CN106356110A - Continuous evaporation-denitration technology - Google Patents
Continuous evaporation-denitration technology Download PDFInfo
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- CN106356110A CN106356110A CN201610820126.2A CN201610820126A CN106356110A CN 106356110 A CN106356110 A CN 106356110A CN 201610820126 A CN201610820126 A CN 201610820126A CN 106356110 A CN106356110 A CN 106356110A
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- denitration
- reaction
- continuous evaporation
- feed liquid
- evaporation
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/08—Processing by evaporation; by distillation
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/20—Disposal of liquid waste
- G21F9/22—Disposal of liquid waste by storage in a tank or other container
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Environmental & Geological Engineering (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention relates to a continuous evaporation-denitration technology. The technology comprises the following steps that 1, initial denitration material liquid is heated to 90 DEG C to 120 DEG C under negative pressure; 2, a denitration reaction is induced to be conducted, wherein formaldehyde is continuously injected into the heated initial denitration material liquid, sodium nitrite is added to induce the denitration reaction to be conducted, all reaction products flow back while the reaction is induced to be conducted, the temperature is kept at 90 DEG C to 120 DEG C, the denitration reaction induction period is metered by t (the unit is s), and when the denitration reaction induction period t is smaller than 30 s and brown smoke is generated in the reaction, it is determined that the denitration reaction is steadily conducted; 3, continuous evaporation-denitration is conducted, wherein denitration material liquid is continuously injected into the reaction material liquid obtained in the step 2, heating is conducted for continuous evaporation-denitration, and meanwhile mixed gas generated in the reaction is exhausted. According to the technology, the induction period of the formaldehyde denitration reaction can be significantly eliminated, so that stable operation of the continuous evaporation-denitration technology is achieved, pollution of secondary steam is reduced, and the production efficiency is improved.
Description
Technical field
The invention belongs to the denitrating technique technical field of formaldehyde and nitric acid reaction is and in particular to one kind can eliminate formaldehyde denitration
Continuous evaporation-the denitrating technique of induction period.
Background technology
The radioactive liquid waste that nuclear fuel reprocessing plant produces is mainly by the acid waste liquid containing fission product and actinidess
Composition, in order to reduce the storage volume of waste liquid and reduce the Financial cost that waste liquid is disposed, needs radioactive liquid waste is evaporated
Concentration.
Its acidity of radioactive liquid waste that reprocessing plant produces typically in 2mol/l, in waste liquid evaporating concentration process,
The acidity of waste liquid can reach 6-8mol/l, and under the conditions of being in high temperature high radioactivity, the evaporation to waste liquid is dense with this understanding
Contracting mainly has the adverse effect of three aspects: the concentrated nitric acid 1. seething with excitement has strong corrosiveness to stainless steel equipment, reduces equipment
Service life；2. dissolubility in concentrated solution for the nitrate is remarkably decreased with the rising of concentration of nitric acid, and simultaneously tiny divides
The precipitation capacity of scattered seed also increases, and these limit the raising of cycles of concentration；3. evaporate under high concentration of nitric acid, radioactivity is split
Becoming nucleic increases with steam escaped quantity, is unfavorable for the purification of indirect steam.Therefore, adopt first in waste liquid evaporating concentration process
There is denitration reaction with the nitric acid in waste liquid in aldehyde, to reduce the acidity of waste liquid.
At present, waste liquid concentration process adopts " continuous evaporation denitration " technique of formaldehyde denitration can reduce concentrated solution
Acidity, the treating capacity of raising vaporizer, but the initial reaction stage of formaldehyde and nitric acid, the decomposition rate of nitric acid is very slow, treats a timing
Between after, denitration reaction produce gas flow suddenly increase, cause reactor pressure abruptly increase, thus occurring " bumping " to cause indirect steam
Condensed fluid is contaminated.Traditionally, also formaldehyde is added after denitration feed liquid, nitric acid decomposition reaction speed is from slow until swashing suddenly
The time increasing is referred to as the induction period of formaldehyde denitration reaction.
Content of the invention
For defect present in prior art, it is an object of the invention to provide a kind of continuous evaporation-denitrating technique, adopt
This technique can significantly mitigate or alleviate the induction period of formaldehyde denitration reaction, to realize the stable operation of continuous evaporation-denitrating technique,
Reduce the pollution of indirect steam, improve production efficiency.
For reaching object above, the technical solution used in the present invention is: a kind of continuous evaporation-denitrating technique, including following
Step:
(1) negative pressure heats initial denitration feed liquid: under condition of negative pressure, will treat that denitration feed liquid is heated to 90～102 DEG C；
(2) induction denitration reaction is carried out: constantly injects formaldehyde in the initial denitration feed liquid of heating, is simultaneously introduced nitrous
Sour sodium, to induce denitration reaction to carry out, induced reaction makes product all flow back while carrying out, keeping temperature be 90～
102 DEG C, denitration reaction induction period is by t (in terms of unit s), when denitration reaction induction period t < during 30s, and brown in observing response
Smog when, judge denitration reaction steadily carry out；
(3) continuous evaporation-denitration: after denitration reaction is steadily carried out, persistently note in the reaction feed liquid obtaining to step (2)
Enter denitration feed liquid, heating, carry out continuous evaporation-denitration, discharge the gaseous mixture that reaction produces simultaneously.
Further, in step (1), condition of negative pressure is finger pressure is -7～-12kpa.
Further, in step (1), denitration feed liquid is heated to 95 DEG C～102 DEG C.
Further, in step (3), formaldehyde, the injection rate of denitration feed liquid make increased formaldehyde, nitric acid in reactant full
Sufficient aldehyde, sour mol ratio are 0.4-0.6mol/mol.
Further, in step (3), reaction pressure is -7kpa～-12kpa, and reaction temperature is 90-102 DEG C.
Further, the continuous evaporation-denitrating technique of the present invention is further comprising the steps of:
(4) make the gaseous mixture condensation of discharge, and condensed fluid is reclaimed, simultaneously by fixed gas after alkali liquor absorption,
Discharge tail gas.
Further, the continuous evaporation-denitrating technique of the present invention is further comprising the steps of:
(5) the partial condensation liquid of step (4) is back in the reactant of step (3), control reflux ratio is 8%-13%.
A kind of continuous evaporation-denitrating technique provided by the present invention, just produces obvious Brown gas, energy in initial reaction stage
Enough notable shorten formaldehyde denitration reaction induction period, make entirely to evaporate-denitrification process can reach stable operation within a short period of time
State, it is to avoid long " bumping " problem leading to formaldehyde accumulation to produce of induction period, decreases indirect steam condensed fluid and is contaminated
Risk, and during whole operation, feed acidity remains unchanged substantially, it is to avoid the too high institute of acidity in traditional evaporation process
A series of adverse effects brought, possess stability, reliability and practicality.
Brief description
Fig. 1 is a kind of flow chart of continuous evaporation-denitrating technique that the present invention provides；
Fig. 2 is a kind of structural representation of the continuous evaporation-denitrating technique for realizing present invention process.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and detailed description.
The main chemical reactions equation that a kind of continuous evaporation-denitrating technique provided by the present invention is related to is as follows:
hcho+xhno3→co2+(2-x/2)no+(3x/2-2)no2+(1+x/2)h2o
This reaction is a reaction rate from slow to fast self-catalyzed reaction.Initial reaction stage speed slowly, here mistake
Nitrite anions are constantly had to produce in journey.After nitrite anions accumulate to a certain extent, under the catalytic action of nitrite anions, denitration
Reaction rate is accelerated suddenly, and the oxides of nitrogen gas amount of generation increases suddenly, causes reactor pressure abruptly increase, there is generation " bumping "
Danger.
For this reason, the invention provides a kind of new continuous evaporation-denitrating technique, as shown in figure 1, described continuous evaporation-de-
Nitre technique comprises the following steps:
(1) negative pressure heats initial denitration feed liquid: under condition of negative pressure, by a certain amount of initial denitration feed liquid heating containing nitric acid
To 90～102 DEG C；
(2) induction denitration reaction is carried out: constantly injects formaldehyde in the initial denitration feed liquid of heating, is simultaneously introduced nitrous
Sour sodium, to induce denitration reaction to carry out, induced reaction makes product all flow back while carrying out, keeping temperature be 90～
102 DEG C, denitration reaction induction period is by t (in terms of unit s), when denitration reaction induction period t < during 30s, dense palm fibre in simultaneous reactions
Color smog, to judge that denitration reaction steadily carries out；
(3) continuous evaporation-denitration: after denitration reaction is steadily carried out, persistently note in the reaction feed liquid obtaining to step (2)
Enter denitration feed liquid, heating, carry out continuous evaporation-denitration, discharge the gaseous mixture that reaction produces simultaneously.
Because the present invention adds a certain amount of nitrite (sodium nitrite) in initial reaction stage, by providing extra nitrous
Acid ion, to accelerate catalytic action, makes nitric acid decomposition reaction quickly carry out and not suffer from surge process from slow to fast, thus
Reach the effect shortened or eliminate induction period, reduce the risk that " bumping " occurs.
In the present invention, the condition of negative pressure in step (1) is tiny structure, be finger pressure be -7～-12kpa.Under preferable case,
Initial denitration feed liquid is heated to 95-102 DEG C.
In order to reduce the addition of formaldehyde and sodium nitrite as far as possible, initial denitration feed liquid nitration acid heat extremely seethes with excitement, and
Formaldehyde and sodium nitrite are added in the initial denitration feed liquid of boiling.
Realize after denitration reaction steadily carries out, in step (3) of the present invention, should ensure that formaldehyde, denitration feed liquid by step (2)
Injection rate make the formaldehyde increasing in reactant, nitric acid meet aldehyde, sour mol ratio is 0.4-0.6mol/mol.
Preferably, in step (3), reaction pressure is -7kpa～-12kpa, and reaction temperature is 90-102 DEG C.
Additionally, a kind of continuous denitration-evaporation technology provided by the present invention can also comprise the following steps:
(4) make the gaseous mixture condensation of discharge, and condensed fluid is reclaimed, simultaneously by fixed gas after alkali liquor absorption,
Discharge tail gas.
In addition, a kind of continuous denitration-evaporation technology provided by the present invention can further include following steps:
(5) the partial condensation liquid of step (4) is back in the reactant of step (3), control reflux ratio is 8%-13%.
For realizing the technique of the present invention, present invention also offers a kind of structural representation of continuous evaporation-denitrating technique.
As shown in figure 1, a kind of continuous evaporation denitrating system that the present invention provides includes formaldehyde feeder channel 2, denitration feed liquid supplies
Hopper 3, jacket type reactor 1, reactor caloic feed mechanism 12, rectifying column 4, condenser 5, condensed fluid receiving slit 6, fixed gas
Reception device 7 and vacuum system 10；The chuck of jacket type reactor 1 lower half setting and reactor caloic feed mechanism 12 phase
Even, the top of jacket type reactor 1 is provided with sodium nitrite charge door 13, and the top of jacket type reactor 1 is passed through to connect respectively
Pipeline is connected with formaldehyde feeder channel 2, denitration feed liquid feeder channel 3, corresponding connecting pipeline is respectively equipped with formaldehyde charging pump 8, takes off
Nitre feed liquid charging pump 9；Rectifying column 4 is located above jacket type reactor 1, and the top of the bottom of rectifying column 4 and jacket type reactor 1
Portion connects, and the top of rectifying column 4 is connected with condenser 5 tube side import, condenser 5 tube side liquid-phase outlet and condensed fluid receiving slit 6
It is connected, condenser 5 tube side gaseous phase outlet is connected with fixed gas reception device 7, fixed gas reception device 7 and vacuum equipment 10 (can
Using vacuum jet pump) it is connected；And, the pipeline that condenser 5 tube side liquid-phase outlet is connected with condensed fluid receiving slit 6 is provided with back
Flow ratio controllers 11, reflux ratio controller 11 is connected with rectifying column 4 top.
Below using the radioactive liquid waste of spentnuclear fuel reprocessing plant (concentration of nitric acid be about 2～3mol/l about) as denitration
Feed liquid, and combine the continuous evaporation-denitrating technique of the system brief description present invention shown in Fig. 1.
First, open denitration feed liquid charging pump 9, by the radioactive liquid waste injection jacket type reactor 1 of certain volume, make
For initial denitration feed liquid, heated by reactor heating agent feed mechanism 12, and opened vacuum equipment 10, controlled pressure in kettle
For -10kpa, temperature is 101 DEG C；
When after feed pressure in kettle, temperature stabilization, open formaldehyde feed pump 8, continuously note into jacket type reactor 1
Enter formaldehyde, sodium nitrite charge door 13 from jacket reactor 1 for the sodium nitrite solution having configured disposably is injected meanwhile
To in jacket reactor 1, there are Brown gas to produce in kettle soon, condensed by condenser 5, adjusting reflux ratio controller 11 makes
Condensed fluid is all back in rectifying column, after fixed gas alkali liquor absorption in the fixed gas reception device 7, discharges tail gas.
Carry out after 10min after denitration reaction, reacting balance, it is again turned on denitration feed liquid charging pump 9 and (keep formaldehyde injection speed
Rate is constant), continuously into jacket type reactor 1, inject nitric acid feed liquid, keep operating pressure in kettle to be -10kpa, operation temperature
For 101 DEG C, start continuous denitration-evaporation reaction, so that the condensed device of gaseous mixture 5 of discharge is condensed, adjust reflux ratio controller 11
Make partial condensation liquid be back to rectifying column 4 (control of reflux ratio is 10%), receive condenser 5 row using condensed fluid receiving slit 6
Other condensed fluid going out, after the fixed gas simultaneously discharged condenser 5 alkali liquor absorption in the fixed gas reception device 7, discharge
Tail gas.
Above-described embodiment is the illustration to the present invention, and the present invention can also be with other ad hoc fashions or other
Particular form is implemented, without departing from idea of the invention or substitutive characteristics.Therefore, from the point of view of the embodiment of description is in terms of any
It is regarded as illustrative rather than determinate.The scope of the present invention should be illustrated by appended claims, any and claim
Intention and the equivalent change of scope also should be within the scope of the present invention.
Claims (7)
1. a kind of continuous evaporation-denitrating technique is it is characterised in that comprise the following steps:
(1) negative pressure heats initial denitration feed liquid: under condition of negative pressure, by a certain amount of heating of the initial denitration feed liquid containing nitric acid 90～
102℃；
(2) induction denitration reaction is carried out: constantly injects formaldehyde in the initial denitration feed liquid of heating, is simultaneously introduced nitrous acid
Sodium, to induce denitration reaction to carry out, induced reaction makes product all flow back while carrying out, and keeping temperature is 90～102
DEG C, denitration reaction induction period is by t (in terms of unit s), when denitration reaction induction period t < during 30s, brown fume in simultaneous reactions
When, to judge that denitration reaction steadily carries out；
(3) continuous evaporation-denitration: after denitration reaction is steadily carried out, persistently inject de- in the reaction feed liquid obtaining to step (2)
Nitre feed liquid, heating, carry out continuous evaporation-denitration, discharge the gaseous mixture that reaction produces simultaneously.
2. a kind of continuous evaporation-denitrating technique according to claim 1 is it is characterised in that in step (1), condition of negative pressure
Be finger pressure be -7～-12kpa.
3. a kind of continuous evaporation-denitrating technique according to claim 2 is it is characterised in that in step (1), denitration feed liquid
It is heated to 90 DEG C～102 DEG C.
4. according to a kind of arbitrary described continuous evaporation-denitrating technique of claim 1-3 it is characterised in that in step (3), first
Aldehyde, the injection rate of denitration feed liquid make the formaldehyde increasing in reactant, nitric acid meet aldehyde, sour mol ratio is 0.4-0.6mol/
mol.
5. a kind of evaporation according to claim 4 continuous-denitrating technique it is characterised in that in step (3), reaction pressure
For -7kpa～-12kpa, reaction temperature is 95-102 DEG C.
6. a kind of continuous evaporation-denitrating technique according to claim 1 it is characterised in that described technique also include following
Step:
(4) make the gaseous mixture condensation of discharge, and condensed fluid is reclaimed, simultaneously by fixed gas after alkali liquor absorption, discharge
Tail gas.
7. a kind of continuous evaporation-denitrating technique according to claim 6 it is characterised in that described technique also include following
Step:
(5) the partial condensation liquid of step (4) is back in the reactant of step (3), control reflux ratio is 8%-13%.
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| CN201610820126.2A CN106356110B (en) | 2016-09-13 | 2016-09-13 | Continuous evaporation-denitration process |
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| CN201610820126.2A CN106356110B (en) | 2016-09-13 | 2016-09-13 | Continuous evaporation-denitration process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108447578A (en) * | 2018-05-08 | 2018-08-24 | 中国原子能科学研究院 | Intermittently operated formula high activity liquid waste evaporation-denitration device |
| CN108630332A (en) * | 2018-03-26 | 2018-10-09 | 中国核电工程有限公司 | A kind of breaking plant and destruction methods of oxalate precipitation filtrated stock oxalate |
| CN111508631A (en) * | 2020-04-24 | 2020-08-07 | 清华大学 | External circulation type high-level radioactive waste liquid continuous evaporation concentration denitrator |
| CN114678152A (en) * | 2022-03-17 | 2022-06-28 | 清华大学 | Device and method for continuous evaporation, concentration and denitration of radioactive material liquid |
| CN115477287A (en) * | 2022-10-17 | 2022-12-16 | 中核四0四有限公司 | Nitric acid recovery system and method in uranium purification process |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108630332A (en) * | 2018-03-26 | 2018-10-09 | 中国核电工程有限公司 | A kind of breaking plant and destruction methods of oxalate precipitation filtrated stock oxalate |
| CN108630332B (en) * | 2018-03-26 | 2021-06-18 | 中国核电工程有限公司 | Device and method for destroying oxalate in oxalate precipitation and filtration mother liquor |
| CN108447578A (en) * | 2018-05-08 | 2018-08-24 | 中国原子能科学研究院 | Intermittently operated formula high activity liquid waste evaporation-denitration device |
| CN111508631A (en) * | 2020-04-24 | 2020-08-07 | 清华大学 | External circulation type high-level radioactive waste liquid continuous evaporation concentration denitrator |
| CN111508631B (en) * | 2020-04-24 | 2021-11-09 | 清华大学 | External circulation type high-level radioactive waste liquid continuous evaporation concentration denitrator |
| CN114678152A (en) * | 2022-03-17 | 2022-06-28 | 清华大学 | Device and method for continuous evaporation, concentration and denitration of radioactive material liquid |
| CN114678152B (en) * | 2022-03-17 | 2024-06-11 | 清华大学 | Continuous evaporation concentration denitration device and method with radioactive feed liquid |
| CN115477287A (en) * | 2022-10-17 | 2022-12-16 | 中核四0四有限公司 | Nitric acid recovery system and method in uranium purification process |
| CN115477287B (en) * | 2022-10-17 | 2023-09-26 | 中核四0四有限公司 | Nitric acid recovery system and method in uranium purification process |
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