CN103714876A - Method for removing nitrous acid - Google Patents

Method for removing nitrous acid Download PDF

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Publication number
CN103714876A
CN103714876A CN201410005672.1A CN201410005672A CN103714876A CN 103714876 A CN103714876 A CN 103714876A CN 201410005672 A CN201410005672 A CN 201410005672A CN 103714876 A CN103714876 A CN 103714876A
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nitrous acid
air
filled column
material liquid
ring filler
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CN201410005672.1A
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CN103714876B (en
Inventor
李高亮
何辉
常尚文
兰天
陈志旭
孟照凯
常利
唐洪彬
王孝荣
郑卫芳
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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 relates to a method for removing chemical substances in a solution. In order to solve the problem that in the prior art, a method which is used for removing nitrous acid in an air carrying band and is suitable for actual application does not exist, and in order to improve the rate for removing the nitrous acid under the premise that radiating operation is facilitated, the method for removing the nitrous acid is provided. The method comprises the following steps that first, a filled column is arranged, and the filled column is filled with stainless steel theta-ring filler or glass theta-ring filler; second, air is blown into the filled column form an air inlet through an air blower; third, material liquid with the nitrous acid to be removed is led into the filled column from a material liquid inlet through a charge pump, and the nitrous acid is removed. According to the method for removing the nitrous acid, the nitrous acid is removed in the air carrying band mode, the concentration of the nitrous acid in the material liquid can be lower than 1.0*10-3mol/L, the method is suitable for radiating operation, operation is convenient, cost is low, and the method can be used for removing the nitrous acid in 1 BP material liquid.

Description

A kind of removal methods of nitrous acid
Technical field
The present invention relates to the removal methods of chemical substance in a kind of solution, particularly a kind of removal methods of nitrous acid.
Background technology
In nuclear fuel reprocessing process, the plutonium head product (1BP) obtaining after uranium plutonium codecontamination separating cycle contains trivalent plutonium, thereafter, trivalent plutonium need be oxidizing to tetravalence so that further abstraction purification.Because the oxidation of plutonium adopts oxides of nitrogen or nitrite as oxygenant conventionally, therefore can residual a large amount of nitrous acid in the solution after oxidation.These residual nitrous acid can enter organic phase in follow-up extraction process, then in the back extraction process of plutonium, consume reductive agent, affect the reduction reextraction effect of plutonium, can cause the reduction of plutonium back extraction ratio and the recovery when serious.Therefore in order to reduce the impact of residual nitrous acid, the nitrous acid in the 1BP feed liquid after oxidation price modification need be removed to reduced levels.
At present, in nitric acid system, the removal methods of nitrous acid mainly comprises air carrying band removal method, vacuumize degassing method, ultrasonic degas method and heating.Vacuumize degassing method is to utilize to vacuumize the amount of nitrogen oxides reducing in gas phase, promotes nitrous acid to resolve into oxides of nitrogen and enters gas phase, thereby the nitrous acid in solution is removed; Ultrasonic degas method is to utilize ultrasound wave to accelerate the molecular motion in solution, and nitrous acid becomes unstable being decomposed and removes from solution, but vacuumize degassing method and ultrasonic degas method equipment are complicated, are unfavorable for hot operation; Heating is to make the nitrous acid in system resolve into oxides of nitrogen by heated solution, oxides of nitrogen is overflowed from solution, thereby reaches removal object, but the speed of heating removal nitrous acid is slower, and during heating, easily the plutonium in feed liquid is oxidizing to sexavalence, affects subsequent technique.
Air carrying band removal method is mode by blasting air by the nitrous acid in solution with the form carrier band of oxides of nitrogen out, and its method is easy, and the feature of synthesise various, is more suitable in hot operation.But due to the restriction of the factors such as technical field, therefore not yet find the comparatively concrete application in nuclear fuel aftertreatment field of air carrying band removal method, the removal methods that therefore need to develop a kind of nitrous acid is to be suitable for practical application.
Summary of the invention
The air carrying band that is not suitable for practical application for solving in prior art removes the method for nitrous acid, and for the removal efficiency being convenient to improve under the prerequisite of hot operation nitrous acid, the invention provides a kind of removal methods of nitrous acid.
A removal methods for nitrous acid, the method comprises the following steps:
(1) filled column is set, stainless steel θ ring filler or glass θ ring filler are housed in filled column, filled column top is provided with liquor inlet and air out, and filled column bottom is provided with material liquid outlet and air in;
(2) by fan blower, by air in, in filled column, blast air, and adopt gas meter to realize the monitoring of air mass flow and adjusting;
(3) by charge pump by liquor inlet to the feed liquid that passes into nitrous acid to be removed in filled column; The air adopting, material liquid volume throughput ratio are: (180-230): 1, and the volumescope that wherein volume of air is depressed with 1 normal atmosphere; Now, the feed liquid of nitrous acid to be removed and air carry out gas-liquid counter current on stainless steel θ ring filler or glass θ ring filler surface and contact, nitrous acid is decomposed into oxides of nitrogen gas at filling surface, and by air by oxides of nitrogen carrier band out, thereby realize removing of nitrous acid.
Described air, material liquid volume throughput ratio are preferably: 200:1.
The removal methods of nitrous acid of the present invention removes nitrous acid in the mode of air carrying band, by the processing of this method, can make the concentration of nitrous acid in feed liquid lower than 1.0 * 10 -3mol/L.Practical using result demonstration, the removal methods of nitrous acid of the present invention is comparatively suitable for hot operation, and easy to operate, with low cost, and the nitrous acid can be used in 1BP feed liquid is removed.
Accompanying drawing explanation
The process diagram of the removal methods of Fig. 1 nitrous acid of the present invention.
Reference numeral: 1. filled column, 2. air out, 3. charge pump, 4. gas meter, 5. fan blower, 6. material liquid outlet, 7. liquor inlet, 8. air in.
Embodiment
Below in conjunction with accompanying drawing, embodiments of the present invention are described further.
Embodiment 1
A removal methods for nitrous acid, its step is as follows:
(1) filled column 1 is set, glass θ ring filler is housed in filled column 1, filled column 1 top is provided with liquor inlet 7 and air out 2, and filled column 1 bottom is provided with material liquid outlet 6 and air in 8;
(2) by fan blower 5, by air in 8, in filled column 1, blast air, and adopt gas meter 4 to realize the monitoring of air mass flow and adjusting;
(3) by charge pump 3 by liquor inlet 7 to the feed liquid that passes into nitrous acid to be removed in filled column 1; Air mass flow is 3000mL/min, and feed liquid flow is 15mL/min, the volumescope that wherein volume of air is depressed with 1 normal atmosphere; Now, the feed liquid of nitrous acid to be removed is carried out gas-liquid counter current with air on glass θ ring filler surface and is contacted, and nitrous acid is decomposed into oxides of nitrogen gas at filling surface, and by air by oxides of nitrogen carrier band out, thereby realize removing of nitrous acid.
The feed liquid of nitrous acid described to be removed is simulation 1BP feed liquid, HNO in feed liquid 2concentration is 27.25 * 10 -3mol/L.The feed liquid removing after nitrous acid is detected, record HNO 2concentration is down to 0.7 * 10 -3mol/L.
Embodiment 2
A removal methods for nitrous acid, its step is as follows:
(1) filled column 1 is set, stainless steel θ ring filler is housed in filled column 1, filled column 1 top is provided with liquor inlet 7 and air out 2, and filled column 1 bottom is provided with material liquid outlet 6 and air in 8;
(2) by fan blower 5, by air in 8, in filled column 1, blast air, and adopt gas meter 4 to realize the monitoring of air mass flow and adjusting;
(3) by charge pump 3 by liquor inlet 7 to the feed liquid that passes into nitrous acid to be removed in filled column 1; Air mass flow is 5000mL/min, and feed liquid flow is 23mL/min, the volumescope that wherein volume of air is depressed with 1 normal atmosphere; Now, the feed liquid of nitrous acid to be removed is carried out gas-liquid counter current with air on stainless steel θ ring filler surface and is contacted, and nitrous acid is decomposed into oxides of nitrogen gas at filling surface, and by air by oxides of nitrogen carrier band out, thereby realize removing of nitrous acid.
The feed liquid of nitrous acid described to be removed is simulation 1BP feed liquid, HNO in feed liquid 2concentration is 55 * 10 -3mol/L.The feed liquid removing after nitrous acid is detected, record HNO 2concentration is down to 0.8 * 10 -3mol/L.

Claims (2)

1. a removal methods for nitrous acid, is characterized in that the method comprises the following steps:
(1) filled column is set, stainless steel θ ring filler or glass θ ring filler are housed in filled column, filled column top is provided with liquor inlet and air out, and filled column bottom is provided with material liquid outlet and air in;
(2) by fan blower, by air in, in filled column, blast air, and adopt gas meter to realize the monitoring of air mass flow and adjusting;
(3) by charge pump by liquor inlet to the feed liquid that passes into nitrous acid to be removed in filled column; The air adopting, material liquid volume throughput ratio are: (180-230): 1, and the volumescope that wherein volume of air is depressed with 1 normal atmosphere; Now, the feed liquid of nitrous acid to be removed and air carry out gas-liquid counter current on stainless steel θ ring filler or glass θ ring filler surface and contact, nitrous acid is decomposed into oxides of nitrogen gas at filling surface, and by air by oxides of nitrogen carrier band out, thereby realize removing of nitrous acid.
2. the removal methods of nitrous acid as claimed in claim 1, is characterized in that: described air, material liquid volume throughput ratio are: 200:1.
CN201410005672.1A 2014-01-06 2014-01-06 A kind of removal methods of nitrous acid Active CN103714876B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107369486A (en) * 2017-07-27 2017-11-21 中国原子能科学研究院 The regulation of 2AF and OF feed liquids prepares integrated system in a kind of aftertreatment technology flow
CN112037954A (en) * 2020-07-21 2020-12-04 中国原子能科学研究院 Method suitable for continuously removing iodine in spent fuel dissolving solution

Citations (8)

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US3204000A (en) * 1960-12-22 1965-08-31 Chematur Ab Manufacture of nitrotoluenes
US3359079A (en) * 1965-09-17 1967-12-19 Commissariat Energie Atomique Process for the stripping of actinides contained in organic solvents with nitrous acid
JPH07159589A (en) * 1993-12-06 1995-06-23 Hitachi Ltd Separating method for transplutonium elements
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CN1219444A (en) * 1997-10-30 1999-06-16 苏舍化学技术有限公司 Material exchange column with packing
DE10231314A1 (en) * 2002-07-10 2004-02-05 Plinke Gmbh Process for stripping nitrided waste acid comprises stripping the waste acid using vapor and/or air, and driving off super-heated vapor mixture by scrubbing in a conditioning column with part or all the condensate formed during condensation
DE102009054525A1 (en) * 2009-12-10 2011-06-16 Wacker Chemie Ag Method for removing nitric oxides and hydrogen nitrite from acid mixture, comprises removing the nitrogen oxide and the hydrogen nitrite by the introduction of kinetic energy in the mixture by blowing gas into the acid mixture
CN102412002A (en) * 2011-09-06 2012-04-11 中国原子能科学研究院 N2O4Device for oxidation regulation of plutonium valence state

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3204000A (en) * 1960-12-22 1965-08-31 Chematur Ab Manufacture of nitrotoluenes
US3359079A (en) * 1965-09-17 1967-12-19 Commissariat Energie Atomique Process for the stripping of actinides contained in organic solvents with nitrous acid
JPH07159589A (en) * 1993-12-06 1995-06-23 Hitachi Ltd Separating method for transplutonium elements
CN1145893A (en) * 1995-04-04 1997-03-26 约瑟夫迈斯纳有限公司 Rocovery of nitric acid from nitration processes
CN1219444A (en) * 1997-10-30 1999-06-16 苏舍化学技术有限公司 Material exchange column with packing
DE10231314A1 (en) * 2002-07-10 2004-02-05 Plinke Gmbh Process for stripping nitrided waste acid comprises stripping the waste acid using vapor and/or air, and driving off super-heated vapor mixture by scrubbing in a conditioning column with part or all the condensate formed during condensation
DE102009054525A1 (en) * 2009-12-10 2011-06-16 Wacker Chemie Ag Method for removing nitric oxides and hydrogen nitrite from acid mixture, comprises removing the nitrogen oxide and the hydrogen nitrite by the introduction of kinetic energy in the mixture by blowing gas into the acid mixture
CN102412002A (en) * 2011-09-06 2012-04-11 中国原子能科学研究院 N2O4Device for oxidation regulation of plutonium valence state

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Title
潘高峰等: "金属θ环填料流体力学性能研究", 《天津化工》, vol. 24, no. 6, 30 November 2010 (2010-11-30), pages 14 - 16 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107369486A (en) * 2017-07-27 2017-11-21 中国原子能科学研究院 The regulation of 2AF and OF feed liquids prepares integrated system in a kind of aftertreatment technology flow
CN112037954A (en) * 2020-07-21 2020-12-04 中国原子能科学研究院 Method suitable for continuously removing iodine in spent fuel dissolving solution
CN112037954B (en) * 2020-07-21 2023-03-21 中国原子能科学研究院 Method suitable for continuously removing iodine in spent fuel dissolving solution

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