CN104328291B - A kind of oxidation price modification equipment Pu (III) being oxidizing to Pu (IV) - Google Patents

A kind of oxidation price modification equipment Pu (III) being oxidizing to Pu (IV) Download PDF

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CN104328291B
CN104328291B CN201410558430.5A CN201410558430A CN104328291B CN 104328291 B CN104328291 B CN 104328291B CN 201410558430 A CN201410558430 A CN 201410558430A CN 104328291 B CN104328291 B CN 104328291B
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tower
oxidizing
iii
oxidizing tower
feed liquid
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CN104328291A (en
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常尚文
周贤明
何辉
李高亮
兰天
刘金平
唐洪彬
郑卫芳
孟照凯
陈志旭
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China Institute of Atomic of Energy
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China Institute of Atomic of Energy
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Abstract

The invention belongs to nuclear fuel post-processing technology field, disclose a kind of oxidation price modification equipment Pu (III) being oxidizing to Pu (IV).This equipment mainly comprises oxidizing tower, feed liquid receiving tank and NO xstorage tank, wherein the upper end of oxidizing tower is provided with material liquid outlet, and lower end is provided with Pu (III) liquor inlet and NO xcharging aperture, feed liquid receiving tank is connected by pipeline with the material liquid outlet on the top of oxidizing tower; Filler in the main body of oxidizing tower, tower is resistance to irradiation, the corrosion material of resistance to nitric acid; The outer tower wall of oxidizing tower is provided with heating arrangement; Pu (III) feed liquid enters in oxidizing tower from Pu (III) liquor inlet of oxidizing tower bottom; NO xthe NO that storage tank provides xgas is separately or with carrier gas together by the NO of oxidizing tower bottom xcharging aperture enters in oxidizing tower; Feed liquid after price modification enters feed liquid receiving tank via the material liquid outlet on oxidizing tower top.This equipment has that treatment scale is large, NO xutilization factor is high, price modification process safety is stablized and oxides of nitrogen tail gas disposes the little advantage of burden.

Description

A kind of oxidation price modification equipment Pu (III) being oxidizing to Pu (IV)
Technical field
The invention belongs to nuclear fuel post-processing technology field, be specifically related to the oxidation price modification equipment that 1BP to 2AF and plutonium precipitation in nuclear fuel aftertreatment Purex flow transform plutonium in front 2BP feed liquid.
Background technology
Aftertreatment technology flow process adopts U (IV)-hydrazine, azanol-hydrazine or N usually, the reductive agents such as N-dimethyl hydroxylamine-methyl hydrazine carry out reduction reextraction Pu (III), in the 1BP feed liquid that uranium plutonium obtains after being separated, plutonium is trivalent, next step to be undertaken by extraction and back extraction the purification of plutonium concentrated before, Pu (III) need be adjusted to Pu (IV); Nitric acid Pu (III) solution that plutonium purification cycle obtains simultaneously needs to be converted into Pu (IV) when precipitating step of converting.Traditional aftertreatment technology flow process adopts sodium nitrite (NaNO 2) adjust the valence state (adopt Flavouring jar, batch operate) of plutonium in 1BP, 2BP feed liquid, by NaNO 2add in the Flavouring jar that 1BP, 2BP feed liquid is housed, Oxidative demage reductive agent wherein and holding reductant, thus oxidation Pu (III) is Pu (IV).But this method is equivalent to introduce salt in system, be unfavorable for the process that aftertreatment flow process is follow-up.
There are some researches show that NOx (oxides of nitrogen) can be used for oxidation and regulates plutonium valence state at present, if but directly NOx is passed in Pu (III) feed liquid, react oxides of nitrogen gas a large amount of for effusion, both caused the utilization factor of NOx to reduce, tail gas can be increased the weight of again and dispose burden.For this reason, need to set up suitable price modification equipment with the continued operation of the technique that realizes readjusting prices on a large scale, improve the utilization factor of NOx, reduce the disposal burden of oxides of nitrogen tail gas.
Summary of the invention
(1) goal of the invention
Problem existing for prior art, the present invention establishes that a kind for the treatment of scale is large, NOx utilization factor is high, price modification process safety is stablized and oxides of nitrogen tail gas disposes little oxidation price modification equipment Pu (III) being oxidizing to Pu (IV) of burden.
(2) technical scheme
In order to solve the problem existing for prior art, the present invention is achieved by the following technical solutions:
A kind of oxidation price modification equipment Pu (III) being oxidizing to Pu (IV), key is, this equipment mainly comprises oxidizing tower, feed liquid receiving tank and NO xstorage tank, wherein the upper end of oxidizing tower is provided with material liquid outlet, and lower end is provided with Pu (III) liquor inlet and NO xcharging aperture, feed liquid receiving tank is connected by pipeline with the material liquid outlet on the top of oxidizing tower; Filler in the main body of oxidizing tower, tower is resistance to irradiation, the corrosion material of resistance to nitric acid; The outer tower wall of oxidizing tower is provided with heating arrangement; Pu (III) feed liquid enters in oxidizing tower from Pu (III) liquor inlet of oxidizing tower bottom; NO xthe NO that storage tank provides xgas is separately or with carrier gas together by the NO of oxidizing tower bottom xcharging aperture enters in oxidizing tower, NO xgas fully contacts with Pu (III) feed liquid and reacts with feed liquid in uphill process; Feed liquid after price modification enters feed liquid receiving tank via the material liquid outlet on oxidizing tower top, and the tail gas generated in price modification process enters exhaust treatment system by tower top.
Preferably, oxidizing tower inside is also provided with one or more sieve plate and is separated by filler.
Preferably, NO xthe pipeline that gas enters oxidizing tower tower body is inverted U pipe, pours in down a chimney enter NO to prevent feed liquid xstorage tank and inverted U pipe pipeline peak are higher than material liquid outlet 200 ~ 400mm.
Preferably, NO xfor NO, NO 2or N 2o 4, work as NO xfor N 2o 4time, first will be positioned at N 2o 4n in storage tank 2o 4liquid enters gasification tank through pipeline and NOx syringe pump and in gasification tank, is heated to 70 ~ 90 DEG C of N obtained 2o 4again by NO after gas xcharging aperture enters in oxidizing tower.
Preferably, NO xwith carrier gas jointly by NO xcharging aperture enters in tower, and wherein carrier gas is air or oxygen, works as NO xduring for NO, in carrier gas, oxygen content is NO x1 ~ 3 times; Work as NO xfor N 2o 4or NO 2time, in carrier gas, oxygen content is NO x0 ~ 3 times.
Preferably, the type of heating of gasification tank is electrical heating or heating water bath; The heating arrangement that the outer tower wall of oxidizing tower is arranged for being wound with heat tape or heating water jacket, or arranges electric boiling plate on outer tower wall, makes feed temperature in tower be 30 ~ 50 DEG C
Preferably, being provided with the material of Absorbable rod neutron at the middle part of oxidizing tower or tower wall, wherein absorbing the material of neutron for containing 10b or 6the material of Li.
Preferably, the tower top of oxidizing tower is provided with demister, the feed liquid drop carried secretly with gas in separation of oxygenated tower.
Preferably, be equipped with cyclone separator in demister rear end, enter exhaust treatment system by after the drop separation in tail gas further.
Preferably, the pipeline that Pu (III) feed liquid enters oxidizing tower by feed liquid discharge pump is inverted U pipeline.
Preferably, resistance to irradiation, the corrosion material of resistance to nitric acid are stainless steel.
Preferably, being oxidized inner-tower filling material is the western tower ring of stainless steel.
(3) beneficial effect
Equipment Pu (III) being oxidizing to Pu (IV) provided by the invention, it adopts tower oxidation equipment and is furnished with NO xstorage tank, demister, cyclone separator, temperature and pressure-measuring device etc., improve treatment scale, makes the utilization factor of NOx improve about 30%, and decrease the disposal burden of oxides of nitrogen tail gas, ensure that the safe and stable operation of price modification technique, specific explanations is:
1) NOx and carrier gas together enter in oxidizing tower, improve the utilization factor of NOx.This mainly generates nitrous acid, the reaction such as reductive agent azanol, hydrazine, U (IV) in nitrous acid and 1BP feed liquid due to the water reaction in NOx and 1BP feed liquid, generates NO and other products, and the NO of generation generates NO with the oxygen reaction in carrier gas again 2, NO 2can react with the water in feed liquid again and generate nitrous acid, so repeatedly, make the utilization factor of NOx improve about 30%, decrease the disposal burden of oxides of nitrogen tail gas.
2) during extensive price modification process, filler in tower too much to cause at the bottom of tower burden heavy and the inner-tower filling material problem of sinking because of Action of Gravity Field, by arranging sieve plate in the filler of oxidizing tower inside, alleviate the heavy burden burden at the bottom of tower, also make the distribution of the filler in oxidizing tower in tower more stable simultaneously.
3) heating arrangement is set on oxidizing tower outer tower wall, for the feed liquid in oxidizing tower heats up, makes reaction more quick, and nitrous acid concentration reduction in feed liquid after oxidation is readjusted prices, alleviate follow-up nitrous acid and catch up with the burden removed.
4) oxides of nitrogen gas enters oxidizing tower and adopts the pipe of falling U mode to enter, and the peak of pipeline exceeds material liquid outlet height 200 ~ 400mm, and on pipeline, retaining valve is installed, prevent feed liquid from being refunded in gasification tank by oxides of nitrogen conveyance conduit in operational process.
5) during extensive price modification process, there is criticality safety problem in plutonium feed liquid, and the application can head it off by the material arranging Absorbable rod neutron in the middle of oxidizing tower or on tower wall.
Accompanying drawing explanation
Fig. 1 is the oxidation price modification equipment schematic diagram that the application provides,
Wherein 1.NOx syringe pump; 2.NOx storage tank; 3. gasification tank; 4. fan blower; 5. oxidizing tower; 6.NO xcharging aperture; 7. bottom temp measuring instrument; 8. base pressure measuring instrument; 9. filler; 10. electric boiling plate; 11. retaining valves; 12. head temperature measuring instruments; 13. top pressure measuring instruments; 14. demisters; 15. cyclone separators; 16. tail gas; 17. material liquid outlets; 18. retaining valves; 19. flowmeters; 20. feed liquid receiving tanks; 21. feed liquid discharge pumps; 22.Pu (III) liquor inlet.
Embodiment
Below in conjunction with Figure of description and specific embodiment, the present invention is further elaborated.
Embodiment 1
A kind of oxidation price modification equipment Pu (III) being oxidizing to Pu (IV), as shown in Figure 1, this equipment mainly comprises oxidizing tower 5, feed liquid receiving tank 20 and NO xstorage tank 2, wherein the upper end of oxidizing tower 5 is provided with material liquid outlet 17, and lower end is provided with Pu (III) liquor inlet 22 and NO xcharging aperture 6, feed liquid receiving tank 20 is connected by pipeline with the material liquid outlet 17 on the top of oxidizing tower 5; Filler wherein in the main body of oxidizing tower 5, tower is resistance to irradiation, the western tower ring of resistance to nitric acid corrosion stainless steel; The outer tower wall of oxidizing tower 5 is provided with electric boiling plate 10, makes feed temperature in tower be 40 DEG C; The material of Absorbable rod neutron is provided with at the middle part of oxidizing tower 5 10b 4c.The tower top of oxidizing tower 5 is provided with demister 14, the feed liquid of carrying secretly with gas in separation of oxygenated tower 5, is equipped with cyclone separator 15 in demister 14 rear end, is separated feed liquid drop and tail gas further.The top of oxidizing tower 5 and bottom are all provided with temperature and pressure measuring instrument, for the temperature, pressure situation in Real-Time Monitoring course of reaction, to instruct the safe and stable operation of whole condiment technique.
Pu (III) feed liquid enters in the tower of oxidizing tower 5 from Pu (III) liquor inlet 22 of oxidizing tower 5 bottom, and its pipeline entering oxidizing tower 5 by feed liquid discharge pump 21 is inverted U pipeline.
NO xthe gas that storage tank 2 provides is by the NO of oxidizing tower 5 bottom xcharging aperture 6 enters oxidizing tower 5 tower body, fully contacts and react with feed liquid with Pu (III) feed liquid in uphill process; Feed liquid after price modification enters feed liquid receiving tank 20 via the material liquid outlet 17 on oxidizing tower 5 top.Wherein, described NO xfor N 2o 4, be positioned at NO xn in storage tank 2 2o 4liquid is through pipeline and NO xsyringe pump enters gasification tank 3 and be heated to 70 DEG C of N obtained by Electric heating in gasification tank 3 2o 4gas, N 2o 4the air that gas provides with fan blower again through inverted U pipeline jointly to enter in oxidizing tower 5 and inverted U pipe pipeline peak higher than material liquid outlet 200mm, prevent feed liquid from pouring in down a chimney and enter NO xstorage tank 2.
When utilizing this price modification operate, carry out according to following steps:
(1) open gasification tank electrical heating controller, arranging heating-up temperature is 70 DEG C;
(2) opening the heating of oxidizing tower electric boiling plate makes feed temperature in tower be 40 DEG C;
(3) NO is opened xsyringe pump, the flow arranging fan blower makes oxygen content and N in carrier gas 2o 4content is identical, after gas speed is steady, open feed liquid discharge pump; N 2o 4gas fully contacts with Pu (III) feed liquid and reacts with feed liquid in uphill process; Feed liquid after price modification enters feed liquid receiving tank via the material liquid outlet on oxidizing tower top; Tail gas enters exhaust treatment system through cyclone separator.
(4) the pressure, temperature variation situation of observing oxidizing tower in price modification process is oxidized; During end of run, oxidizing tower should close down feed liquid discharge pump, NO successively xsyringe pump, NO xthe heating of storage tank, oxidizing tower, gasification tank heating, emptying oxidizing tower, releases feed liquid residual in tower from tower bottom liquid outlet.
Adopt this equipment to carry out the price modification of Pu (III) feed liquid, make NO xutilization factor improves about 30%, and treatment scale is 100L/h, can guarantee that the oxygenation efficiency of Pu (III) is greater than 99.9%.
Embodiment 2
As different from Example 1, oxidizing tower 5 inside is also provided with one or more sieve plate and is separated by filler; The type of heating of gasification tank 3 is heating water bath, and heating-up temperature is 90 DEG C; The type of heating of oxidizing tower 5, for be wound around one deck heating water jacket on outer tower wall, makes feed temperature in tower be 50 DEG C; The material of the Absorbable rod neutron that oxidizing tower 5 tower wall is placed is 6liF; NO xgas enter oxidizing tower tower body via the peak of inverted U pipe higher than material liquid outlet 300mm.
Embodiment 3
As different from Example 1, the type of heating of oxidizing tower 5 is that outer tower wall is wound around one deck heat tape, makes feed temperature in tower be 40 DEG C; NO xfor NO, NO and oxygen are jointly by NO xcharging aperture enters in tower, and wherein oxygen content is 2 times of NO; NO xgas enter oxidizing tower tower body via the peak of inverted U pipe higher than material liquid outlet 400mm.
Embodiment 4
As different from Example 1, the NO passed in oxidizing tower 5 xfor NO, NO and air are jointly by NO xcharging aperture enters in tower, and wherein content of oxygen in air is 3 times of NO.
Embodiment 5
As different from Example 1, NO xfor NO 2, NO 2with oxygen jointly by NO xcharging aperture enters in tower, and wherein oxygen content is NO 21 times.
Embodiment 6
As different from Example 1, NO xfor NO 2, and do not pass into carrier gas.

Claims (10)

1. Pu (III) is oxidizing to an oxidation price modification equipment of Pu (IV), it is characterized in that, this equipment comprises oxidizing tower, feed liquid receiving tank and NO xstorage tank, wherein the upper end of oxidizing tower is provided with material liquid outlet, and lower end is provided with Pu (III) liquor inlet and NO xcharging aperture, feed liquid receiving tank is connected by pipeline with the material liquid outlet on the top of oxidizing tower; Filler wherein in the main body of oxidizing tower, oxidizing tower is resistance to irradiation and the corrosion material of resistance to nitric acid; The outer tower wall of oxidizing tower is provided with heating arrangement; Pu (III) feed liquid enters in oxidizing tower from Pu (III) liquor inlet of oxidizing tower bottom; NO xthe NO that storage tank provides xgas is separately or with carrier gas together by the NO of oxidizing tower bottom xcharging aperture enters in oxidizing tower, NO xgas fully contacts with Pu (III) feed liquid and reacts with feed liquid in uphill process; Feed liquid after price modification enters feed liquid receiving tank via the material liquid outlet on oxidizing tower top, and the tail gas generated in price modification process enters exhaust treatment system by tower top.
2. Pu (III) is oxidizing to the oxidation price modification equipment of Pu (IV) by one according to claim 1, and it is characterized in that, described oxidizing tower inside is also provided with one or more sieve plate and is separated by filler.
3. Pu (III) is oxidizing to the oxidation price modification equipment of Pu (IV) by one according to claim 1, it is characterized in that, described NO xthe pipeline that gas enters oxidizing tower tower body be inverted U pipe and inverted U pipe pipeline peak higher than material liquid outlet 200 ~ 400mm.
4. Pu (III) is oxidizing to the oxidation price modification equipment of Pu (IV) by the one according to claim 1 or 3, it is characterized in that, described NO xfor NO, NO 2or N 2o 4, work as NO xfor N 2o 4time, first will be positioned at N 2o 4n in storage tank 2o 4liquid enters gasification tank through pipeline and NOx syringe pump and in gasification tank, is heated to 70 ~ 90 DEG C of N obtained 2o 4again by NO after gas xcharging aperture enters in oxidizing tower.
5. Pu (III) is oxidizing to the oxidation price modification equipment of Pu (IV) by one according to claim 1, it is characterized in that, described NO xwith carrier gas together by NO xcharging aperture enters in tower, and wherein carrier gas is air or oxygen, works as NO xduring for NO, in carrier gas, oxygen content is NO x1 ~ 3 times; Work as NO xfor N 2o 4or NO 2time, in carrier gas, oxygen content is NO x0 ~ 3 times.
6. Pu (III) is oxidizing to the oxidation price modification equipment of Pu (IV) by one according to claim 4, and it is characterized in that, the type of heating of described gasification tank is electrical heating or heating water bath.
7. Pu (III) is oxidizing to the oxidation price modification equipment of Pu (IV) by one according to claim 1, it is characterized in that, the heating arrangement that the outer tower wall of described oxidizing tower is arranged is for being wound with heat tape or heating water jacket, or electric boiling plate is set on outer tower wall, make feed temperature in tower be 30 ~ 50 DEG C.
8. Pu (III) is oxidizing to the oxidation price modification equipment of Pu (IV) by one according to claim 1, it is characterized in that, is provided with the material of Absorbable rod neutron at the middle part of described oxidizing tower or tower wall.
9. Pu (III) is oxidizing to the oxidation price modification equipment of Pu (IV) by one according to claim 1, and it is characterized in that, the tower top of described oxidizing tower is provided with demister, is equipped with cyclone separator in demister rear end.
10. Pu (III) is oxidizing to the oxidation price modification equipment of Pu (IV) by one according to claim 1, and it is characterized in that, the pipeline that described Pu (III) feed liquid enters oxidizing tower by feed liquid discharge pump is inverted U pipeline.
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CN104789782A (en) * 2015-04-10 2015-07-22 中国原子能科学研究院 BP price-adjusting, degassing and acid-adjusting integrated device and method in Purex process
CN106884098A (en) * 2015-12-15 2017-06-23 中核四○四有限公司 A kind of system and method for the price adjustment of feed liquid containing plutonium
CN107369486B (en) * 2017-07-27 2019-05-24 中国原子能科学研究院 The adjusting of 2AF and OF feed liquid prepares integrated system in a kind of aftertreatment technology process
CN108682466B (en) * 2018-05-22 2020-10-09 中国原子能科学研究院 Oxidation device and method for plutonium-containing feed liquid
CN108922645A (en) * 2018-08-23 2018-11-30 中国原子能科学研究院 The adjusting preparation facilities of 2AF feed liquid in nuclear fuel aftertreatment technology process
CN111640520B (en) * 2020-04-26 2022-07-01 中国原子能科学研究院 Device and method for adjusting valence states of neptunium and plutonium in hot chamber
CN113990543B (en) * 2021-10-29 2024-03-19 中国核电工程有限公司 Post-treatment continuous oxidation price adjustment system and oxidation price adjustment method

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