CN103420347A - 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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- CN103420347A CN103420347A CN2012101525633A CN201210152563A CN103420347A CN 103420347 A CN103420347 A CN 103420347A CN 2012101525633 A CN2012101525633 A CN 2012101525633A CN 201210152563 A CN201210152563 A CN 201210152563A CN 103420347 A CN103420347 A CN 103420347A
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- nitric acid
- defluorination
- filled column
- evaporated
- feed liquid
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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 52
- 229910017604 nitric acid Inorganic materials 0.000 title claims abstract description 52
- 238000006115 defluorination reaction Methods 0.000 title claims abstract description 42
- 238000001704 evaporation Methods 0.000 title claims abstract description 29
- 230000008020 evaporation Effects 0.000 title claims abstract description 25
- 238000011084 recovery Methods 0.000 title abstract 3
- 238000012856 packing Methods 0.000 claims abstract description 3
- 230000000630 rising effect Effects 0.000 claims abstract description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 17
- 239000011737 fluorine Substances 0.000 claims description 17
- 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
- 238000001179 sorption measurement Methods 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 36
- 230000000694 effects Effects 0.000 abstract description 7
- 238000004821 distillation Methods 0.000 abstract 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 16
- 239000000463 material Substances 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 6
- -1 oxonium ion Chemical class 0.000 description 6
- 238000012958 reprocessing Methods 0.000 description 5
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 229910052778 Plutonium Inorganic materials 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
- 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
- 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
- 150000002222 fluorine compounds Chemical class 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 239000000203 mixture Substances 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
- 229930006000 Sucrose Natural products 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
- 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
- 238000013459 approach Methods 0.000 description 1
- 239000011324 bead Substances 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
- 239000012141 concentrate Substances 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
- 238000002309 gasification Methods 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
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000002994 raw material 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
- 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
- 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
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (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 the nuclear fuel reprocessing technical field, particularly a kind of nuclear fuel reprocessing plant nitric acid reclaims method and the device of defluorination in multiplex process.
Background technology
Typical water law aftertreatment technology flow process is that spent fuel first dissolves in nitric acid, makes the 1AF feed liquid, then through chemical separation, obtains high activity liquid waste and uranium, plutonium product liquid, and the fluorion in system mainly enters high activity liquid waste.High activity liquid waste need to carry out evaporation concentration, is to reclaim multiplexing nitric acid wherein on the one hand, on the other hand the height after evaporation concentration is put to raffinate and further processes, and then carries out the vitrification processing.In addition, some processing unit in reprocessing plant need to be used fluorine-containing nitric acid to strengthen cleaning, and this part fluorine-containing nitric acid need to reclaim multiplexing equally.Nitric acid is in the evaporation removal process, and fluorion will enter with the form of HF in multiplexing nitric acid, nitric acid repeatedly reclaim multiplexing after, wherein fluorinion concentration will constantly be increased accumulation, and finally cause in system hydrofluoric acid concentration 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, also may cause the loss of plutonium, have influence on the yield of plutonium.Therefore, in the nitric acid removal process, the removal of fluorion is very important.
At present, the fluoride ion removing method of reporting in document, mainly be divided into the precipitator method and absorption method.Precipitator method defluorination mainly comprises 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 defluorination, activated magnesia defluorination, anionite-exchange resin defluorination, granular carbon defluorination, osmose process defluorination etc.But aforesaid method is all for weak acid or weakly alkaline systems such as ambient water and trade effluents, need to control material liquid pH 5～9 as the precipitator method, the precipitation of generation is colloidal attitude, be difficult for separating out, and the treatment time is long; For the absorption method defluorination, at present the method for bibliographical information is all for tap water or approach neutral wastewater treatment aspect.And, in nuclear fuel reprocessing process, the defluorination feed liquid is the strongly-acid system, and the feed liquid composition is complicated, for the defluorination method in the higher concentration nitric acid system, there is not yet report.
Summary of the invention
The present invention has overcome the limitation of existing defluorination method and device, provides a kind of nitric acid be applicable in the higher system of feed acidity easy and simple to handle, that defluorination effect is good to evaporate defluorination method and the device in removal process.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions:
Defluorination method in a kind of nitric acid evaporation removal process, key is, nitric acid is evaporated, and carries out defluorination in the steam uphill process, nitric acid is reclaimed in condensation.
Defluorination method device used in a kind of nitric acid evaporation removal process, it comprises vaporizer, condenser, a position of heating up in a steamer of vaporizer installs filled column additional, heats up in a steamer a rear end and connects condenser.
The present invention is all right:
Described in the steam rising process, carry out defluorination in the steam uphill process by the filler of Adsorption of fluoride is housed, fluorine is adsorbed in filled column.Described nitric acid is evaporated under normal pressure or reduced pressure and is evaporated.Described nitric acid is evaporated under the out of stock condition of nitric acid and is evaporated.
Described filled column is in-built alumina packing.Described filled column is in-built zirconia filler.Heating jacket or thermal insulation layer parcel for the outside of described filled column.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention adopts and to carry out defluorination at nitric acid and hydrofluoric acid vapor in uphill process, and this can be avoided the fluorine sorbent material to contact with evaporating the direct of feed liquid, and the impact of minimizing on the nitric acid evaporation operation can not cause interference to the technique of the evaporation concentration of nitric acid substantially.In addition, present method does not require the pH value of handled fluorine-containing feed liquid, can be used for the defluorination in formaldehyde, formic acid or the sucrose denitration evaporating concentration process of nitric acid yet.The invention solves the defluorination problem in reprocessing plant nitric acid multiplex process.
The 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 of vaporizer 1 install filled column 2 additional, heat up in a steamer 4 rear end and connect condenser 3.The rectifying column of the filled column 2 that defluorination material is housed during as nitric acid evaporation removal process, the filler of the Adsorption of fluorides such as activated alumina or zirconium white is housed in filled column 2, filled column 2 outer walls can have heating jacket 7 or thermal insulation layer, to avoid nitric acid vapor condensing reflux in filler, simultaneously be equipped with and heat up in a steamer a system for detecting temperature 5 heating up in a steamer 4, guarantee that steam steams smoothly.
In the nitric acid process is reclaimed in fluorine-containing nitric acid feed liquid evaporation, the feed liquid gasification of being heated, steam contacts with defluorination material through filled column 2 in uphill process, fluorine will be adsorbed in filler, thereby reach the purpose that reclaims the nitric acid defluorination, nitric acid vapor or oxynitride reclaim by condensation or other absorption patterns the nitric acid produced.Carrying out along with evaporation, in vaporizer 1, feed liquid reduces gradually, can pass through fluid level control system 6 Real-Time Monitoring liquid levels, wherein add new fluorine-containing feed liquid by the feed liquid transferpump when liquid level during lower than certain value, when liquid level, stop feeding in raw material during higher than certain value, concentrated with the consecutive evaporation that realizes feed liquid., can will concentrate by the discharge opening of vaporizer 1 bottom raffinate and discharge to after to a certain degree when the feed liquid evaporation concentration.In the process of evaporation, also can add out of stock dose of formic acid or formaldehyde etc. to be evaporated.
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 fluorides such as activated alumina or zirconium white is housed in filled column 2, using defluorination material is housed filled column 2 as rectifying column, nitric acid vapor in uphill process with defluorination material, as activated alumina contact, the fluorine risen with nitric acid vapor with absorption, to reach the purpose of defluorination.Why activated alumina has absorption property preferably, and this structure with it is relevant, and the aluminum oxide the first layer of surface drying consists of oxonium ion, and oxonium ion is connected with the second aluminum ion, and its amount is only half of second layer oxonium ion.Therefore, have the aluminum ion of half will be exposed to surface above, the oxonium ion of the second layer just in time meets Al
2O
3The Al/O ratio, stronger with the fluorion bonding force.The research of x-ray photoelectron spectroscopy shows, activated alumina is to realize by the chemisorption to HF to the absorption of F-: Al
2O
3+ H
++ F
----Al
2O
3HF, at the Al of some hydrations
2O
3Surface, F
-Adsorption by hydrogen bond can occur.In actual defluorination operation, can, according to differences such as feed liquid composing system, defluorination 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 modes such as magnetic agitation or mechanical stirring to be mixed according to situations such as concrete treatment scales, to improve feed liquid, is heated evenly and evaporates.After the feed liquid evaporation concentration completes, the concentrated solution in vaporizer 1 can be emitted by the discharge opening of vaporizer 1 bottom as required, or pours out or extract out by the opening on vaporizer 1 top.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
The polytetrafluoro flask that the Design and Machining capacity is 500ml; Filled column 2 is similarly the 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%, the activated alumina bead that filler is φ 2mm; Heating jackets 7 parcel for filled column 2 outsides, on pillar, termination heats up in a steamer 4, after connect prolong 3 and receiving bottle etc., fluorine-containing feed liquid employing constant temperature oil bath controller carries out heating evaporation.
2) defluorinating process test in the nitric acid evaporating concentration process
Fluorine-containing feed liquid forms: concentration of nitric acid-1.5mol/L, and F--1g/L, volume is 2L altogether.
For improving the speed of nitric acid evaporation concentration, this experiment adopts is distilled under normal pressure or reduced pressure, transferpump by the tank level control system 6 in flask is connected, when material liquid volume during lower than 330mL, the feed liquid transferpump brings into operation and pump into feed liquid in flask, and when in bottle, material liquid volume is greater than 380mL, the feed liquid transferpump stops charging, make the liquid volume in flask maintain 330～380mL, until the 2L feed liquid all is disposed; It is out of service when in being evaporated to bottle, feed liquid is about 330mL.This experiment has concentrated approximately 6 times to initial fluorine-containing feed liquid, collect altogether phlegma 1.6L (all the other about 70mL feed liquids are volatilization loss), 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 (8)
1. a nitric acid evaporates the defluorination method in removal process, it is characterized in that, nitric acid is evaporated, and carries out defluorination in the steam uphill process, and nitric acid is reclaimed in condensation.
2. defluorination method in a kind of nitric acid evaporation removal process according to claim 1, is characterized in that, described in the steam rising process, carry out defluorination in the steam uphill process by the filler of Adsorption of fluoride is housed, fluorine is adsorbed in filled column.
3. defluorination method in a kind of nitric acid evaporation removal process according to claim 1, is characterized in that, described nitric acid is evaporated under normal pressure or reduced pressure and is evaporated.
4. defluorination method in a kind of nitric acid evaporation removal process according to claim 1, is characterized in that, described nitric acid is evaporated under the out of stock condition of nitric acid and is evaporated.
5. the device that claim 1 is used, is characterized in that, it comprises vaporizer, condenser, and a position of heating up in a steamer of vaporizer installs filled column additional, heats up in a steamer a rear end and connect condenser.
6. device according to claim 5, is characterized in that, described filled column is in-built alumina packing.
7. device according to claim 5, is characterized in that, described filled column is in-built zirconia filler.
8. device according to claim 5, is characterized in that, heating jacket or thermal insulation layer parcel for the outside of described filled column.
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| Application Number | Priority Date | Filing Date | Title |
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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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| CN201210152563.3A CN103420347B (en) | 2012-05-17 | 2012-05-17 | Defluorination method and device in nitric acid evaporation recovery process |
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| Publication Number | Publication Date |
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| CN103420347A true CN103420347A (en) | 2013-12-04 |
| CN103420347B CN103420347B (en) | 2015-04-29 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112593081A (en) * | 2020-11-09 | 2021-04-02 | 中核四0四有限公司 | Method for leaching plutonium in plutonium-containing activated carbon |
| CN113447614A (en) * | 2021-06-21 | 2021-09-28 | 中国原子能科学研究院 | Method for measuring denitration rate in radioactive waste liquid calcination process |
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| 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 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112593081A (en) * | 2020-11-09 | 2021-04-02 | 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 |
| CN112537814B (en) * | 2020-12-31 | 2024-07-23 | 江苏电科环保有限公司 | Treatment system for fluorine-containing nitric acid waste liquid |
| CN113447614A (en) * | 2021-06-21 | 2021-09-28 | 中国原子能科学研究院 | Method for measuring denitration rate in radioactive waste liquid calcination process |
| 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 |
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