h, stopping stirring by compressed air, sampling the prepared waste liquid, and analyzing the uranium, fluorine, carbonate, bicarbonate and chloride ion contents and pH value; filtering the blended waste liquid;
step four: opening a waste liquid inlet control valve of the ion exchange column; adjusting the opening of a waste liquid inlet control valve of the ion exchange column to ensure that the flow of the liquid entering the column is controlled to be 600L/h; opening a sampling port control valve at the bottom end of the ion exchange column, and observing whether tail liquid flows out of an outlet of the ion exchange column; when tail liquid flows out from a sampling port at the bottom end of the ion exchange column, sampling effluent liquid at the bottom of the ion exchange column, and analyzing the content of uranium, fluorine, carbonate, bicarbonate and chloride ions in the effluent liquid; when the uranium content in the effluent of the ion exchange column is increased to 50 mug/L, the other ion exchange column is switched in, so that the two ion exchange columns are connected in series to run, and the uranium content in the effluent of the tail column is ensured to be lower than 50 mug/L; when the first ion exchange column approaches or reaches adsorption saturation, the first ion exchange column is withdrawn from operation;
step five: preparing a mixed solution of 2mol/L NaCl and 5% sodium carbonate in a resolving liquid preparation tank; stirring compressed air for about 2 hours, standing and clarifying;
step six: the analytic solution enters from the upper end of the ion exchange column; opening a resolving liquid inlet valve of the ion exchange column to pressurize resolving liquid to the ion exchange column; adjusting an inlet valve of the desorption solution of the ion exchange column to ensure that the flow rate of the desorption solution entering the column is 900L/h; opening a sampling port valve at the bottom end of the ion exchange column, and observing whether liquid flows out from an outlet at the bottom of the ion exchange column; when the outlet at the bottom of the ion exchange column is filled with the analysis solution, sampling the analysis solution flowing out from the bottom of the ion exchange column to analyze the content of uranium, fluorine, carbonate, bicarbonate and chloride ions in the analysis solution; when the uranium content in the resolving liquid of the ion exchange column is reduced to 300mg/L, adjusting an inlet control valve of the resolving liquid of the ion exchange column, adjusting the flow rate of the resolving liquid entering the column to 300L/h, sampling according to the same frequency, and analyzing the uranium, fluorine, carbonate, bicarbonate and chloride ion content; when the uranium content in the resolving liquid flowing out of the ion exchange column is reduced to be below 150mg/L, determining that resolving is finished;
step seven: sampling and analyzing the uranium content in the analysis solution; according to UO2(CO3)3 4-Calculating the theoretical metering value of the required sodium hydroxide, adding the sodium hydroxide according to the amount which is 1.2 times of the theoretical metering value, and stirring for 1 hour; filtering and analyzing the uranium, fluorine ion, carbonate and hydroxyl ion content in the filtrate; discharging the filtrate after the filtrate is qualified by analysis, and barreling and recycling the filter cake.
In the first step, the domestic trade mark of the anion exchange resin is 201 multiplied by 7.
The packing amount of the ion exchange column was 1625 kg.
In the third step, the content of bicarbonate ions in the sodium hydroxide solution is not more than 5.0g/L, and the pH value is 10-11.
The beneficial effects obtained by the invention are as follows:
UF6the production tail gas leacheate adopts sodium hydroxide solution to neutralize bicarbonate ions in the production tail gas leacheate so as to reduce competitive adsorption of the bicarbonate ions to uranium and improve adsorption efficiency of resin to metal uranium. The uranium content in the waste liquid after adsorption can be reduced to below 1 mg/L. Then, the calcium oxide is used for precipitation treatment, and the content of metal uranium in the treated waste liquid can reach the discharge level. And the produced waste slag can reach the exemption level. The maximum recovery of metal uranium is realized, and the recovery rate of uranium can reach more than 90% after the uranium is subjected to sodium hydroxide solution preparation, ion exchange adsorption, desorption and precipitation treatment.
Detailed Description
The present invention will be described in detail with reference to specific examples.
UF according to the invention6The treatment method of the production tail gas leacheate comprises the following steps:
(1) selection of UF in the invention6The wastewater generated in the process of leaching the process tail gas is taken as a treatment object, and the leaching process is shown in the following equation:
UF6+H2O＝UO2F2+4HF
UO2F2+3NaCO3＝Na4[UO2(CO3)3]+2NaF
the main components in the wastewater after washing are shown in table 1.
TABLE 1 content of each ion in wastewater
| Serial number | Item | Unit of | Content (wt.) |
| 1 | [U] | g/L | 0.2～0.8 |
| 2 | [HCO3 -+CO3 2-] | g/L | 15～25 |
| 3 | [F-] | g/L | 5～15 |
| 4 | [Cl-] | g/L | 1～2 |
| 5 | [Na+] | g/L | 20 |
(2) Preparing 15-20% sodium hydroxide solution for neutralizing bicarbonate ions in the process wastewater, converting the bicarbonate ions into carbonate ions and reducing HCO3 -Competitive adsorption of metallic uranium.
(3) Adding the prepared sodium hydroxide solution into a process wastewater tank, and uniformly stirring by using compressed air.
(4) And (3) the prepared alkaline uranium-containing waste liquid is sent to a filter by a magnetic driving centrifugal pump for filtering and removing suspended particle impurities.
(5) The waste liquid is pressed into an ion exchange column by compressed air for adsorption treatment, the ion exchange column is filled with strongly basic anion exchange resin (201 x 7 type), and the reaction mechanism is as follows:
2RX+UO2(CO3)2 2-＝R2UO2(CO3)2+2X- (1)
4RX+UO2(CO3)3 4-＝R4UO2(CO3)3+4X- (2)
(6) after the ion exchange resin is adsorbed and saturated, desorbing the ion exchange resin by using a mixed solution of 2mol/L sodium chloride and 5% sodium carbonate as a desorbent.
(7) Precipitating the desorption solution by using solid sodium hydroxide, and recovering the metal uranium in the desorption solution, wherein the reaction formula is as follows:
2Na4[UO2(CO3)3]+6NaOH＝Na2U2O7↓+6NaCO3+3H2O
the method comprises the following steps: filling of ion exchange columns
After checking and confirming that the ion exchange column has the column loading condition, new strongly basic styrene quaternary ammonium type I anion exchange resin (domestic number 201 x 7) is loaded into the ion exchange column, the resin loading amount is considered to be compact after being swelled, and the resin is ensured not to be disturbed by the flow of liquid in the column, and the loading amount of each column is 1625 kg. After the resin is filled, the upper and lower ends are fixed by the sieve plates.
Step two: transformation of novel resins
1) Preparing a sodium carbonate solution with the mass percentage of 5% in a transformation liquid preparation tank;
2) opening the inlet and outlet control valves of the ion exchange column;
3) opening an inlet control valve of a transformation liquid preparation tank to ensure that transformation liquid enters from the top of the ion exchange column at a flow rate of 900L/h;
4) sampling from a sampling port at the bottom of the ion exchange column, sampling once every 3h, and analyzing the content of chloride ions in the transformation liquid;
5) when the content of chloride ions is reduced to 3g/L, the flow rate of the transformation liquid is adjusted to 300L/h for continuous transformation, and sampling is carried out according to the same frequency. And (4) judging that the transformation is finished until the content of chloride ions in the transformation effluent is reduced to be below 1 g/L.
Step three: preparation of liquid to be treated
In order to avoid the influence of the bicarbonate ions in the liquid to be treated on the adsorption of the uranium, the uranium is required to be prepared according to the content and the pH value of the bicarbonate ions in the liquid to be treated before entering the column. After blending, the content of bicarbonate ions in the column entering liquid should not exceed 5.0g/L, and the pH value is 10-11. The blending substance is sodium hydroxide solution with the mass percentage of 15-20%.
1) Transferring the alkaline uranium-containing waste liquid into a waste liquid storage tank, and sampling and analyzing the content and pH value of uranium, fluorine ions, chloride ions, carbonate ions and bicarbonate ions;
2) adding 50kg of sodium hydroxide into a sodium hydroxide lye preparation tank, and then adding water into the sodium hydroxide lye preparation tank to prepare 15-20% of sodium hydroxide solution;
3) starting a sodium hydroxide alkali liquor preparation tank to stir compressed air to accelerate the dissolution of sodium hydroxide, and stopping stirring after stirring for 10 min;
4) opening a compressed air stirring control valve to stir the compressed air stirring control valve;
5) opening an outlet valve at the bottom of the sodium hydroxide preparation tank, and conveying the sodium hydroxide lye into a waste liquid storage tank;
6) stirring for about 1h, stopping stirring by compressed air, sampling the prepared waste liquid (prepared liquid), and analyzing the content and pH value of uranium, fluorine, carbonate, bicarbonate and chloride ions in the waste liquid;
7) filtering the prepared liquid.
Step four: adsorption on ion exchange columns
1) After the system is checked and confirmed to have the waste liquid inlet condition, opening a waste liquid inlet control valve of the ion exchange column;
2) adjusting the opening of a waste liquid inlet control valve of the ion exchange column to ensure that the flow of the liquid entering the column is controlled to be 600L/h;
3) opening a sampling port control valve at the bottom end of the ion exchange column, and observing whether tail liquid flows out of an outlet of the ion exchange column;
4) when tail liquid flows out from a sampling port at the bottom end of the ion exchange column, sampling effluent liquid at the bottom of the ion exchange column, and analyzing the content of uranium, fluorine, carbonate, bicarbonate and chloride ions in the effluent liquid;
5) when the uranium content in the effluent of the ion exchange column is increased to 50 mug/L, the other ion exchange column is switched into the system, so that the two ion exchange columns are connected in series to run, and the uranium content in the effluent of the tail column is ensured to be lower than 50 mug/L;
6) when the first ion exchange column approaches or reaches adsorption saturation, the first ion exchange column is removed from operation.
Step five: preparation of analytical solution
1) Preparing a mixed solution of 2mol/L NaCl and 5% sodium carbonate in a resolving liquid preparation tank;
2) stirring with compressed air for about 2h, standing and clarifying;
step six: resolution of ion exchange column
The analytic solution enters from the upper end of the ion exchange column.
1) Opening a resolving liquid inlet valve of the ion exchange column to pressurize resolving liquid to the ion exchange column;
2) adjusting an inlet valve of the desorption solution of the ion exchange column to ensure that the flow rate of the desorption solution entering the column is 900L/h;
3) opening a sampling port valve at the bottom end of the ion exchange column, and observing whether liquid flows out from an outlet at the bottom of the ion exchange column;
4) when the outlet at the bottom of the ion exchange column is filled with the analysis solution, sampling the analysis solution flowing out from the bottom of the ion exchange column to analyze the content of uranium, fluorine, carbonate, bicarbonate and chloride ions in the analysis solution;
5) when the uranium content in the resolving liquid of the ion exchange column is reduced to 300mg/L, adjusting an inlet control valve of the resolving liquid of the ion exchange column, adjusting the flow rate of the resolving liquid entering the column to 300L/h, sampling according to the same frequency, and analyzing the uranium, fluorine, carbonate, bicarbonate and chloride ion content;
6) and when the uranium content in the analysis liquid flowing out of the ion exchange column is reduced to be below 150mg/L, the analysis is considered to be finished.
Step seven: precipitation of sodium hydroxide
1) And sampling and analyzing the uranium content in the analysis solution.
2) According to UO2(CO3)3 4-Calculating the theoretical metering value of the required sodium hydroxide, adding the sodium hydroxide according to the amount which is 1.2 times of the theoretical metering value, and stirring for 1 hour.
3) The filtrate was filtered and analyzed for uranium, fluoride, carbonate and hydroxide ion content.
4) Discharging the filtrate after the filtrate is analyzed to be qualified,filter cake (Na as main component)2U2O7) And (5) barreling and recycling.
Claims (4)
1. UF (ultra filtration factor)6The treatment method of the production tail gas leacheate is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: putting strongly basic styrene quaternary ammonium type I anion exchange resin into an ion exchange column, and fixing the upper end and the lower end of the ion exchange column by sieve plates;
step two: preparing a sodium carbonate solution with the mass percentage of 5% in a transformation liquid preparation tank; opening the inlet and outlet control valves of the ion exchange column; opening an inlet control valve of a transformation liquid preparation tank to ensure that transformation liquid enters from the top of the ion exchange column at a flow rate of 900L/h; sampling from a sampling port at the bottom of the ion exchange column, sampling once every 3h, and analyzing the content of chloride ions in the transformation liquid; when the content of chloride ions is reduced to 3g/L, the flow rate of the transformation liquid is adjusted to 300L/h for continuous transformation, and sampling is carried out according to the same frequency until the content of the chloride ions in the transformation effluent liquid is reduced to below 1g/L, and the transformation is considered to be finished;
step three: transferring the alkaline uranium-containing waste liquid into a waste liquid storage tank, and sampling and analyzing the content and pH value of uranium, fluorine ions, chloride ions, carbonate ions and bicarbonate ions; adding 50kg of sodium hydroxide into a sodium hydroxide lye preparation tank, and then adding water into the sodium hydroxide lye preparation tank to prepare 15-20% of sodium hydroxide solution; starting a sodium hydroxide alkali liquor preparation tank to stir compressed air, accelerating the dissolution of sodium hydroxide, and stopping stirring after stirring for 10 min; opening an outlet valve at the bottom of a sodium hydroxide alkali liquor preparation tank, conveying the sodium hydroxide alkali liquor into a waste liquor storage tank, opening a compressed air stirring control valve, stirring the sodium hydroxide alkali liquor, stopping stirring the compressed air after stirring for 1h, sampling the prepared waste liquor, and analyzing the uranium, fluorine, carbonate, bicarbonate radical and chloride ion content and pH value in the waste liquor; filtering the blended waste liquid;
step four: opening a waste liquid inlet control valve of the ion exchange column; adjusting the opening of a waste liquid inlet control valve of the ion exchange column to ensure that the flow of the liquid entering the column is controlled at 600L/h; opening a sampling port control valve at the bottom end of the ion exchange column, and observing whether tail liquid flows out of an outlet of the ion exchange column; when tail liquid flows out from a sampling port at the bottom end of the ion exchange column, sampling effluent liquid at the bottom of the ion exchange column, and analyzing the content of uranium, fluorine, carbonate, bicarbonate and chloride ions in the effluent liquid; when the uranium content in the effluent of the ion exchange column is increased to 50 mug/L, the other ion exchange column is switched in, so that the two ion exchange columns are connected in series to run, and the uranium content in the effluent of the tail column is ensured to be lower than 50 mug/L; when the first ion exchange column reaches adsorption saturation, the first ion exchange column is withdrawn from operation;
step five: preparing a mixed solution of 2mol/L NaCl and 5% sodium carbonate in a resolving liquid preparation tank; stirring with compressed air for 2h, standing and clarifying;
step six: the analytic solution enters from the upper end of the ion exchange column; opening a resolving liquid inlet valve of the ion exchange column to pressurize resolving liquid to the ion exchange column; adjusting an inlet valve of the desorption solution of the ion exchange column to ensure that the flow rate of the desorption solution entering the column is 900L/h; opening a sampling port valve at the bottom end of the ion exchange column, and observing whether liquid flows out from an outlet at the bottom of the ion exchange column; when the outlet at the bottom of the ion exchange column is filled with the analysis solution, sampling the analysis solution flowing out from the bottom of the ion exchange column to analyze the content of uranium, fluorine, carbonate, bicarbonate and chloride ions in the analysis solution; when the uranium content in the resolving liquid of the ion exchange column is reduced to 300mg/L, adjusting an inlet control valve of the resolving liquid of the ion exchange column, adjusting the flow rate of the resolving liquid entering the column to 300L/h, sampling according to the same frequency, and analyzing the uranium, fluorine, carbonate, bicarbonate and chloride ion content; when the uranium content in the resolving liquid flowing out of the ion exchange column is reduced to be below 150mg/L, determining that resolving is finished;
step seven: sampling and analyzing the uranium content in the analysis solution; according to UO2(CO3)3 4-Calculating the theoretical metering value of the required sodium hydroxide, adding the sodium hydroxide according to the amount which is 1.2 times of the theoretical metering value, and stirring for 1 hour; filtering and analyzing the uranium, fluorine ion, carbonate and hydroxyl ion content in the filtrate; discharging the filtrate after the filtrate is qualified by analysis, and barreling and recycling the filter cake.
2. The UF of claim 16The treatment method of the production tail gas leacheate is characterized by comprising the following steps: in the first step, the domestic trade mark of the anion exchange resin is 201 multiplied by 7.
3. The UF of claim 16The treatment method of the production tail gas leacheate is characterized by comprising the following steps: the packing amount of the ion exchange column was 1625 kg.
4. The UF of claim 16The treatment method of the production tail gas leacheate is characterized by comprising the following steps: in the third step, the content of bicarbonate ions in the sodium hydroxide solution is not more than 5.0g/L, and the pH value is 10-11.
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| CN109637686B (en) * | 2018-12-27 | 2023-03-17 | 中核四0四有限公司 | Purification treatment method for uranium tetrafluoride fluorinated tail gas leacheate |
| CN109741849B (en) * | 2018-12-27 | 2023-06-16 | 中核四0四有限公司 | Deep purification method for uranium-containing fluorine-containing waste liquid from uranium purification and conversion |
| CN113413928B (en) * | 2021-06-23 | 2023-04-21 | 中国核动力研究设计院 | Nickel-63 automatic separation device and separation process thereof |
| CN114192195A (en) * | 2021-12-09 | 2022-03-18 | 中核内蒙古矿业有限公司 | Elution device for uranium extraction by ion exchange method and elution method of ion exchange resin |
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