CN103714876B - A kind of removal methods of nitrous acid - Google Patents

A kind of removal methods of nitrous acid Download PDF

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Publication number
CN103714876B
CN103714876B CN201410005672.1A CN201410005672A CN103714876B CN 103714876 B CN103714876 B CN 103714876B CN 201410005672 A CN201410005672 A CN 201410005672A CN 103714876 B CN103714876 B CN 103714876B
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nitrous acid
air
filled column
feed liquid
removal methods
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CN103714876A (en
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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 present invention relates to the removal methods of chemical substance in a kind of solution.For the method solving not to be suitable to the air carrying band removing nitrous acid of actual application in prior art, and in order to improve the removal efficiency of nitrous acid on the premise of being easy to hot operation, the invention provides the removal methods of a kind of nitrous acid, the method comprises the following steps: (1) arranges filled column, and filled column is built with rustless steel θ ring filler or glass θ ring filler;(2) in filled column, air is blasted by aerator by air intlet;(3) in filled column, the feed liquid of nitrous acid to be removed it is passed through by liquor inlet by charge pump, it is achieved the removing of nitrous acid.The removal methods of the nitrous acid of the present invention removes nitrous acid in the way of air carrying band, it is possible to make nitrous acid concentration in feed liquid less than 1.0 × 10-3Mol/L, is suitable to hot operation, and easy to operate, with low cost, can be used for the nitrous acid in 1BP feed liquid and removes.

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 to the removal methods of a kind of nitrous acid.
Background technology
In nuclear fuel reprocessing process, the plutonium head product (1BP) obtained after uranium plutonium codecontamination separates circulation is containing trivalent Plutonium, thereafter, need to be oxidizing to tetravalence by trivalent plutonium so that further abstraction purification.Due to the oxidation of plutonium generally use nitrogen oxides or Nitrite, as oxidant, therefore can remain substantial amounts of nitrous acid in the solution after oxidation.The nitrous acid of these residuals is follow-up Extraction process can enter organic facies, in the stripping process of plutonium, then consume reducing agent, affect the reduction reextraction effect of plutonium, sternly The reduction of plutonium back extraction ratio and the response rate can be caused during weight.Therefore to reduce the impact of residual nitrous acid, need to be by after oxidation price modification Nitrous acid in 1BP feed liquid is removed to reduced levels.
At present, in nitric acid system, the removal methods of nitrous acid mainly includes air carrying band removal method, evacuation degassing method, ultrasonic de- Gas method and heating.Evacuation degassing method is the amount of nitrogen oxides utilizing evacuation to reduce in gas phase, promotes that nitrous acid resolves into Nitrogen oxides enters gas phase, thus is removed by the nitrous acid in solution;Ultrasonic degassing method is to utilize ultrasound wave to accelerate dividing in solution Son motion, nitrous acid becomes instability and is decomposed and removes from solution, but evacuation degassing method and ultrasonic degassing method equipment are multiple Miscellaneous, it is unfavorable for hot operation;Heating is to make the nitrous acid in system resolve into nitrogen oxides by heated solution, and nitrogen aoxidizes Thing escapes from solution, thus reaches to remove purpose, but the speed that heating removes nitrous acid is relatively slow, and easily by feed liquid during heating In plutonium be oxidizing to sexavalence, affect subsequent technique.
Air carrying band removal method is to carry out with the form of nitrogen oxides by the nitrous acid in solution by the way of blasting air, Its method is easy, for the feature of comprehensive each side, is more suitable for hot operation.But due to the restriction of the factors such as technical field, The most not yet find the application that air carrying band removal method is the most concrete in nuclear fuel reprocessing field, it is therefore desirable to exploitation is a kind of sub- The removal methods of nitric acid is suitable for actual application.
Summary of the invention
For solving prior art is not suitable to the method that the air carrying band of actual application removes nitrous acid, and in order to put being easy to Improve the removal efficiency of nitrous acid on the premise of the operation of penetrating property, the invention provides the removal methods of a kind of nitrous acid.
A kind of removal methods of nitrous acid, the method comprises the following steps:
(1) arranging filled column, filled column is built with rustless steel θ ring filler or glass θ ring filler, and filled column top is provided with feed liquid Import and air outlet slit, filled column bottom is provided with material liquid outlet and air intlet;
(2) in filled column, blasted air by aerator by air intlet, and use gas flowmeter to realize air mass flow Monitoring and regulation;
(3) in filled column, it is passed through the feed liquid of nitrous acid to be removed by liquor inlet by charge pump;The air that used, feed liquid Volume flow ratio is: (180-230): 1, the stereometer that wherein volume of air is depressed with 1 standard atmosphere;Now, Asia to be removed The feed liquid of nitric acid carries out gas-liquid counter current with air contact at rustless steel θ ring filler or glass θ ring filler surface, and nitrous acid is at filler Surface is decomposed into oxides of nitrogen gas, and carries out by nitrogen oxides by air, thus realizes the removing of nitrous acid.
Described air, material liquid volume flow-rate ratio are preferably: 200:1.
The removal methods of the nitrous acid of the present invention removes nitrous acid in the way of air carrying band, by the process of this method, it is possible to make Nitrous acid concentration in feed liquid is less than 1.0 × 10-3mol/L.Practical using result shows, the removal methods of the nitrous acid of the present invention More be suitable to hot operation, and easy to operate, with low cost, can be used for the nitrous acid in 1BP feed liquid and remove.
Accompanying drawing explanation
The process diagram of the removal methods of the nitrous acid of Fig. 1 present invention.
Reference: 1. filled column, 2. air outlet slit, 3. charge pump, 4. gas flowmeter, 5. aerator, 6. material liquid outlet, 7. liquor inlet, 8. air intlet.
Detailed description of the invention
Below in conjunction with the accompanying drawings embodiments of the present invention are described further.
Embodiment 1
A kind of removal methods of nitrous acid, its step is as follows:
(1) arranging filled column 1, filled column 1 is provided with liquor inlet 7 and sky built with glass θ ring filler, filled column 1 top Gas outlet 2, filled column 1 bottom is provided with material liquid outlet 6 and air intlet 8;
(2) in filled column 1, blasted air by aerator 5 by air intlet 8, and use gas flowmeter 4 right to realize The monitoring of air mass flow and regulation;
(3) in filled column 1, it is passed through the feed liquid of nitrous acid to be removed by liquor inlet 7 by charge pump 3;Air mass flow is 3000mL/min, feed liquid flow is 15mL/min, the stereometer that wherein volume of air is depressed with 1 standard atmosphere;Now, treat The feed liquid of removing nitrous acid carries out gas-liquid counter current with air on glass θ ring filler surface and contacts, and nitrous acid is decomposed at filling surface Oxides of nitrogen gas, and carry out by nitrogen oxides by air, thus realize the removing of nitrous acid.
The feed liquid of described nitrous acid to be removed is simulation 1BP feed liquid, HNO in feed liquid2Concentration is 27.25 × 10-3mol/L.Right Feed liquid after removing nitrous acid detects, and records HNO2Concentration is down to 0.7 × 10-3mol/L。
Embodiment 2
A kind of removal methods of nitrous acid, its step is as follows:
(1) arranging filled column 1, filled column 1 is provided with liquor inlet 7 He built with rustless steel θ ring filler, filled column 1 top Air outlet slit 2, filled column 1 bottom is provided with material liquid outlet 6 and air intlet 8;
(2) in filled column 1, blasted air by aerator 5 by air intlet 8, and use gas flowmeter 4 right to realize The monitoring of air mass flow and regulation;
(3) in filled column 1, it is passed through the feed liquid of nitrous acid to be removed by liquor inlet 7 by charge pump 3;Air mass flow is 5000mL/min, feed liquid flow is 23mL/min, the stereometer that wherein volume of air is depressed with 1 standard atmosphere;Now, treat The feed liquid of removing nitrous acid carries out gas-liquid counter current with air on rustless steel θ ring filler surface and contacts, and nitrous acid decomposes at filling surface For oxides of nitrogen gas, and carry out by nitrogen oxides by air, thus realize the removing of nitrous acid.
The feed liquid of described nitrous acid to be removed is simulation 1BP feed liquid, HNO in feed liquid2Concentration is 55 × 10-3mol/L.To removing Feed liquid after nitrous acid detects, and records HNO2Concentration is down to 0.8 × 10-3mol/L。

Claims (2)

1. the removal methods of a nitrous acid, it is characterised in that the method comprises the following steps:
(1) arranging filled column, filled column is built with rustless steel θ ring filler or glass θ ring filler, and filled column top is provided with feed liquid Import and air outlet slit, filled column bottom is provided with material liquid outlet and air intlet;
(2) in filled column, blasted air by aerator by air intlet, and use gas flowmeter to realize air mass flow Monitoring and regulation;
(3) in filled column, it is passed through the feed liquid of nitrous acid to be removed by liquor inlet by charge pump;The air that used, feed liquid Volume flow ratio is: (180-230): 1, the stereometer that wherein volume of air is depressed with 1 standard atmosphere;Now, Asia to be removed The feed liquid of nitric acid carries out gas-liquid counter current with air contact at rustless steel θ ring filler or glass θ ring filler surface, and nitrous acid is at filler Surface is decomposed into oxides of nitrogen gas, and carries out by nitrogen oxides by air, thus realizes the removing of nitrous acid.
2. the removal methods of nitrous acid as claimed in claim 1, it is characterised in that: described air, material liquid volume flow-rate ratio be: 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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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
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

Citations (7)

* 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

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102412002B (en) * 2011-09-06 2013-10-30 中国原子能科学研究院 N2O4Device for oxidation regulation of plutonium valence state

Patent Citations (7)

* 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

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