CN103420347B - Defluorination method and device in nitric acid evaporation recovery process - Google Patents
Defluorination method and device in nitric acid evaporation recovery process Download PDFInfo
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- CN103420347B CN103420347B CN201210152563.3A CN201210152563A CN103420347B CN 103420347 B CN103420347 B CN 103420347B CN 201210152563 A CN201210152563 A CN 201210152563A CN 103420347 B CN103420347 B CN 103420347B
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- nitric acid
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- fluorine
- defluorination
- defluorination method
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- 238000000034 method Methods 0.000 title claims abstract description 65
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910017604 nitric acid Inorganic materials 0.000 title claims abstract description 51
- 238000001704 evaporation Methods 0.000 title claims abstract description 32
- 230000008020 evaporation Effects 0.000 title claims abstract description 27
- 238000006115 defluorination reaction Methods 0.000 title claims abstract description 22
- 238000011084 recovery Methods 0.000 title abstract description 4
- 229910052731 fluorine Inorganic materials 0.000 claims description 37
- 239000011737 fluorine Substances 0.000 claims description 37
- 239000000945 filler Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000006200 vaporizer Substances 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 239000011324 bead Substances 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims 4
- 239000007788 liquid Substances 0.000 abstract description 36
- 230000000694 effects Effects 0.000 abstract description 7
- 238000012856 packing Methods 0.000 abstract description 2
- 238000004821 distillation Methods 0.000 abstract 2
- 230000000630 rising effect Effects 0.000 abstract 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 33
- 239000000463 material Substances 0.000 description 10
- 238000010521 absorption reaction Methods 0.000 description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- -1 oxonium ion Chemical class 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 5
- 238000012958 reprocessing Methods 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 229910052778 Plutonium Inorganic materials 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000010808 liquid waste Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000003758 nuclear fuel Substances 0.000 description 3
- OYEHPCDNVJXUIW-UHFFFAOYSA-N plutonium atom Chemical compound [Pu] OYEHPCDNVJXUIW-UHFFFAOYSA-N 0.000 description 3
- 239000012716 precipitator Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical class [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 159000000013 aluminium salts Chemical class 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000009297 electrocoagulation Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 239000002915 spent fuel radioactive waste Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000004017 vitrification Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a defluorination method in the nitric acid evaporation recovery process, which evaporates nitric acid, defluorinates in the steam rising process, and condenses to recover nitric acid. The device used in the method comprises an evaporator and a condenser, wherein a packing column is additionally arranged at the distillation head position of the evaporator, and the rear end of the distillation head is connected with the condenser. The invention provides the defluorination method and the device which are simple and convenient to operate and good in defluorination effect and are suitable for the nitric acid evaporation recovery process in the system with higher acidity of the feed liquid.
Description
Technical field
The present invention relates to nuclear fuel reprocessing technical field, particularly in a kind of nuclear fuel reprocessing plant nitric acid utilization and recycle process, remove method and the device of fluorine.
Background technology
Typical water law aftertreatment technology flow process is that spent fuel first dissolves in nitric acid, and obtained 1AF feed liquid, then obtain high activity liquid waste and uranium, plutonium product liquid through chemical separation, the fluorion in system mainly enters high activity liquid waste.High activity liquid waste needs to carry out evaporation concentration, is utilization and recycle nitric acid wherein on the one hand, on the other hand the height after evaporation concentration is put raffinate and processes further, then carry out vitrification process.In addition, some processing unit in reprocessing plant needs to use fluorine-containing nitric acid to carry out strengthening cleaning, and this part fluorine-containing nitric acid needs utilization and recycle equally.Nitric acid is in evaporation removal process, and fluorion enters in multiplexing nitric acid by with the form of HF, and nitric acid is after repeatedly utilization and recycle, and wherein fluorinion concentration will constantly be increased accumulation, and finally causes hydrofluoric acid concentration in system more and more higher.Hydrofluoric acid has severe corrosive, will cause heavy corrosion to processing unit; And on stream due to the complexing action of fluorion, the loss of plutonium also may be caused, have influence on the yield of plutonium.Therefore, in nitric acid removal process, the removal of fluorion is very important.
At present, the fluoride ion removing method reported in document, is mainly divided into the precipitator method and absorption method.The precipitator method are removed fluorine and are mainly comprised lime method, magnesium hydroxide flocculent precipitation, aluminium salt, electrocoagulation, electroosmose process etc.Absorption method mainly comprises Defluorination of Formation Mater By Adsorption On Activated Alumina, phosphorus containg substances absorption method, sex change material except fluorine, activated magnesia are except fluorine, anionite-exchange resin are except fluorine, granular carbon are except fluorine, osmose process are except fluorine etc.But aforesaid method is all for the weak acid such as ambient water and trade effluent or weakly alkaline system, as the precipitator method need to control material liquid pH 5 ~ 9, the precipitation of generation is colloidal attitude, not easily separates out, and the treatment time is long; For absorption method except fluorine, the method for current bibliographical information is all for tap water or close to neutral wastewater treatment aspect.And in nuclear fuel reprocessing process, fluoride removing material liquid is strongly-acid system, and feed liquid composition is complicated, and for the defluorination method in higher concentration nitric acid system, there is not been reported.
Summary of the invention
Instant invention overcomes the limitation of existing defluorination method and device, provide the defluorination method in the good nitric acid evaporation removal process being applicable in the higher system of feed acidity of a kind of easy and simple to handle, defluorination effect and device.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions:
A defluorination method in nitric acid evaporation removal process, key is, is evaporated by nitric acid, and carry out except fluorine in steam uphill process, nitric acid is reclaimed in condensation.
The device that defluorination method in nitric acid evaporation removal process is used, it comprises vaporizer, condenser, and a position of heating up in a steamer for vaporizer installs filled column additional, heats up in a steamer a rear end and connects condenser.
The present invention is all right:
Described carry out in steam uphill process except fluorine be in steam uphill process by being equipped with the filler of Adsorption of fluoride, fluorine is adsorbed in filled column.Described nitric acid is carried out being evaporated to evaporate under normal pressure or reduced pressure.Describedly nitric acid is carried out be evaporated to evaporating under the out of stock condition of nitric acid.
Described filled column is built with alumina packing.Described filled column is built with zirconia filler.The outside heating jacket of described filled column or thermal insulation layer parcel.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention adopts and carries out except fluorine in uphill process at nitric acid and hydrofluoric acid vapor, and this can be avoided fluorine sorbent material to contact with evaporation the direct of feed liquid, reduces the impact on nitric acid evaporation operation, substantially can not cause interference to the technique of the evaporation concentration of nitric acid.In addition, present method to the pH value not requirement of handled fluorine-containing feed liquid, also can be used in the formaldehyde of nitric acid, formic acid or sucrose denitration evaporating concentration process except fluorine.The invention solves in reprocessing plant nitric acid multiplex process except fluorine problem.
Accompanying drawing explanation
Fig. 1 fluorine removal device structural representation
1 vaporizer, 2 filled columns, 3 condensers, 4 heat up in a steamer head, 5 and heat up in a steamer a system for detecting temperature, 6 fluid level control systems, 7 heating jackets
Embodiment
Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail:
As shown in Figure 1, it comprises vaporizer 1, condenser 3 to fluorine removal device in a kind of nitric acid evaporation removal process, and 4 position of heating up in a steamer for vaporizer 1 install filled column 2 additional, heats up in a steamer 4 rear end and connects condenser 3.The filled column 2 of defluorination material is housed as rectifying column during nitric acid evaporation removal process, the filler of the Adsorption of fluoride such as activated alumina or zirconium white is housed in filled column 2, filled column 2 outer wall can have heating jacket 7 or thermal insulation layer, to avoid nitric acid vapor condensing reflux in filler, simultaneously be provided with and heat up in a steamer a system for detecting temperature 5 heating up in a steamer 4, guarantee that steam steams smoothly.
Reclaim in nitric acid process in fluorine-containing nitric acid feed liquid evaporation, feed liquid is by thermal evaporation, steam contacts with defluorination material through filled column 2 in uphill process, fluorine will be adsorbed in filler, thus reaching the object of recovery nitric acid except fluorine, nitric acid vapor or oxynitride reclaim by condensation or other absorption patterns the nitric acid produced.Along with the carrying out of evaporation, in vaporizer 1, feed liquid reduces gradually, by fluid level control system 6 Real-Time Monitoring liquid level, when liquid level adds new fluorine-containing feed liquid lower than during certain value wherein by feed liquid transferpump, when liquid level is reinforced higher than stopping during certain value, concentrate with the consecutive evaporation realizing feed liquid.When feed liquid evaporation concentration is to after to a certain degree, will concentrate raffinate discharge by the discharge opening bottom vaporizer 1.In the process of evaporation, also can add out of stock dose of formic acid or formaldehyde etc. evaporate.
When the filling adsorption fluorine in filled column 2 reaches capacity, can unload filled column 2 regeneration filler or more renew filler again, to guarantee defluorination effect, filler regeneration or replacement cycle can be determined as the case may be.
The filler of the Adsorption of fluoride such as activated alumina or zirconium white is housed in filled column 2, to be equipped with the filled column 2 of defluorination material as rectifying column, nitric acid vapor in uphill process with defluorination material, as activated alumina contact, with the fluorine that absorption is risen with nitric acid vapor, to reach the object except fluorine.Why activated alumina has good absorption property, and this is relevant with its structure, and the aluminum oxide the first layer of surface drying is made up of oxonium ion, and oxonium ion is connected with the second aluminum ion, and its amount is only the half of second layer oxonium ion.Therefore, have the aluminum ion of half will be exposed on the surface, the oxonium ion of the second layer just in time meets Al
2o
3al/O ratio, stronger with fluorion bonding force.The research of x-ray photoelectron spectroscopy shows, the absorption of activated alumina to F-is by realizing the chemisorption of HF: Al
2o
3+ H
++ F
----Al
2o
3hF, at the Al of some hydrations
2o
3surface, F
-adsorption by hydrogen bond can be there is.Actual in fluorine operation, can form according to feed liquid system, except differences such as fluorine index and processing flux, select the parameters such as suitable filling kind, filler shape, size, amount of filler.
The heating of vaporizer 1 can adopt heating means and the modes such as electrically heated, steam heating, chuck heating and bottom-heated, in evaporative process, in vaporizer 1, feed liquid can select the mode such as magnetic agitation or mechanical stirring to mix according to situations such as concrete treatment scales, is heated evenly to improve feed liquid and evaporates.After feed liquid evaporation concentration completes, the concentrated solution in vaporizer 1 can be released by the discharge opening bottom vaporizer 1 as required, or is poured out by the opening on vaporizer 1 top or extracted out.The situations such as the actual composition of the visual feed liquid of feed liquid cycles of concentration, subsequent technique requirement are determined.
Embodiment
1) foundation of nitric acid evaporation fluorine removal device
Design and Machining capacity is the polytetrafluoro flask of 500ml; Filled column 2 is similarly polytetrafluoro material, and dimensional parameters is: φ 2.5cm*8cm, and the sieve tray of φ 1mm is made at the upper and lower two ends of pillar, and percentage of open area is 40%, and filler is the activated alumina bead of φ 2mm; Wrap up with heating jacket 7 outside filled column 2, on pillar, termination heats up in a steamer 4, after connect prolong 3 and receiving bottle etc., fluorine-containing feed liquid adopts constant temperature oil bath controller to carry out heating evaporation.
2) defluorinating process test in nitric acid evaporating concentration process
Fluorine-containing feed liquid composition: concentration of nitric acid-1.5mol/L, F--1g/L, volume is 2L altogether.
For improving the speed of nitric acid evaporation concentration, this experiment adopts distills under normal pressure or reduced pressure, be connected by the transferpump of the tank level control system 6 in flask, when material liquid volume is lower than 330mL, feed liquid transferpump brings into operation and pump into feed liquid in flask, and when in bottle, material liquid volume is greater than 380mL, feed liquid transferpump stops charging, the liquid volume in flask is made to maintain 330 ~ 380mL, until 2L feed liquid is all disposed; Out of service when being evaporated to when feed liquid in bottle is about 330mL.This experiment concentrates about 6 times to initial fluorine-containing feed liquid, collect phlegma 1.6L (all the other are about 70mL feed liquid is volatilization loss) altogether, employing ion chromatography analysis wherein fluorinion concentration is 0.013g/L, the clearance that fluorion in this experiment nitric acid evaporating concentration process is described is (1-0.013)/* 100%=98.7%, and defluorination effect is better.
Claims (5)
1. the defluorination method in nitric acid evaporation removal process, is characterized in that, evaporated by nitric acid, carry out except fluorine in steam uphill process, nitric acid is reclaimed in condensation; Describedly carry out in steam uphill process except fluorine is the sieve tray being made Ф 1mm in steam uphill process by the upper and lower two ends of filled column, percentage of open area is 40%, and the filled column that the activated alumina bead filler of Ф 2mm is housed is except fluorine, and fluorine is adsorbed in filled column.
2. defluorination method in a kind of nitric acid evaporation removal process according to claim 1, is characterized in that, described nitric acid is carried out being evaporated to evaporate under normal pressure or reduced pressure.
3. defluorination method in a kind of nitric acid evaporation removal process according to claim 1, is characterized in that, is describedly carried out by nitric acid being evaporated to evaporating under nitric acid denitration condition.
4. the device that uses of defluorination method as claimed in claim 1, it is characterized in that, it comprises vaporizer, condenser, a position of heating up in a steamer for vaporizer installs filled column additional, the sieve tray of Ф 1mm is made at the two ends up and down of filled column, percentage of open area is 40%, and filler is the aluminum oxide of Ф 2mm, heats up in a steamer a rear end and connects condenser.
5. device according to claim 4, is characterized in that, the outside heating jacket of described filled column or thermal insulation layer parcel.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210152563.3A CN103420347B (en) | 2012-05-17 | 2012-05-17 | Defluorination method and device in nitric acid evaporation recovery process |
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| CN201210152563.3A CN103420347B (en) | 2012-05-17 | 2012-05-17 | Defluorination method and device in nitric acid evaporation recovery process |
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| CN103420347A CN103420347A (en) | 2013-12-04 |
| CN103420347B true CN103420347B (en) | 2015-04-29 |
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|---|---|---|---|---|
| CN112593081B (en) * | 2020-11-09 | 2023-01-03 | 中核四0四有限公司 | Method for leaching plutonium in plutonium-containing activated carbon |
| CN112537814A (en) * | 2020-12-31 | 2021-03-23 | 江苏电科环保有限公司 | Treatment system for fluorine-containing nitric acid waste liquid |
| CN113447614B (en) * | 2021-06-21 | 2022-08-09 | 中国原子能科学研究院 | Method for measuring denitration rate in radioactive waste liquid calcination process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102247808A (en) * | 2011-06-28 | 2011-11-23 | 中国原子能科学研究院 | Separating material for separating and extracting technetium from acid solution system |
| CN102351359A (en) * | 2011-07-01 | 2012-02-15 | 清华大学 | Device and method for radioactive waste water concentration treatment |
-
2012
- 2012-05-17 CN CN201210152563.3A patent/CN103420347B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102247808A (en) * | 2011-06-28 | 2011-11-23 | 中国原子能科学研究院 | Separating material for separating and extracting technetium from acid solution system |
| CN102351359A (en) * | 2011-07-01 | 2012-02-15 | 清华大学 | Device and method for radioactive waste water concentration treatment |
Non-Patent Citations (3)
| Title |
|---|
| 低中水平放射性废液的水泥固化研究;谷万成;《湿法冶金》;20050331;第24卷(第1期);2.1废液组成，表1 * |
| 无忌离子交换材料在放射性废水处理中的演讲和应用;李楷君;《水处理技术》;19851231;第11卷(第6期);一、前言，三、氧化物 2.氧化锆和3.其他氧化物 * |
| 真空蒸发浓缩装置在核放射废水处理中的应用试验;尉凤珍等;《工业水处理》;20090930;第29卷(第9期);1 试验装置与方法 * |
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