CN110201623A - A kind of quick oxidation unit of ammonia nitrogen and the quick method for oxidation of ammonia nitrogen - Google Patents
A kind of quick oxidation unit of ammonia nitrogen and the quick method for oxidation of ammonia nitrogen Download PDFInfo
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- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 90
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 230000003647 oxidation Effects 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000007800 oxidant agent Substances 0.000 claims abstract description 53
- 230000001590 oxidative effect Effects 0.000 claims abstract description 51
- 239000000243 solution Substances 0.000 claims description 62
- JGJLWPGRMCADHB-UHFFFAOYSA-N hypobromite Chemical compound Br[O-] JGJLWPGRMCADHB-UHFFFAOYSA-N 0.000 claims description 38
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- 239000011550 stock solution Substances 0.000 claims description 9
- JVMRPSJZNHXORP-UHFFFAOYSA-N ON=O.ON=O.ON=O.N Chemical compound ON=O.ON=O.ON=O.N JVMRPSJZNHXORP-UHFFFAOYSA-N 0.000 claims description 7
- XWNSFEAWWGGSKJ-UHFFFAOYSA-N 4-acetyl-4-methylheptanedinitrile Chemical compound N#CCCC(C)(C(=O)C)CCC#N XWNSFEAWWGGSKJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000004153 Potassium bromate Substances 0.000 claims description 6
- 229940094037 potassium bromate Drugs 0.000 claims description 6
- 235000019396 potassium bromate Nutrition 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- FWLDLPLBLLYROD-UHFFFAOYSA-N N.[N].[O] Chemical compound N.[N].[O] FWLDLPLBLLYROD-UHFFFAOYSA-N 0.000 claims description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims 1
- WJVMHVRTWHJFPH-UHFFFAOYSA-N [N].N.[N].N Chemical compound [N].N.[N].N WJVMHVRTWHJFPH-UHFFFAOYSA-N 0.000 claims 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims 1
- 229910052794 bromium Inorganic materials 0.000 claims 1
- 239000008236 heating water Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 230000035484 reaction time Effects 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000005259 measurement Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- CRWJEUDFKNYSBX-UHFFFAOYSA-N sodium;hypobromite Chemical compound [Na+].Br[O-] CRWJEUDFKNYSBX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- SXDBWCPKPHAZSM-UHFFFAOYSA-N bromic acid Chemical class OBr(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
- B01J19/243—Tubular reactors spirally, concentrically or zigzag wound
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N2021/3125—Measuring the absorption by excited molecules
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention relates to a kind of quick oxidation unit of ammonia nitrogen and the quick method for oxidation of ammonia nitrogen, device includes an ammonia nitrogen solution delivery branch pipe and an oxidant delivery branch pipe, the ammonia nitrogen solution delivery branch pipe output end is equipped with a heater, for the ammonia nitrogen solution to be preheated, it further include an oxidation reaction helix tube, the arrival end of the oxidation reaction helix tube is connected with the outlet ends of the ammonia nitrogen solution delivery branch pipe and the oxidant delivery branch pipe.Compared with prior art, the mixed pipeline of the present invention uses helix tube, one section of reaction pipeline and reaction time are provided for oxidation reaction, and with the Coriolis force of spiral channel interior, realize that the high speed rotation stirring in sample traveling, accelerated oxidation reaction are reacted completely so that ammonia nitrogen solution carries out 100% with oxidant in oxidation reaction helix tube, minute can be reduced, measuring apparatus efficiency is improved.
Description
Technical field
The present invention relates to technical field of analytical instruments, and in particular to a kind of quick oxidation unit of ammonia nitrogen and ammonia nitrogen quickly aoxidize
Method.
Background technique
Gas-phase molecular absorption spectrometry method (hereinafter referred to as GPMAS) is the suction of the gas that is resolved into based on tested ingredient to light
The relationship for receiving intensity and measured component concentration abides by this principle of law of Beer to be quantitative determined, according to absorbing wavelength
Difference can also determine tested ingredient and carry out qualitative analysis.Gas phase molecular absorption spectrometer is passed through based on GPMAS principle
Conversion to be measured in liquid phase sample is gas by chemical reaction, is separated gas from liquid phase sample and is loaded into measurement
The content of system measurement gas finally calculates the equipment of constituent concentration to be measured in sample.It is used to measure ammonia nitrogen, sulfide,
Kjeldahl nitrogen, total nitrogen, nitrate, nitrite, sulphite, chloride ion, permanganate index.
When using gas phase molecular absorption spectrometer measurement ammonia nitrogen index, need ammonia nitrogen oxygen through hypobromite oxidant
Turn to nitrite nitrogen (nitrite nitrogen is that itrogenous organic substance further aoxidizes in water body, during changing into nitrate in
Between product), then can just be measured.According to State Ministry of Environmental Protection, People's Republic of China (PRC) environmental standard method HJ/T195-2005
(the 2nd row of page 3) is recorded, and ammonia nitrogen water sample needs after hypobromite oxidant is added in 18 DEG C or more Oxidation at room temperature 20min
After could measure.If encountering microthermal climate, when environment temperature is less than 18 DEG C, water bath with thermostatic control auxiliary heating must be just used.Cause
Ammonium oxidation method described in this standard is not only time-consuming very long and complex for operation step, and working efficiency is low.In addition,
Also without the record of dedicated ammonium oxidation device in relevant document
Patent CN102628847A discloses a kind of method and device for quickly oxidizing ammonia nitrogen, is related to analytical instrumentation techniques neck
Domain.For existing ammonium oxidation method, time-consuming, complex for operation step, and the problem of no dedicated ammonium oxidation device.
Method: a, ammonia nitrogen solution is preheated；B, it is nitrite nitrogen that oxidant, which is added, by ammonium oxidation.Device: it includes that an ammonia nitrogen is molten
Liquid delivery branch pipe, an oxidant delivery branch pipe, one communicate and are used in combination with ammonia nitrogen solution delivery branch pipe and oxidant delivery branch pipe respectively
In the container of output nitrite nitrogen reactant；Ammonia nitrogen solution delivery branch pipe output end is equipped with a heater, for ammonia nitrogen is molten
Liquid preheating.
The device is primarily present following deficiency: ammonia nitrogen solution delivery branch pipe is directly connected to use with oxidant delivery branch pipe end
In the container of oxidation reaction, after of short duration confluence, ammonia nitrogen solution and oxidant are completely anti-without carrying out 100% in a reservoir
It answers；The liner oxidation upper limit of concentration of the patent is relatively low, and enriched sample oxidation efficiency cannot reach 100% oxidation, Wu Fazhi
The oxidation concentration for the 2mg/L being up to state standards is connect, measurement result accuracy, system oxidation efficiency have to be hoisted.
Summary of the invention
The purpose of the present invention is to solve the above-mentioned problems and provides a kind of quick oxidation unit of ammonia nitrogen and ammonia nitrogen is quick
Method for oxidation.
The purpose of the present invention is achieved through the following technical solutions:
A kind of quick oxidation unit of ammonia nitrogen, including an ammonia nitrogen solution delivery branch pipe and an oxidant delivery branch pipe, the ammonia
It further includes an oxidation reaction spiral shell that nitrogen solution delivery branch pipe output end, which is equipped with a heater for preheating the ammonia nitrogen solution,
Coil, the arrival end of the oxidation reaction helix tube and the ammonia nitrogen solution delivery branch pipe and the oxidant delivery branch pipe go out
Mouth end is connected.
Further, the internal diameter of the oxidation reaction helix tube is 0.5-3mm, using plastic material, as PTFE, PFA,
FEP etc. is made, and it is 3-30 seconds that oxidation reaction helix tube, which makes ammonia nitrogen molten with the reaction time of oxidant,.
Further, the heater is water-bath heater, oil bath heater or electric heater.
Further, the heater makes the ammonia nitrogen solution in the ammonia nitrogen solution delivery branch pipe be heated to 70-95 DEG C, excellent
It is selected as 80-85 DEG C.
Further, the oxidant conveyed in the oxidant delivery branch pipe is hypobromite solutions.
A kind of quick method for oxidation of ammonia nitrogen, includes the following steps:
(1) the heated device of ammonia nitrogen solution is preheated, is delivered to oxidation reaction helix tube through ammonia nitrogen solution delivery branch pipe；
(2) oxidant is delivered to oxidation reaction helix tube through oxidant delivery branch pipe；
(3) ammonia nitrogen solution and oxidant carry out oxidation reaction in oxidation reaction helix tube, and oxidant is by the ammonia in solution
Nitrogen oxidation is nitrite nitrogen.
Step (1) described heater makes the ammonia nitrogen solution in the ammonia nitrogen solution delivery branch pipe be heated to 70-95 DEG C.
The time that step (3) ammonia nitrogen solution and oxidant carry out oxidation reaction in oxidation reaction helix tube is 3-30 seconds.
The oxidant is hypobromite solutions, is prepared by the following method to obtain:
(1) potassium bromate, potassium bromide is soluble in water, hypobromite stock solution is configured, the concentration of the potassium bromate is
0.0005-0.0006g/ml, the concentration of the potassium bromide are 0.03-0.05g/ml；
(2) hypobromite stock solution made from step (1) is mixed with water, hydrochloric acid and sodium hydroxide solution, is prepared
Sodium hypobromite oxidant, the concentration of hydrochloric acid are 6mol/L, and the sodium hydroxide solution is the hydroxide that mass fraction is 40%
The volume ratio of sodium solution, hypobromite stock solution and water, hydrochloric acid and sodium hydroxide solution is 2-4:150:6:50.
Compared with prior art, the present invention is designed mixed pipeline, is oxygen using helix tube type reaction designing
Change reaction and one section of reaction pipeline and reaction time are provided, and with the Coriolis force of spiral channel interior, realizes that sample is advanced
In high speed rotation stirring, accelerated oxidation reaction so that ammonia nitrogen solution and oxidant carry out 100% in oxidation reaction helix tube
Reaction completely.
Helical structure design in the present invention, effectively increases liquid line hybrid perturbation, improves efficiency, pass through
The spiral reaction tube of offer can effectively promote the time of oxidation reaction, can provide the continuous on-line oxidation of 3-30S for entire reaction
The oxidation efficiency of system is greatly improved to allow the fully oxidized completion of enriched sample in time, and extension system aoxidizes concentration model
It encloses, the measurement range of whole set equipment is effectively widened, part enriched sample can be complete without dilution in reagent continuous mode
At 100% oxidation, minute is reduced, improves measuring apparatus efficiency.
In addition, the present invention optimizes oxidizer formula, to further increase efficiency, heating is promoted for reaction
Acceleration effect, and since oxidant itself can not heat (heat resolve), therefore the present invention improves the heating of ammonia nitrogen solution sample
Temperature.To make up the technology drawback that oxidant decomposes after high temperature bring flows back, is optimized by oxidant agent prescription, increased secondary
Cost content is aoxidized in bromic acid salt oxidizing agent, to ensure that the oxidant in subsequent reactions is enough.
The present invention can effectively expand the concentration range of linearity of ammonium oxidation efficiency, from original liner oxidation upper limit of concentration
1.2mg/L is increased to 2.4mg/L, greatly improves oxidation efficiency, so that the ammonia nitrogen sample of conventional 2mg/L and its following concentration
It can be realized complete oxidation, the standard curve fit related coefficient of such ammonia nitrogen will get a promotion, and the accuracy of sample measurement will
It greatly promotes, the extension rate of enriched sample can effectively reduce, and measurement result also will be more accurate therewith.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of apparatus of the present invention；
Fig. 2-5 is the linear relationship chart of one experimental test of scheme；
Fig. 6-10 is the linear relationship chart of two experimental test of scheme；
In figure: 1- ammonia nitrogen solution delivery branch pipe；2- oxidant delivery branch pipe；3- oxidation reaction helix tube；4- heater.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
A kind of quick oxidation unit of ammonia nitrogen, as shown in Figure 1, including that an ammonia nitrogen solution delivery branch pipe 1 and an oxidant convey
Branch pipe 2, it further includes an oxidation that 1 output end of ammonia nitrogen solution delivery branch pipe, which is equipped with a heater 4 for preheating ammonia nitrogen solution,
React helix tube 3, the arrival end and ammonia nitrogen solution delivery branch pipe 1 of oxidation reaction helix tube 3 and the outlet of oxidant delivery branch pipe 1
End is connected.The oxidant conveyed in oxidant delivery branch pipe is hypobromite.The internal diameter of oxidation reaction helix tube is 0.5-
3mm, using plastic material, such as PTFE, PFA, FEP are made, and oxidation reaction helix tube ammonia nitrogen molten to react with oxidant
Time is 3-30 seconds.Water-bath heater, oil bath heater or electric heater can be used in heater.Heater conveys ammonia nitrogen solution
Ammonia nitrogen solution in branch pipe is heated to 70-95 DEG C, preferably 80-85 DEG C.
The present invention by original mixed circuit design be helix tube, can be provided for oxidation reaction one section of reaction pipeline with instead
Between seasonable, and with the Coriolis force of spiral channel interior, the high speed rotation stirring in sample traveling is realized, accelerated oxidation is anti-
It answers, is reacted completely so that ammonia nitrogen solution carries out 100% with oxidant in oxidation reaction helix tube.
Embodiment 2
A kind of quick method for oxidation of ammonia nitrogen is included the following steps: using 1 described device of embodiment
(1) the heated device of ammonia nitrogen solution is preheated, is delivered to oxidation reaction helix tube through ammonia nitrogen solution delivery branch pipe；
(2) oxidant hypobromite is delivered to oxidation reaction helix tube through oxidant delivery branch pipe；
(3) ammonia nitrogen solution and hypobromite carry out oxidation reaction in oxidation reaction helix tube, and oxidant will be in solution
Ammonium oxidation is nitrite nitrogen.
Step (1) heater makes the ammonia nitrogen solution in the ammonia nitrogen solution delivery branch pipe be heated to 80 DEG C.
When experiment, the oxidant used is hypobromite solutions, is prepared especially by following methods:
(1) potassium bromate, potassium bromide is soluble in water, hypobromite stock solution is configured, the concentration of potassium bromate is 0.00056g/
Ml, the concentration of potassium bromide are 0.04g/ml；
(2) hypobromite stock solution made from step (1) is mixed with water, hydrochloric acid and sodium hydroxide solution, is prepared
Sodium hypobromite oxidant, the concentration of hydrochloric acid are 6mol/L, and the sodium hydroxide solution is the hydroxide that mass fraction is 40%
The volume ratio of sodium solution, hypobromite stock solution and water, hydrochloric acid and sodium hydroxide solution is 3:150:6:50.
Respectively with the quick side of oxidation of ammonia nitrogen disclosed in patent CN102628847A (scheme one) and of the invention (scheme two)
Method and device carry out ammonium oxidation test.
Using the Ammonia nitrogen standard liquid (1000mg/L) for having card, the ammonia nitrogen standard solution of 2mg/L is configured, certainly using instrument
Dynamic dilution, is tested using the device of apparatus of the present invention and certain company.
By Fig. 2-5 it is found that in the case where deleting graticule point highest point 2.00mg/L, r=0.9999, it was demonstrated that oxidant can
Energy oxidation efficiency is insufficient, and for the average value of the linear relationship r≤0.9998, r of scheme one 0.9997, linear relationship is general.By scheming
6-10 is it is found that the linear relationship of scheme two is r >=0.9999, and the good r average value of linear relationship is 0.99994, and linear relationship has
It is obviously improved.By experimental verification, the ammonia nitrogen on-line oxidation linear relationship of this patent scheme two more preferably, RSD it is more preferable.
Test result is as follows for precision:
The test of 1 scheme of table, one 2.00mg/L precision
The test of one 0.20mg/L precision of table 2-2 scheme
As seen from the above table, it is 1.00% that scheme one, which tests the Ammonia nitrogen standard liquid RSD of 0.2mg/L (n=3), test
Ammonia nitrogen standard liquid (n=8 the uses different extension rates) RSD of 2.0mg/L is 2.35%.
The test of 3 scheme of table, two 0.50mg/L precision
The test of 4 scheme of table, two 0.20mg/L precision
By upper Biao Ke get, scheme two tests the Ammonia nitrogen standard liquid of 0.2mg/L, and RSD (n=6) is 0.80%；Test
The Ammonia nitrogen standard liquid of 0.5mg/L, RSD (n=6) are 0.552%.It can be seen that the precision of scheme two is wanted compared with the precision of scheme one
It is good.
It follows that the scheme of relatively patent CN102628847A of the invention, from linear and precision, oxidation efficiency angle
It sees to have on degree and be obviously improved, have more preferably effect.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (10)
1. a kind of quick oxidation unit of ammonia nitrogen, including an ammonia nitrogen solution delivery branch pipe and an oxidant delivery branch pipe, the ammonia nitrogen
Solution delivery branch pipe output end is equipped with a heater, for the ammonia nitrogen solution to be preheated,
It is characterized in that, further including an oxidation reaction helix tube, the arrival end and the ammonia nitrogen of the oxidation reaction helix tube are molten
The outlet ends of liquid delivery branch pipe and the oxidant delivery branch pipe are connected.
2. the quick oxidation unit of a kind of ammonia nitrogen according to claim 1, which is characterized in that the oxidation reaction helix tube
Internal diameter be 0.5-3mm.
3. the quick oxidation unit of a kind of ammonia nitrogen according to claim 2, which is characterized in that the oxidation reaction helix tube
It is made using plastic material.
4. the quick oxidation unit of a kind of ammonia nitrogen according to claim 1, which is characterized in that the heater is heating water bath
Device, oil bath heater or electric heater.
5. the quick oxidation unit of a kind of ammonia nitrogen according to claim 1, which is characterized in that the heater makes the ammonia nitrogen
Ammonia nitrogen solution in solution delivery branch pipe is heated to 70-95 DEG C.
6. the quick oxidation unit of a kind of ammonia nitrogen according to claim 1, which is characterized in that in the oxidant delivery branch pipe
The oxidant of conveying is hypobromite solutions.
7. a kind of based on a kind of quick method for oxidation of ammonia nitrogen of the quick oxidation unit of ammonia nitrogen as described in claim 1, feature
It is, includes the following steps:
(1) the heated device of ammonia nitrogen solution is preheated, is delivered to oxidation reaction helix tube through ammonia nitrogen solution delivery branch pipe；
(2) oxidant is delivered to oxidation reaction helix tube through oxidant delivery branch pipe；
(3) ammonia nitrogen solution and oxidant carry out oxidation reaction in oxidation reaction helix tube, and oxidant is by the ammonia nitrogen oxygen in solution
Turn to nitrite nitrogen.
8. the quick method for oxidation of ammonia nitrogen according to claim 7, which is characterized in that step (1) described heater makes described
Ammonia nitrogen solution in ammonia nitrogen solution delivery branch pipe is heated to 70-95 DEG C.
9. the quick method for oxidation of ammonia nitrogen according to claim 7, which is characterized in that step (3) ammonia nitrogen solution and oxidant
The time that oxidation reaction is carried out in oxidation reaction helix tube is 3-30 seconds.
10. the quick method for oxidation of ammonia nitrogen according to claim 7, which is characterized in that the oxidant is that hypobromite is molten
Liquid is prepared by the following method to obtain:
(1) potassium bromate, potassium bromide is soluble in water, hypobromite stock solution is configured, the concentration of the potassium bromate is 0.0005-
0.0006g/ml, the concentration of the potassium bromide are 0.03-0.05g/ml；
(2) hypobromite stock solution made from step (1) is mixed with water, hydrochloric acid and sodium hydroxide solution, time bromine is prepared
Sour sodium oxidant, the concentration of hydrochloric acid are 6mol/L, and the sodium hydroxide solution is that the sodium hydroxide that mass fraction is 40% is molten
The volume ratio of liquid, hypobromite stock solution and water, hydrochloric acid and sodium hydroxide solution is 2-4:150:6:50.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910595054.XA CN110201623A (en) | 2019-07-03 | 2019-07-03 | A kind of quick oxidation unit of ammonia nitrogen and the quick method for oxidation of ammonia nitrogen |
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