CN204479467U - Nitrate thermal decomposition product constituent determinator - Google Patents
Nitrate thermal decomposition product constituent determinator Download PDFInfo
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- CN204479467U CN204479467U CN201520148122.5U CN201520148122U CN204479467U CN 204479467 U CN204479467 U CN 204479467U CN 201520148122 U CN201520148122 U CN 201520148122U CN 204479467 U CN204479467 U CN 204479467U
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- decomposition product
- quartz ampoule
- thermal decomposition
- ark
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Abstract
The utility model nitrate thermal decomposition product constituent determinator, comprising: tubular electric resistance case, in described tubular electric resistance case, is provided with corundum Noah's ark; Quartz ampoule, described quartz ampoule is arranged in described tubular electric resistance case, is communicated with described corundum Noah's ark; Gas generating unit, described gas generating unit is communicated with one end of described quartz ampoule; Test cell, described test cell is communicated with the other end of described quartz ampoule by annular condenser pipe; Wherein said test cell comprises the gas automatic on-line monitoring instrument of separate setting, the automatic discontinuous monitor of instrument and absorption process ultraviolet spectrophotometry monitor.The utility model nitrate thermal decomposition product constituent determinator quantitatively accurately can record the composition of decomposition product by instrument automatic discontinuous monitor/ultraviolet spectrophotometer/gas on-line monitoring analyser, and compensate for differential thermal analysis (DTA) and thermogravimetric analysis can only the deficiency of coarse analysis fusing point Sum decomposition point.
Description
Technical field
The utility model relates to metallurgical technology field, particularly relates to a kind of nitrate thermal decomposition product constituent determinator.
Background technology
Nitrate, as industrial conventional thermophore, is commonly employed at chemical industry and new energy field.In chemical industry, often have the reaction that some thermal discharges are very large to carry out in shell and tube reactor, in the reactor, the heat that tube side reacts is taken away by the heat-conducting medium of shell side, and this heat-conducting medium is usually take nitrate as the molten salt system of representative.
Nitrate is liquid more than its fusing point, can use safely, such as, consist of the KNO of 53% in certain temperature range
3, 40% NaNO
2, 7% NaNO
3nitric acid fused salt fusing point be 142 DEG C, can use safely in 150 DEG C to 450 DEG C temperature ranges.When more than 500 DEG C, fused salt just can decompose gradually, generates refractory oxide and gaseous product, thus causes fused salt to lose efficacy, lose the capacity of heat transmission.Once fused salt generation decomposition failure, whole reaction can not lead away heat in time, thus temperature of reaction is acutely raised, and produce the follow-up harm that cannot estimate.
At present, the research of nitric acid molten heat transfer salt intensification decomposable process is mainly fused salt is placed in thermal analyzer, analyze its thermogravimetric (TG) curve in heating process and differential thermal (DTA) curve.By analytic curve, a series of data comprising fusing point, decomposition point can be obtained, but the method cannot provide the variations in detail of fused salt decomposable process, as decomposition product and residue components of molten salt concentration thereof, decomposition gas composition content etc.
Utility model content
The purpose of this utility model is to provide a kind of nitrate thermal decomposition product constituent determinator that can measure nitrate thermal decomposition product constituent.
For solving the problems of the technologies described above, the utility model nitrate thermal decomposition product constituent determinator, comprising: tubular electric resistance case, in described tubular electric resistance case, is provided with corundum Noah's ark; Quartz ampoule, described quartz ampoule is arranged in described tubular electric resistance case, is communicated with described corundum Noah's ark; Gas generating unit, described gas generating unit is communicated with one end of described quartz ampoule; Test cell, described test cell is communicated with the other end of described quartz ampoule by annular condenser pipe; Wherein said test cell comprises the gas automatic on-line monitoring instrument of separate setting, the automatic discontinuous monitor of instrument and absorption process ultraviolet spectrophotometry monitor.
Preferably, described gas generating unit comprises: steel cylinder; Reduction valve, described reduction valve is arranged on described steel cylinder; And spinner-type flowmeter and tensimeter, described spinner-type flowmeter is connected with described reduction valve successively with described tensimeter.
Preferably, between described quartz ampoule and described annular condenser pipe, safety valve is connected with.
Preferably, flange is separately installed with at the two ends of described quartz ampoule.
Preferably, the surface of contact of described quartz ampoule and described tubular electric resistance case is provided with heat-insulating plug.
Preferably, described corundum Noah's ark comprises Noah's ark body and is arranged on the lid on described Noah's ark body.
Preferably, described lid offers multiple pore.
Preferably, described absorption process ultraviolet spectrophotometry monitor comprises the first absorption bottle, oxygen cylinder, the second absorption bottle, surge flask and all band ultraviolet spectrophotometer that connect successively.
The utility model nitrate thermal decomposition product constituent determinator quantitatively accurately can record the composition of decomposition product by instrument automatic discontinuous monitor/ultraviolet spectrophotometer/gas on-line monitoring analyser, and compensate for differential thermal analysis (DTA) and thermogravimetric analysis can only the deficiency of coarse analysis fusing point Sum decomposition point; Tubular electric resistance case freely can arrange heating curve, can control decomposable process and the degree of nitrate, also for the research of research nitrate thermal decomposition rule is provided convenience; Because the caliber of quartz ampoule in tubular electric resistance case is comparatively large, places multiple leptosomatic corundum boat so can walk abreast, contrast test can be carried out easily like this.
Accompanying drawing explanation
Fig. 1 is the utility model nitrate thermal decomposition product constituent assay device structures schematic diagram;
Fig. 2 is the utility model nitrate thermal decomposition product constituent determinator corundum Noah's ark structural representation.
Description of reference numerals in the utility model nitrate thermal decomposition product constituent determinator accompanying drawing:
1-steel cylinder 2-reduction valve 3-spinner-type flowmeter
4-tensimeter 5-flange 6-quartz ampoule
7-heat-insulating plug 8-tubular electric resistance case 9-corundum Noah's ark
10-Noah's ark body 11-safety valve 12-lid
13-annular condenser pipe 14-instrument automatic discontinuous monitor 15-first absorption bottle
16-oxygen cylinder 17-second absorption bottle 18-surge flask
19-all band ultraviolet spectrophotometer 20-gas on-line monitoring analyser 21-pore
Embodiment
Below in conjunction with accompanying drawing, the utility model nitrate thermal decomposition product constituent determinator is described in further detail.
As Fig. 1, shown in Fig. 2, the utility model nitrate thermal decomposition product constituent determinator, whole process is driven by air-flow (airflow direction is shown in thick arrow in Fig. 1), gas is delivered to quartz ampoule 6 by steel cylinder 1, flow in quartz ampoule 6 and take away the decomposition gas reacting and produce, then through cooling the test of laggard line correlation, specific as follows: steel cylinder 1 is furnished with corresponding reduction valve 2, gas from reduction valve 2 out after, lead to spinner-type flowmeter 3, required air-flow velocity is adjusted to through flowmeter 3, after the display of tensimeter 4 pressure is normal, lead to quartz ampoule 6, can shield in high temperature thermal decomposition process on the one hand, the decomposition gas that pyrolysis discharges brings in follow-up receiving flask by the mode can carried by malleation on the other hand, gas can adjust according to the difference of research material Sum decomposition product.
Dismountable flange 5 is equipped with at quartz ampoule two ends, after gas passes through the heat-insulating plug 7 of front end, through the corundum Noah's ark 9 that nitrate to be measured is housed that tubular electric resistance case 3 heats.Corundum Noah's ark 9 to be, thickness identical with Noah's ark body 10 area with area the be corundum lid 12 of 3 millimeters ~ 5 millimeters, this thickness is selected to consider load-bearing and the gas flow rate of quartz ampoule 6, not because weight causes too greatly quartz ampoule 6 high-temperature heating undermined also not because weight too gently causes lid 12 to come off by airflow influence, corundum lid 12 covers on Noah's ark body 10, lid 12 is distinguished without pros and cons, weight is suitable with Noah's ark body 10, so can fit together perfectly (see Fig. 2) with deadweight and surperficial roughening and Noah's ark body 10.The Main Function of lid 12 leaks out when being and preventing liquid fused salt from reaching boiling from Noah's ark, ensure the accuracy of subsequent detection on the one hand, major embodiment makes the fused salt in corundum Noah's ark 9 be heated evenly and prevent fused salt leakage from causing mass loss to heating process, after preventing fused salt from leaking on the other hand, stay the junction of corundum Noah's ark 9 and quartz ampoule 6, the two can be bondd when cooling, reducing the security that operation easier improves operation.In addition lid 12 designs 10 pores 21, pore 21 mainly concentrates on middle part, and point two row's arrangements the gas of reaction decomposes can be allowed to come out flow to next link with carrier gas.In addition, tubular electric resistance case 8 can arrange the parameter such as the rate of heat addition, temperature retention time.
Gas is by the gas of reaction decomposes in the lump with heat-insulating plug 7 to the back-end, and out of control and produce a large amount of gas decomposition products and cause superpressure once fused salt decomposition reaction, safety valve 11 will play decompression function.Then, the method for testing of decomposition gas is selected according to actual conditions.The mensuration of decomposition gas has three kinds of modes, one is pass into the automatic discontinuous monitor 14 (gas chromatograph) of instrument to detect, two is after gas is dissolved in corresponding absorbing liquid, measure its composition by development process all band ultraviolet spectrophotometer 19 in visible region, three is pass into gas on-line monitoring analyser 20.Can according to the method for the cost of the kind of decomposition gas to be determined and the practical operation test corresponding to feasibility option.
Absorbing ultraviolet spectrophotometry is that hot gas leads to annular condenser pipe 13; for cooling down high-temperature gas; the quantity of receiving flask and the kind of collecting liquid are by different for the kind of the decomposition gas collected as required and carry out corresponding adjustment; oxygen cylinder for be oxidized water-fast reducibility gas (as by oxidation of nitric oxide to nitrogen dioxide), surge flask plays buffer protection function.First gas lead to the first absorption bottle 15 that absorbing liquid is housed, nitrogen dioxide wherein will be absorbed by liquid absorption, remaining gas is by being equipped with the oxygen cylinder 16 of acid potassium permanganate subsequently, nitrogen monoxide wherein can be oxidized to nitrogen dioxide, then gas leads to the second absorption bottle 17 that absorbing liquid is housed, be absorbed by liquid absorption, be finally provided with a gas buffer bottle 18, serve the same role with safety valve 11.
The acquisition of decomposable process related data: the mensuration (test selection spectrophotometric method) of 1. decomposing the amount of the nitrogen dioxide of generation: by the solution in the first absorption bottle 15, by " the mensuration hydrochloride naphthodiamide spectrophotometric method of surrounding air oxides of nitrogen (nitrogen monoxide and nitrogen dioxide) " HJ479-2009, in wavelength 540 nanometers, take deionized water as reference, by its absorbance of spectrophotometric determination, and with the standard curve control made in advance, determine its concentration, then calculate the content of nitrogen dioxide according to the gauge of absorbing liquid, 2. the mensuration (test selection spectrophotometric method) of the nitric oxide production amount of generation is decomposed: by the solution in the second absorption bottle 17, by " the mensuration hydrochloride naphthodiamide spectrophotometric method of surrounding air oxides of nitrogen (nitrogen monoxide and nitrogen dioxide) " HJ479-2009, in wavelength 540 nanometers its absorbance of spectrophotometric determination, and with the standard curve control made in advance, determine its concentration, calculate the content of nitrogen dioxide again according to the gauge of absorbing liquid, then be scaled nitric oxide production quality according to the ratio of molal weight, 3. the mensuration of nitrate radical content in residual salts: remaining salt is dissolved in water, by " the mensuration part 1 of boiler feed water and chilled water analytical approach NO3-N and NO2-N: nitrate Ultraviolet Photometric Method " GB/T6912.1-2006, first add sulfamic acid solution destruction nitrite anions wherein, then at wavelength 219 nanometers (sulfaminic acid, the generation product that sulfaminic acid and sodium nitrite react in wavelength 219 nanometers without absorbance, and sulfaminic acid add the mensuration that can not affect nitrate radical), take deionized water as reference, measure the absorbance of nitrate radical, and with the standard curve control made in advance, determine its concentration, again according to the water yield that residual salts is dissolved in, determine the content of nitrate radical, 4. the mensuration of residual salts Nitrite content: remaining salt is dissolved in water, by " mensuration of boiler feed water and chilled water analytical approach nitrite " GB/T6912-2008, remove two parts of solution, first part adds sulfamic acid solution destruction nitrite anions wherein as reference, second part is liquid to be measured, then at wavelength 219 nanometers (sulfaminic acid, the generation product that sulfaminic acid and sodium nitrite react in wavelength 219 nanometers without absorbance, and sulfaminic acid add the mensuration that can not affect nitrate radical) measure the absorbance of nitrite anions, and with the standard curve control made in advance, determine its concentration, again according to the water yield that residual salts is dissolved in, determine the content of nitrite anions.
Measure 5g nitric acid fused salt (mass ratio of potassium nitrate, sodium nitrite and sodium nitrate is 53:40:7), twice experiment, is once heated to 500 DEG C from room temperature, is once heated to 550 DEG C from room temperature, and nitrates decompose situation is as follows:
500 DEG C: generate nitrogen dioxide 1.2 μ g, generate nitrogen monoxide 40 μ g, containing nitrate radical 1.873g in remaining salt, containing nitrite anions 1.311g in remaining salt.
550 DEG C: generate nitrogen dioxide 65.9 μ g, generate nitrogen monoxide 157.6 μ g, containing nitrate radical 1.703g in remaining salt, containing nitrite anions 1.176g in remaining salt.
Initial analysis, along with the rising of temperature, nitrates decompose process nitrogen dioxide and nitric oxide production growing amount increase; Along with the rising nitrate radical of temperature and the loss amount of nitrite anions increase.
The utility model nitrate thermal decomposition product constituent determinator quantitatively accurately can record the composition of decomposition product by instrument automatic discontinuous monitor/ultraviolet spectrophotometer/gas on-line monitoring analyser, and compensate for differential thermal analysis (DTA) and thermogravimetric analysis can only the deficiency of coarse analysis fusing point Sum decomposition point; Tubular electric resistance case freely can arrange heating curve, can control decomposable process and the degree of nitrate, also for the research of research nitrate thermal decomposition rule is provided convenience; Because the caliber of quartz ampoule in tubular electric resistance case is comparatively large, places multiple leptosomatic corundum boat so can walk abreast, contrast test can be carried out easily like this.
Below the preferred embodiment that the utility model is created is illustrated, but the utility model is created and is not limited to described embodiment, those of ordinary skill in the art also can make all equivalent modification or replacement under the prerequisite without prejudice to the utility model creative spirit, and these equivalent modification or replacement are all included in the application's claim limited range.
Claims (8)
1. nitrate thermal decomposition product constituent determinator, is characterized in that, comprising:
Tubular electric resistance case, is provided with corundum Noah's ark in described tubular electric resistance case;
Quartz ampoule, described quartz ampoule is arranged in described tubular electric resistance case, is communicated with described corundum Noah's ark;
Gas generating unit, described gas generating unit is communicated with one end of described quartz ampoule;
Test cell, described test cell is communicated with the other end of described quartz ampoule by annular condenser pipe; Wherein
Described test cell comprises the gas automatic on-line monitoring instrument of separate setting, the automatic discontinuous monitor of instrument and absorption process ultraviolet spectrophotometry monitor.
2. nitrate thermal decomposition product constituent determinator according to claim 1, it is characterized in that, described gas generating unit comprises:
Steel cylinder;
Reduction valve, described reduction valve is arranged on described steel cylinder; And
Spinner-type flowmeter and tensimeter, described spinner-type flowmeter is connected with described reduction valve successively with described tensimeter.
3. nitrate thermal decomposition product constituent determinator according to claim 1, is characterized in that, between described quartz ampoule and described annular condenser pipe, be connected with safety valve.
4. the nitrate thermal decomposition product constituent determinator according to claim 1 or 3, is characterized in that, be separately installed with flange at the two ends of described quartz ampoule.
5. nitrate thermal decomposition product constituent determinator according to claim 4, is characterized in that, the surface of contact of described quartz ampoule and described tubular electric resistance case is provided with heat-insulating plug.
6. nitrate thermal decomposition product constituent determinator according to claim 1, is characterized in that, described corundum Noah's ark comprises Noah's ark body and is arranged on the lid on described Noah's ark body.
7. nitrate thermal decomposition product constituent determinator according to claim 6, is characterized in that, described lid offers multiple pore.
8. nitrate thermal decomposition product constituent determinator according to claim 1, it is characterized in that, described absorption process ultraviolet spectrophotometry monitor comprises the first absorption bottle, oxygen cylinder, the second absorption bottle, surge flask and all band ultraviolet spectrophotometer that connect successively.
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| CN201520148122.5U CN204479467U (en) | 2015-03-16 | 2015-03-16 | Nitrate thermal decomposition product constituent determinator |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424540A (en) * | 2015-11-30 | 2016-03-23 | 国网河南省电力公司电力科学研究院 | Testing device for volatilization properties of ammonium bisulfate in coal-fired flue gas |
-
2015
- 2015-03-16 CN CN201520148122.5U patent/CN204479467U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424540A (en) * | 2015-11-30 | 2016-03-23 | 国网河南省电力公司电力科学研究院 | Testing device for volatilization properties of ammonium bisulfate in coal-fired flue gas |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150715 Termination date: 20170316 |