CN108693204B - Potassium salt composition on-line measuring device - Google Patents
Potassium salt composition on-line measuring device Download PDFInfo
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- CN108693204B CN108693204B CN201810592498.3A CN201810592498A CN108693204B CN 108693204 B CN108693204 B CN 108693204B CN 201810592498 A CN201810592498 A CN 201810592498A CN 108693204 B CN108693204 B CN 108693204B
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- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 title claims abstract description 118
- 239000000203 mixture Substances 0.000 title claims description 3
- 230000007246 mechanism Effects 0.000 claims abstract description 79
- 239000000463 material Substances 0.000 claims abstract description 67
- 238000005259 measurement Methods 0.000 claims abstract description 55
- 238000001514 detection method Methods 0.000 claims abstract description 50
- 238000012937 correction Methods 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 35
- 238000007493 shaping process Methods 0.000 claims abstract description 20
- 238000012544 monitoring process Methods 0.000 claims abstract description 11
- 238000007405 data analysis Methods 0.000 claims abstract description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 56
- 238000004876 x-ray fluorescence Methods 0.000 claims description 47
- 239000001103 potassium chloride Substances 0.000 claims description 35
- 235000011164 potassium chloride Nutrition 0.000 claims description 35
- 238000007790 scraping Methods 0.000 claims description 31
- 238000006073 displacement reaction Methods 0.000 claims description 16
- 239000000523 sample Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000004364 calculation method Methods 0.000 claims description 14
- 238000010926 purge Methods 0.000 claims description 11
- 229910001220 stainless steel Inorganic materials 0.000 claims description 11
- 239000010935 stainless steel Substances 0.000 claims description 11
- 238000004891 communication Methods 0.000 claims description 9
- 239000004065 semiconductor Substances 0.000 claims description 9
- 238000013519 translation Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 8
- 238000009434 installation Methods 0.000 claims description 7
- 230000006870 function Effects 0.000 claims description 6
- 239000010963 304 stainless steel Substances 0.000 claims description 5
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 5
- 238000002474 experimental method Methods 0.000 claims description 5
- 210000001503 joint Anatomy 0.000 claims description 5
- 238000007477 logistic regression Methods 0.000 claims description 4
- 230000006855 networking Effects 0.000 claims description 4
- 230000000737 periodic effect Effects 0.000 claims description 4
- 159000000001 potassium salts Chemical class 0.000 claims description 4
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 230000035515 penetration Effects 0.000 claims description 3
- 229920002530 polyetherether ketone Polymers 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000001917 fluorescence detection Methods 0.000 abstract description 3
- 238000004458 analytical method Methods 0.000 description 16
- 229910052700 potassium Inorganic materials 0.000 description 11
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 10
- 239000011591 potassium Substances 0.000 description 10
- 230000008901 benefit Effects 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 7
- 238000010408 sweeping Methods 0.000 description 6
- 239000003337 fertilizer Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000009616 inductively coupled plasma Methods 0.000 description 3
- 238000002536 laser-induced breakdown spectroscopy Methods 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- -1 sodium tetraphenylborate Chemical compound 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 238000003321 atomic absorption spectrophotometry Methods 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000608 laser ablation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003947 neutron activation analysis Methods 0.000 description 2
- 230000008447 perception Effects 0.000 description 2
- 229940072033 potash Drugs 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 235000015320 potassium carbonate Nutrition 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 229910001369 Brass Inorganic materials 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001804 chlorine Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011900 installation process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000003032 molecular docking Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses an on-line detection device for potassium salt components, which comprises a material shaping mechanism for flattening the surface of potassium salt; x fluorescent element on-line measuring mechanism with distance measuring sensor for measuring potassium salt element component; an on-line moisture measuring mechanism for potassium salt moisture measurement; and an industrial control computer system for system control and data analysis; the method utilizes the online moisture meter to monitor the moisture content of the potassium salt material, is used for online monitoring of the potassium salt moisture, is also used for influence correction of X fluorescence intensity, reduces the influence of moisture fluctuation on the X fluorescence intensity, and improves the X fluorescence detection precision.
Description
Technical Field
The invention relates to the field of detection of industrial material components, in particular to an on-line detection device for potassium salt components.
Background
The Chinese soluble potassium salt resource is seriously deficient, the ascertained reserves are mainly potassium chloride, and most ore deposits have the disadvantages of poor construction conditions, low potassium grade, high development cost and the like. 95% of potassium salt in the world is used as fertilizer, china is a large agricultural country, and the consumption of potassium fertilizer is large, so that the requirement is always maintained mainly by import. In recent years, with the development of potassium salt industry, the self-supporting rate of domestic potassium salt is continuously improved, but the high-grade potassium salt still depends on imported supply too much.
In order to improve the utilization rate of soluble potassium resources, various countries are dedicated to improving the technology of potassium salt production, and meanwhile, in order to cooperate with real-time monitoring of chlorine salt components in the purification process, a simple, rapid and accurate potassium salt component detection method needs to be developed. On the one hand, the application of the perception detection equipment represented by on-line detection can provide large quality monitoring data for the potassium salt industry, and the perception detection equipment has become the basis for improving the process and realizing intelligent manufacturing. On the other hand, in the unique field of industrial analysis, it is sought to maximize economic benefits in the shortest time. Therefore, compared with other application fields, a technology capable of performing real-time online analysis is most urgently needed.
The conventional methods for measuring potassium salt components mainly include the following: sodium tetraphenylborate gravimetric, flame atomic absorption spectrophotometry, derivative spectrophotometry, inductively coupled plasma emission spectrometry, and X-ray fluorescence analysis. The sodium tetraphenylborate gravimetric method is a national standard method for detecting potassium element, belongs to a chemical method, and has complex experimental operation; the flame atomic absorption spectrophotometry is simple and convenient to operate, but takes a long time, and multiple elements cannot be analyzed simultaneously; derivative spectrophotometry improves the resolution of the spectrum, can separate respective absorption peaks from overlapped absorption spectra, and can obtain higher quantitative accuracy, but the calculation process takes too long time; the inductively coupled plasma emission spectrometry has the advantages of high analysis speed, low detection limit and high precision, but higher equipment and operation cost and unobvious advantage on chlorine element in potassium salt.
The X-ray fluorescence analysis is also called as X-ray fluorescence analysis method, which utilizes the energy and intensity of X-ray fluorescence emitted by the sample after being irradiated by X-rays to analyze and determine the components and content of the sample, and has the advantages of high analysis speed, simultaneous multi-element analysis, high detection precision and simple operation and maintenance. The above five methods have advantages in terms of detection time, detection limit, application range and the like, wherein the sodium tetraphenylborate gravimetric method and the table type X-ray fluorescence analyzer are commonly applied to an assay workshop of a potassium salt factory, but all the above five methods depend on a manual sampling and sending and detecting sample preparation process, not only require a large amount of manpower, but also have the problem of sampling representativeness, are limited to the use in the assay room, and are difficult to realize real-time online detection on an industrial production site.
The instant gamma neutron activation analysis (PGNAA) and the Laser Induced Breakdown Spectroscopy (LIBS) in the current industrial online detection field are paid attention to, the instant gamma neutron activation analysis technology has the remarkable advantages of high sensitivity, nondestructivity and suitability for online analysis of large samples, but the technology is limited by a reaction section, has insignificant detection advantages on potassium elements, is expensive in operation and maintenance and complex in technology, has a service life of 1 to 2 years for neutron tubes and neutron sources, needs to deal with environmental protection licenses for replacing the neutron tubes and the neutron sources, and increases maintenance cost. The laser-induced breakdown spectroscopy (LIBS) is a laser ablation spectroscopy analysis technology, can rapidly and simply perform quantitative analysis and qualitative analysis on elements in a sample, can be applied to the field of industrial online analysis, but is not mature at present, so that the LIBS is developed into a mature quantitative analysis technology with high sensitivity and high detection limit, a great deal of research work is needed, such as solving the problems of influence of laser power density, interference of third element, physical and chemical properties of the sample to be analyzed, pressure of environmental gas, geometric and mechanical properties of the sample surface and the like, and is mainly applicable to the field of samples with harder surfaces such as steel and metallurgy, and loose powdery potassium salt on a conveying belt is easy to splash in the laser ablation process to influence the measurement accuracy of the equipment.
The quality supervision of potassium salt is implemented in national standard of the people's republic of China (GB 6549-2011), wherein the potassium salt is classified into class I and class II potassium salt according to the technical requirements of industry and agriculture, the content of potassium chloride (which is converted into potassium oxide or potassium element content) is the most important technical index of the class classification standard, and is also a key factor influencing the quality and sales of products. The water content is another important parameter which can monitor the production process of the potash fertilizer besides the content of the potassium chloride, so that the method is particularly important for simultaneously detecting the potassium chloride component and the water content in the potash fertilizer on line.
Disclosure of Invention
The invention provides an on-line detection device for potassium salt components. The method can realize the simultaneous high-precision online measurement of the potassium salt element components and the moisture, and solve the problems of uneven potassium salt materials, unstable material quantity and the influence of moisture fluctuation on the measurement precision of X fluorescent elements. Provides accurate quality monitoring big data for potassium salt industry, and has stable power assisting and improved production process.
The invention adopts the following technical scheme:
an on-line detection device for potassium salt components comprises a material shaping mechanism for flattening the surface of potassium salt; x fluorescent element on-line measuring mechanism with distance measuring sensor for measuring potassium salt element component; an on-line moisture measuring mechanism for potassium salt moisture measurement; and an industrial control computer system for system control and data analysis; the material shaping mechanism, the X fluorescent element online measuring mechanism and the online moisture measuring mechanism are sequentially arranged above the potassium salt conveying belt conveyor from front to back and are mutually matched, the material shaping mechanism acts on materials to enable the surfaces of the potassium salt to be smooth and flat, so that the accuracy of measuring results of the rear X fluorescent element online measuring mechanism and the online moisture measuring mechanism is facilitated, the measuring results of moisture values are used for accurately compensating the influence of moisture changes on the measuring results of the X fluorescent element online measuring mechanism, the ranging sensor is used for monitoring material quantity fluctuation and used for distance compensation correction of X fluorescent intensity, and the organic combination of the three mechanisms ensures the high accuracy of X fluorescent measurement.
The potassium salt component online detection device comprises a material shaping mechanism, a material shaping mechanism and a potassium salt component online detection device, wherein the material shaping mechanism comprises a high-level scraping plate 1, a low-level scraping plate 2 and a movable scraping plate 3, and is used for flattening the surface of potassium salt; the high-position scraping plate 1, the low-position scraping plate 2 and the movable scraping plate 3 are sequentially arranged above the conveyor along the conveying direction of the potassium salt, the front end of the high-position scraping plate 1 is of a triangular structure, the bottom of the high-position scraping plate is open, the material layer with higher potassium salt is subjected to peak clipping, the low-position scraping plate 2 is of a triangular structure, the bottom of the high-position scraping plate is open, the mounting height of the high-position scraping plate is lower than that of the high-position scraping plate 1, the high-position scraping plate is positioned at the rear end of the high-position scraping plate 1 and at a distance of more than 50cm, the movable scraping plate 3 is of a rectangular plate-shaped structure, and a top connecting bearing is fixed at the rear end of the low-position scraping plate 2 and provided with a counterweight for flattening treatment of the potassium salt material.
The potassium salt component online detection device comprises an X-ray tube 4, an X-ray collimator 5, a high-voltage power supply 6, an X-fluorescence detector 7, a digital multichannel spectrometer 8, a combined displacement adjusting table 9, a measurement window 10, a purge air pump 11, a CCD digital camera 12, an X-fluorescence calibration device 13, a constant temperature control device 14, a condensate water collecting device 15, an Ethernet communication module 16, a shielding protection body 17 and a ranging sensor 18; in the X-ray fluorescent element on-line measuring mechanism, an X-ray tube 4, an X-ray collimator 5, a high-voltage power supply 6, an X-ray fluorescent detector 7, a digital multichannel spectrometer 8, a combined displacement adjusting table 9, a measuring window 10, a purge air pump 11, a CCD digital camera 12, an X-ray fluorescent calibrating device 13, a constant temperature control device 14, a condensed water collecting device 15 and an Ethernet communication module 16 are all arranged in a shielding protection body 17; the X-ray collimator 5 is connected with the X-ray tube 4, and the included angle between the center line of the X-ray collimator 5 and the surface of the sylvite is not less than 50 degrees.
The potassium salt component on-line detection device is characterized in that the combined displacement adjustment table 9 is formed by combining a X, Y, Z axis translation table and an alpha axis angular displacement table, is connected with the X fluorescence detector 7 and is used for adjusting the included angle between the central line of the probe of the X fluorescence detector 7 and the surface of the potassium salt to be not less than 55 degrees.
The potassium salt component on-line detection device is characterized in that the probe center of the X-ray fluorescence detector 7 and the outlet center of the X-ray collimator 5 are positioned on the same horizontal plane and are 5mm away from the upper surface of the measurement window 10, the central axes of the X-ray collimator 5 and the X-ray fluorescence detector 7 are intersected with the central axis of the measurement window 10, the intersection point is positioned at the position about 20mm below the measurement window 10, and the included angle between the central line of the X-ray collimator 5 and the potassium salt surface is 55 degrees; the X-ray fluorescence detector 7 is mounted on a multi-dimensional (xyzzα) combined displacement adjustment table 9, and the angle between the center line of the X-ray fluorescence detector 7 and the surface of the potassium salt is 55 °.
The potassium salt component on-line detection device is characterized in that the measurement window body 10 is positioned at the center of a bottom plate of the shielding protection body 17 and comprises a polyether-ether-ketone rim structure with a sweeping air hole and a polyimide film, wherein the sweeping air hole is connected with a sweeping air pump 11, and the surface of the film is swept and ash is removed.
The X-ray fluorescence calibration device 13 comprises a standard 304 stainless steel sheet and a translation table driven by a stepping motor, when the stainless steel sheet is driven in a translation way and shields the upper surface of the measurement window 10, source-level X-rays emitted by the X-ray tube 4 are directly irradiated on the stainless steel sheet, and the X-ray fluorescence calibration device 13 can conveniently and rapidly realize the periodic calibration of an X-ray fluorescence element online measurement mechanism quantitative calculation model and the detection of functional faults.
The potassium salt component on-line detection device is characterized in that the constant temperature control device 14 is positioned at the upper part in the shielding protection body 17 and consists of a EKW-1000 type remote networking temperature controller, a temperature sensor, a 200W semiconductor refrigerator and a semiconductor heater, and is used for monitoring the temperature in equipment and controlling the constant temperature, wherein the semiconductor refrigerator is in butt joint with the condensed water collection device 15, and the temperature range in an X fluorescent element on-line measurement mechanism is set to be 25-35 ℃.
The potassium salt component on-line detection device is characterized in that a distance measuring sensor 18 is arranged on the outer side of the shielding protection body 17, vertically irradiates the surface of a potassium salt material, is used for measuring the distance of the surface of the potassium salt material relative to the X fluorescence measurement mechanism in real time, feeds back the change of the material quantity, and is used for compensating and correcting the distance of the X fluorescence intensity; the on-line moisture meter 19 is installed outside the shielding protection body 17 and is on the same central line with the measuring window body 10 to vertically irradiate the surface of the sylvite material.
According to the potassium salt component on-line detection device, helium gas injection devices are added in the space environment between the X fluorescence detector probe and the measurement window and the space environment between the potassium salt and the measurement window, so that the absorption of air to low-energy X fluorescence can be reduced, and the measurement sensitivity to light elements such as Na, mg, al and Si is improved.
The potassium salt component on-line detecting device is characterized in that the front end of the X-ray collimator, the probe of the X-ray fluorescence detector and the measuring window are sealed in a cavity of an acrylic structure, sealing rings are arranged at the joints of the front end of the X-ray collimator, the probe of the X-ray fluorescence detector and the measuring window, and a vacuum cylinder and a vacuum pump are sequentially connected in the cavity to vacuumize the cavity.
The potassium salt component on-line measuring device, material plastic structure in can add roller structure and roll extrusion to potassium salt surface, its aim at improves potassium salt material surface smoothness and closely knit degree, reduces the base body effect influence, improves measurement accuracy.
The method for on-line detection of potassium salt component of any one of the on-line detection devices, comprising the steps of: firstly, flattening the surface of potassium salt; then measuring the potassium salt element component by adopting an X fluorescent element on-line measuring mechanism; synchronously acquiring the water content of potassium salt and fluctuation data of the potassium salt; the influence of the moisture change on the measurement result of the X fluorescent element online measurement mechanism is accurately compensated according to the measurement result of the potassium salt moisture content, and the X fluorescent intensity is subjected to distance compensation correction by adopting a distance compensation correction method according to the fluctuation of the potassium salt material quantity;
the distance compensation correction method of the X fluorescence intensity is shown in the following formula (1) according to the exponential decay law of the monoenergetic X-ray in the material penetration process, and the correction method is shown in the formula (2):
in the middle ofThe X fluorescence intensity after the compensation and correction for the distance influence; />The distance D obtained by direct measurement of the X-ray fluorescence detector x X fluorescence intensity at time; d (D) x D, for the distance between the surface of the sylvite material measured by the distance measuring sensor and the bottom of the distance measuring sensor 0 The distance from the bottom of the ranging sensor to the bottom plate of the X fluorescent element on-line measuring mechanism is a fixed value related to the installation height of the ranging sensor; a. t and b are coefficients in an exponential function, and for potassium salts with different potassium chloride contents, a, t and b can be measured through analog calculation or experiments;
the moisture influence correction of the X fluorescence intensity is that a Logistic regression analysis model is established through statistics of moisture values and probability distribution rules of the X fluorescence intensity, the correction method is shown in the following formula (3), and the correction method is shown in the formula (4):
I＝A2+(A1-A2)/(1+(M x /x0) p ) (3)
wherein M is 0 For the water content reference value, M x In order to measure the value of the moisture,for a moisture value of M 0 Intensity of time X fluorescence, < >>For a moisture value of M x The X fluorescence intensity at the time, A1, A2, X0 and p are equation coefficients, which can be obtained by experimental measurement.
The specific steps of the distance compensation correction method of X fluorescence intensity are as follows:
(1) a, measuring a and t values under different potassium chloride contents through analog calculation or experiments, and establishing a data calculation model;
(2) the X fluorescence intensity measured by the X fluorescence measuring mechanism isThe distance value measured by the distance measuring sensor is D x ；
(3) Comparing the measured value D of the distance x And default value D 0 Size, if D x And D 0 Equal, no correction is performed; if D x And D 0 Equal, at this time, the potassium chloride content is assumed to be Ca;
(4) calculating from (1) the corresponding a and t values at this content using the assumed Ca-x of the potassium chloride content;
(5) obtaining X fluorescence intensity value after distance compensation correction through calculation of (2)
(6) Will beCarrying out an original content calculation model of the X fluorescence measurement mechanism to obtain corrected potassium chloride content Ca;
(7) if |Ca| -Ca|is less than or equal to the limit error value, the correction process is terminated, the potassium chloride content result of potassium salt is Ca, otherwise, the operation is continued after returning to the step (3).
The invention has the following beneficial effects:
1) The invention relates to a potassium salt component online analysis method and a potassium salt component online analysis device, which realize simultaneous online measurement of element components and moisture, solve the problems of result hysteresis and sampling representative errors of the traditional manual sampling analysis method, and provide reliable quality detection big data for a potassium salt factory;
2) The distance measuring device monitors the distance of the surface of the potassium salt material relative to the X fluorescent element on-line measuring mechanism by using the distance measuring sensor, is used for compensating and correcting the distance of the X fluorescent intensity, reduces the influence of potassium salt material fluctuation on the X fluorescent intensity, and improves the X fluorescent detection precision;
3) The method utilizes the online moisture meter to monitor the moisture content of the potassium salt material, is used for online monitoring of the potassium salt moisture and correction of the influence of the X fluorescence intensity, reduces the influence of moisture fluctuation on the X fluorescence intensity, and improves the X fluorescence detection precision;
4) The invention adopts the material shaping mechanism to carry out peak clipping and flattening treatment on the surface of the potassium salt material, so that the surface of the material is smooth and flat, and the influence of the matrix effect on X fluorescence detection precision is reduced;
5) The window film with high mechanical strength and high X-ray transmittance is adopted, so that the high X-ray transmittance is ensured, and the window and the periphery are kept clean by combining a purging system, so that the structure design is reasonable;
6) The invention utilizes the low-power running X-ray tube and the constant temperature control device, improves the stability of the equipment and prolongs the service life of the X-ray tube.
7) The invention utilizes the stepping motor to drive the standard 304 stainless steel sheet to enable the standard 304 stainless steel sheet to translate to the surface of the measurement window, realizes the periodic calibration of the X fluorescence measurement system, and ensures the measurement precision.
8) The method realizes the remote online detection of the potassium salt component by using the Ethernet communication mode, ensures the safe and efficient storage and docking of the detection result to the main control system of the factory, is convenient for the secondary development and utilization of the detection result, and has the remarkable advantage of networking.
Drawings
FIG. 1 is a schematic diagram showing the structure of an on-line analysis apparatus for potassium salt component according to the present invention;
FIG. 2 is a front view of an online measurement mechanism for X-ray fluorescence elements in accordance with one embodiment of the present disclosure;
FIG. 3 is a left side view of an X-ray fluorescence element on-line measuring mechanism in an embodiment of the invention;
FIG. 4 is a front view of a lower scraper mounting structure in a material shaping mechanism according to an embodiment of the present invention;
FIG. 5 is a side view of a low-profile flight mounting structure in a material shaping mechanism in accordance with an embodiment of the present invention;
FIG. 6 is a front view of a movable screed mounting structure in a material truing mechanism in accordance with an embodiment of the present invention;
FIG. 7 is a partial cross-sectional view of a movable screed mounting structure in a material truing mechanism in accordance with an embodiment of the present invention;
FIG. 8 is a side view of a movable screed mounting structure in a material truing mechanism in accordance with an embodiment of the present invention;
FIG. 9 is a graph showing the relationship and fit function between the X fluorescence intensity value I and the distance value D measured by the X fluorescence element on-line measuring mechanism and the distance measuring sensor in the embodiment of the present invention.
FIG. 10 shows the variation law and fitting function of the measured X fluorescence intensity of the potassium element at different moisture drying times obtained in the examples of the present invention.
FIG. 11 is a calibration curve for quantitative analysis of potassium chloride obtained by distance compensation correction and moisture influence correction in the example of the present invention.
1. A high-level scraper; 2: a low-level scraper; 3: a movable scraper; 4: an X-ray tube; 5: an X-ray collimator; 6: a high voltage power supply; 7: an X-ray fluorescence detector; 8: a digital multichannel spectrometer; 9: a combined displacement adjusting table; 10: measuring a window; 11: purging the air pump; 12: a CCD digital camera; 13: an X-ray fluorescence calibration device; 14: a constant temperature control device; 15: a condensed water collecting device; 16: an Ethernet communication module; 17: shielding the protective body; 18: a ranging sensor; 19: an on-line moisture meter; 20: an industrial control computer; 21: a data display and printing system. 23. A movable boom assembly; 24. hoisting the bracket component; 25. the floor hoisting bracket component; 26. spiral lifting suspender; 27. a steel rope; 28. a weight plate; 29. a long pin shaft; 30. and a belt conveyor.
Detailed Description
The present invention will be described in detail with reference to specific examples.
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be noted that, unless explicitly specified and defined otherwise, the term "X-fluorescence" may be understood as a characteristic X-ray fluorescence based on an analysis method of X-ray fluorescence and an element being excited, as the case may be, and the specific meaning of the above term in the present invention may be understood by one of ordinary skill in the art as the case may be; the upper part and the lower part are all based on the position description of the object placement mode in the attached drawings; both the "front" and the "rear" refer to the transport direction of the sample, and the upstream position is the front, and the downstream position is the rear.
As shown in FIG. 1, the invention discloses an on-line detection device for potassium salt components, which comprises a material shaping mechanism for flattening the surface of potassium salt; x fluorescent element on-line measuring mechanism with distance measuring sensor for measuring potassium salt element component; an on-line moisture measuring mechanism for potassium salt moisture measurement; and an industrial control computer system for system control and data analysis. The material shaping mechanism, the X fluorescent element online measuring mechanism and the online moisture measuring mechanism are sequentially arranged above the potassium salt conveying belt conveyor from front to back and are mutually matched, the material shaping mechanism acts on materials to enable the surfaces of the potassium salt to be smooth and flat, so that the accuracy of measuring results of the rear X fluorescent element online measuring mechanism and the online moisture measuring mechanism is facilitated, the measuring results of moisture values are used for accurately compensating the influence of moisture changes on the measuring results of the X fluorescent element online measuring mechanism, the ranging sensor is used for monitoring material quantity fluctuation and used for distance compensation correction of X fluorescent intensity, and the organic combination of the three mechanisms ensures the high accuracy of X fluorescent measurement.
In one embodiment of the invention, as shown in fig. 2 and 3, the structure and the installation mode of the X fluorescence element on-line measuring mechanism are that the structure of an X fluorescence main body (shielding protective body 17) adopts a movable hoisting mode, a hoisting support assembly 24 is installed on a belt conveyor 30 for conveying potassium salt on site, the bottom of a movable boom assembly 23 is connected with the shielding protective body 17 through a bearing, the top of the movable boom assembly is connected with the hoisting support assembly 24 through a threaded boom, and the levelness adjustment and the height adjustment of the structure of the X fluorescence main body in the installation process can be realized by using the threaded boom. The bottom of the shielding protection body 17 is designed into a ship-shaped structure, and the ship head is opposite to the feeding direction, so that the peak clipping and flattening treatment of the materials under special working conditions can be realized. The distance measuring sensor 18 is fixedly arranged on the outer side of the rear end of the shielding protection body 17 through a machine and vertically irradiates the surface of the sylvite material.
The material shaping mechanism comprises a high-level scraping plate 1, a low-level scraping plate 2 and a movable scraping plate 3 and is used for flattening the surface of potassium salt; the X-ray fluorescent element online measuring mechanism comprises an X-ray tube 4, an X-ray collimator 5, a high-voltage power supply 6, an X-ray fluorescent detector 7, a digital multichannel spectrometer 8, a combined displacement adjusting table 9, a measuring window 10, a purge air pump 11, a CCD digital camera 12, an X-ray fluorescent calibrating device 13, a constant temperature control device 14, a condensed water collecting device 15, an Ethernet communication module 16, a shielding protection body 17 and a ranging sensor 18; the online moisture measuring mechanism comprises an online moisture meter 19;
x-ray tube 4, X-ray collimator 5, power supply 6 and X-fluorescence in an X-fluorescence element on-line measuring mechanismThe light detector 7, the digital multichannel spectrometer 8, the combined displacement adjusting table 9, the measuring window 10, the purge air pump 11, the CCD digital camera 12, the X fluorescence calibration device 13, the constant temperature control device 14, the condensed water collecting device 15 and the Ethernet communication module 16 are all arranged in the shielding protection body 17. The X-ray tube 4 is provided with a metal Cr target, a brass shell and an X-ray tube with the highest power of 50W, and the running power is less than 10W, so that the high-efficiency excitation of K and Cl elements is realized; the X-ray collimator 5 is made of high-purity aluminum, has the length of 30mm, the aperture of 3mm, the outer diameter of 10mm, and is coated with lead foil with the thickness of 200 mu m on the outer layer for shielding transmitted X-rays, the X-ray collimator 5 is connected with the X-ray tube 4, and the included angle between the center line of the X-ray collimator 5 and the surface of the sylvite is not less than 50 degrees; the X fluorescence detector 7 adopts a high-count rate silicon drift detector with a detection area of 25mm 2 The method is used for high-efficiency recording of the element characteristic X fluorescence;
the CCD digital camera 12 is provided with a 12-time lens for a compact type camera, is 25cm away from the measurement window and is used for remotely checking the internal conditions of the measurement window 10 and equipment;
the center of the probe of the X-ray fluorescence detector 7 and the center of the outlet of the X-ray collimator 5 are positioned on the same horizontal plane and are 5mm away from the upper surface of the measuring window 10, the central axes of the X-ray collimator 5 and the X-ray fluorescence detector 7 are intersected with the central axis of the measuring window 10, the intersection point is positioned at the position about 20mm below the measuring window 10, and the included angle between the central axis of the X-ray collimator 5 and the surface of the sylvite is 55 degrees. The X-ray fluorescence detector 7 is mounted on a multi-dimensional (xyzzα) combined displacement adjustment table 9, and the angle between the center line of the X-ray fluorescence detector 7 and the surface of the potassium salt is 55 °.
The combined displacement adjusting table 9 is formed by combining a X, Y, Z axis translation table and an alpha axis angular displacement table, is connected with the X fluorescence detector 7 and is used for adjusting the included angle between the central line of the probe of the X fluorescence detector 7 and the surface of the sylvite to be not less than 55 degrees.
The measuring window body 10 is positioned at the center of the bottom plate of the shielding protection body 17, has a diameter of 50mm, comprises a polyether-ether-ketone rim structure with a sweeping air hole and a polyimide film with a thickness of 12.5 mu m, and the sweeping air hole is connected with a sweeping air pump 11 to sweep and clean the surface of the film. The horizontal distance between the lower surface of the measuring window body 10 and the upper surface of the potassium salt material is less than 30mm.
The X-ray fluorescence calibration device 13 comprises a standard 304 stainless steel sheet with the thickness of 2mm and a translation table driven by a stepping motor, when the stainless steel sheet is driven in a translation way and shields the upper surface of the measurement window 10, source-level X-rays emitted by the X-ray tube 4 directly irradiate the stainless steel sheet, almost all X-rays detected by the X-ray fluorescence detector 7 come from the X-rays emitted by the stainless steel sheet after being excited by the source-level X-rays, and the periodic calibration of an X-ray fluorescence element online measurement mechanism quantitative calculation model can be conveniently and quickly realized by utilizing the X-ray fluorescence calibration device 13 due to the stable element component content of the stainless steel sheet; in addition, if the fluorescence intensity of the stainless steel sheet X detected by the X-ray fluorescence detector 7 is obviously reduced, it indicates that the X-ray tube 4 may have performance degradation conditions such as cathode filament aging and anode target damage, so that the emitted source level X-ray intensity is attenuated, or functional faults such as thermal noise enhancement, leakage counting rate increase, and poor detection efficiency may occur in the X-ray fluorescence detector 7.
The constant temperature control device 14 is positioned at the upper part in the shielding protection body 17 and consists of a EKW-1000 remote networking temperature controller, a temperature sensor, a 200W semiconductor refrigerator and a semiconductor heater, and is used for monitoring the temperature in the equipment and controlling the constant temperature, wherein the semiconductor refrigerator is in butt joint with the condensed water collecting device 15, and the temperature range in the X fluorescent element on-line measuring mechanism is set to be 25-35 ℃.
The distance measuring sensor 18 is arranged on the outer side of the shielding protection body 17, vertically irradiates the surface of the potassium salt material, has the measuring range of 60-180mm, the resolution ratio of 30 mu m and the response time of 100ms, is used for measuring the distance of the surface of the potassium salt material relative to the X fluorescence measuring mechanism in real time, feeds back the change of the material quantity and is used for compensating and correcting the distance of the X fluorescence intensity; the on-line moisture meter 19 is arranged outside the shielding protection body 17, is on the same central line with the measuring window body 10, and vertically irradiates the surface of the sylvite material, and is a near-infrared on-line moisture meter with the measuring precision of 0.2%.
The high-voltage control signal of the X-ray tube, the control signal of the X-ray fluorescence detector, the output signal of the digital multichannel spectrometer, the signal of the ranging sensor, the signal of the online moisture meter and the signal of the stepping motor of the calibrating device all adopt TCP/IP communication protocols.
The material shaping mechanism comprises a high-level scraper, a low-level scraper and a movable scraper, wherein the high-level scraper, the low-level scraper and the movable scraper are sequentially arranged along the potassium salt conveying direction, the low-level scraper is similar in structure, is arranged at the position of 100cm from the rear end of the high-level scraper, and is lower than the high-level scraper in installation height.
As shown in fig. 4 and 5, the specific installation structure of the lower blade 2 in the embodiment of the present invention is schematically shown, the lower blade 2 is a stainless steel welding member with a triangular structure having an opening at the bottom, and is installed on a floor-lifting bracket assembly 25 by a threaded lifting boom 26 and a steel rope 27 with a diameter of 8mm, and the floor-lifting bracket assembly 25 is floor-fixed across the belt conveyor 30.
As shown in fig. 6, 7 and 8, the specific installation structure of the movable scraper 3 in the embodiment of the present invention is shown schematically, the movable scraper 3 is a stainless steel welding member with a rectangular plate-shaped structure, and is provided with a counterweight plate 28, the top end of the movable scraper 3 is connected to a spiral lifting boom 26 through a long pin 29, is located at 50cm behind the lower scraper 2, and is installed on the same floor-lifting bracket assembly 25 as the lower scraper 2, and the floor-lifting bracket assembly 25 is fixed across the belt conveyor 30.
The distance compensation correction method of the X fluorescence intensity is shown in the following formula (1) according to the exponential decay law of the monoenergetic X-ray in the material penetration process, and the correction method is shown in the formula (2):
in the middle ofThe X fluorescence intensity after the compensation and correction for the distance influence; />The distance D obtained by direct measurement of the X-ray fluorescence detector x X fluorescence intensity at time; d (D) x D, for the distance between the surface of the sylvite material measured by the distance measuring sensor and the bottom of the distance measuring sensor 0 The distance from the bottom of the ranging sensor to the bottom plate of the X fluorescent element on-line measuring mechanism is a fixed value related to the installation height of the ranging sensor; a. t and b are coefficients in an exponential function, and a, t and b can be measured by analog calculation or experiment for potassium salts with different potassium chloride contents.
The moisture influence correction of the X fluorescence intensity is that a Logistic regression analysis model is established through statistics of moisture values and probability distribution rules of the X fluorescence intensity, the correction method is shown as the following formula (3), and the correction method is shown as the formula (4):
I＝A2+(A1-A2)/(1+(M x /x0) p ) (3)
wherein M is 0 For the water content reference value, M x In order to measure the value of the moisture,for a moisture value of M 0 Intensity of time X fluorescence, < >>For a moisture value of M x The X fluorescence intensity at the time, A1, A2, X0 and p are equation coefficients, which can be obtained by experimental measurement.
In this embodiment of the present invention, the specific steps of the distance compensation correction method for the X fluorescence intensity are as follows:
(8) a, measuring a and t values under different potassium chloride contents through analog calculation or experiments, and establishing a data calculation model;
(9) the X fluorescence intensity measured by the X fluorescence measuring mechanism isThe distance value measured by the distance measuring sensor is D x ；
A comparison of the measured value D of the distance x And default value D 0 Size, if D x And D 0 Equal, no correction is performed; if D x And D 0 Equal, at this time, the potassium chloride content is assumed to be Ca;
calculating from (1) the corresponding a and t values at this content using the assumed Ca-x of the potassium chloride content;
calculating by the formula (2) to obtain X fluorescence intensity value after distance compensation correction>
Will->Carrying out an original content calculation model of the X fluorescence measurement mechanism to obtain corrected potassium chloride content Ca;
if |Ca| -Ca|is less than or equal to the limit error value, the correction process is terminated, the potassium chloride content result of potassium salt is Ca, otherwise, the operation is continued after returning to the step (3).
As shown in FIG. 9, in the embodiment of the invention, the relationship between the X fluorescence intensity value I and the distance value D is measured by using an X fluorescence element on-line measuring mechanism and a distance measuring sensor, and then the function relationship between the X fluorescence intensity and the distance is obtained by fitting according to a single exponential decay law (Expdec 1) as shown in the following formula (5), wherein the fitting degree correlation coefficient R 2 ＝0.99788，The measured value of X fluorescence intensity at the corresponding distance is well matched with the exponential decay law, and finally D with constant distance can be calculated according to the formula (5) 0 The X fluorescence intensity at this point is shown in the formula (6) in the distance compensation correction algorithm of X fluorescence intensity in this embodiment of the present invention.
In the middle ofFor the characteristic X fluorescence intensity of the potassium element after distance compensation correction, < >>The distance D obtained by direct measurement of the X-ray fluorescence detector x Characteristic X fluorescence intensity, D of Potassium element at that time x D, for the distance between the surface of the sylvite material measured by the distance measuring sensor and the bottom of the distance measuring instrument 0 The distance from the bottom of the distance measuring sensor to the bottom plate of the X-ray fluorescence measuring mechanism is a fixed value which is related to the mounting height of the distance measuring sensor, D in this embodiment of the invention 0 The value was 60mm.
As shown in FIG. 10, in the embodiment of the present invention, a relationship of the influence of moisture change (air drying time) on X fluorescence intensity is obtained, and a logistic regression equation is used for fitting to obtain a functional relationship as shown in formula (7), wherein the fitting degree correlation coefficient R 2 = 0.9829, the X fluorescence intensity at the moisture reference value can be calculated according to the formula (7), and moisture influence correction of the X fluorescence intensity can be achieved.
I＝269250.338+29889.641/(1+(M/78.16536)^3.9694) (7)
Wherein I is the characteristic X fluorescence intensity of potassium element, and M is the moisture value measured by an online moisture meter.
In the embodiment of the invention, the quantitative potassium chloride working curve obtained by combining the distance compensation correction of the X fluorescence intensity and the moisture influence correction is shown in fig. 11, the fitting relation of the working curve is shown in formula (8), the fitting relation is 0.9985, the measuring range of the potassium chloride content is more than 70%, and the on-line measuring requirements of industrial sites on high, medium and low grade potassium salts are met.
I＝8.75389*C-250.26416 (8)
Wherein I is element characteristic X fluorescence intensity unit is cps, C is potassium chloride content value in potassium salt, unit wt%.
It will be understood that modifications and variations will be apparent to those skilled in the art from the foregoing description, and it is intended that all such modifications and variations be included within the scope of the following claims.
Claims (12)
1. The potassium salt component online detection device is characterized by comprising a material shaping mechanism for flattening the surface of potassium salt; x fluorescent element on-line measuring mechanism with distance measuring sensor for measuring potassium salt element component; an on-line moisture measuring mechanism for potassium salt moisture measurement; and an industrial control computer system for system control and data analysis; the material shaping mechanism, the X fluorescent element online measuring mechanism and the online moisture measuring mechanism are sequentially arranged above the potassium salt conveying belt conveyor from front to back and are mutually matched, the material shaping mechanism acts on materials to enable the surfaces of the potassium salt to be smooth and flat, so that the accuracy of measuring results of the rear X fluorescent element online measuring mechanism and the online moisture measuring mechanism is facilitated, the measuring results of moisture values are used for accurately compensating the influence of moisture changes on the measuring results of the X fluorescent element online measuring mechanism, the ranging sensor is used for monitoring material quantity fluctuation, measuring the distance of the surface of the potassium salt material relative to the X fluorescent measuring mechanism in real time and compensating and correcting the distance of X fluorescent intensity, and the organic combination of the three mechanisms ensures the high accuracy of X fluorescent measurement;
the distance compensation correction method of the X fluorescence intensity is shown in the following formula (1) according to the exponential decay law of the monoenergetic X-ray in the material penetration process, and the correction method is shown in the formula (2):
in the middle ofThe X fluorescence intensity after the compensation and correction for the distance influence; />The distance D obtained by direct measurement of the X-ray fluorescence detector x X fluorescence intensity at time; d (D) x D, for the distance between the surface of the sylvite material measured by the distance measuring sensor and the bottom of the distance measuring sensor 0 The distance from the bottom of the ranging sensor to the bottom plate of the X fluorescent element on-line measuring mechanism is a fixed value related to the installation height of the ranging sensor; a. t and b are coefficients in an exponential function, and a, t and b are measured through analog calculation or experiments for potassium salts with different potassium chloride contents;
the moisture influence correction of the X fluorescence intensity is that a Logistic regression analysis model is established through statistics of moisture values and probability distribution rules of the X fluorescence intensity, the correction method is shown in the following formula (3), and the correction method is shown in the formula (4):
I＝A2+(A1-A2)/(1+(M x /x0) p )(3)
wherein M is 0 For the water content reference value, M x In order to measure the value of the moisture,for a moisture value of M 0 Intensity of time X fluorescence, < >>For a moisture value of M x The X fluorescence intensity at the time, A1, A2, X0 and p are equation coefficients, and are obtained through experimental measurement.
2. The potassium salt component online detection device according to claim 1, wherein the material shaping mechanism comprises a high-level scraper (1), a low-level scraper (2) and a movable scraper (3) for flattening the potassium salt surface; the high-level scraping plate (1), the low-level scraping plate (2) and the movable scraping plate (3) are sequentially arranged above the conveyor along the conveying direction of the potassium salt, the front end of the high-level scraping plate (1) is of a triangular structure, the bottom of the high-level scraping plate is open, the material layer with higher potassium salt is subjected to peak clipping, the low-level scraping plate (2) is of a triangular structure, the bottom of the high-level scraping plate is open, the mounting height of the low-level scraping plate is lower than that of the high-level scraping plate (1), the rear end of the high-level scraping plate (1) is located at a position with a distance of more than 50cm, the movable scraping plate (3) is of a rectangular plate structure, and the top connecting bearing is fixed at the rear end of the low-level scraping plate (2) and provided with a counterweight and is used for flattening treatment of the potassium salt material.
3. The potassium salt component online detection device according to claim 1, wherein the X-ray fluorescence element online measurement mechanism comprises an X-ray tube (4), an X-ray collimator (5), a high-voltage power supply (6), an X-ray fluorescence detector (7), a digital multichannel spectrometer (8), a combined displacement adjustment table (9), a measurement window (10), a purge air pump (11), a CCD digital camera (12), an X-ray fluorescence calibration device (13), a constant temperature control device (14), a condensed water collection device (15), an Ethernet communication module (16), a shielding protection body (17) and a ranging sensor (18); in the X-ray fluorescence element on-line measuring mechanism, an X-ray tube (4), an X-ray collimator (5), a high-voltage power supply (6), an X-fluorescence detector (7), a digital multichannel spectrometer (8), a combined displacement adjusting table (9), a measuring window (10), a purge air pump (11), a CCD digital camera (12), an X-fluorescence calibrating device (13), a constant-temperature control device (14), a condensed water collecting device (15) and an Ethernet communication module (16) are all arranged in a shielding protection body (17); the X-ray collimator (5) is connected with the X-ray tube (4), and the included angle between the center line of the X-ray collimator (5) and the surface of the sylvite is not less than 50 degrees.
4. The potassium salt component online detection device according to claim 3, wherein the combined displacement adjustment table (9) is formed by combining a X, Y, Z axis translation table and an alpha axis angular displacement table, is connected with the X fluorescence detector (7), and is used for adjusting the included angle between the central line of the probe of the X fluorescence detector (7) and the surface of the potassium salt to be not less than 55 degrees.
5. The potassium salt component online detection device according to claim 3, wherein the probe center of the X-ray fluorescence detector (7) and the outlet center of the X-ray collimator (5) are positioned on the same horizontal plane and are 5mm away from the upper surface of the measurement window (10), the central axes of the X-ray collimator (5) and the X-ray fluorescence detector (7) are intersected at the central axis of the measurement window (10), the intersection point is positioned below the measurement window (10), and the included angle between the central line of the X-ray collimator (5) and the potassium salt surface is 55 °; the X fluorescence detector (7) is arranged on the multidimensional XYZ alpha combination displacement adjustment table (9), and the included angle between the central line of the X fluorescence detector (7) and the surface of the sylvite is 55 degrees.
6. The potassium salt component online detection device according to claim 3, wherein the measurement window (10) is positioned at the center of a bottom plate of the shielding protection body (17), and comprises a polyether-ether-ketone rim structure with a purging air duct and a polyimide film, the purging air duct is connected with a purging air pump (11), and the surface of the film is purged and cleaned.
7. The potassium salt component online detection device according to claim 3, wherein the X-ray fluorescence calibration device (13) comprises a standard 304 stainless steel sheet and a translation table driven by a stepping motor, when the stainless steel sheet is driven in a translation way and shields the upper surface of the measurement window (10), source-level X-rays emitted by the X-ray tube (4) directly irradiate on the stainless steel sheet, and the X-ray fluorescence calibration device (13) can be used for realizing the periodic calibration of an X-ray fluorescence element online measurement mechanism quantitative calculation model and the detection of functional faults.
8. The potassium salt component online detection device according to claim 3, wherein the constant temperature control device (14) is positioned at the upper part in the shielding protection body (17) and consists of a EKW-1000 type remote networking temperature controller, a temperature sensor, a 200W semiconductor refrigerator and a semiconductor heater, and is used for monitoring the temperature in the equipment and controlling the constant temperature, wherein the semiconductor refrigerator is in butt joint with the condensed water collecting device (15), and the temperature range in the X fluorescent element online measurement mechanism is set to be 25-35 ℃.
9. The potassium salt composition online detection device according to claim 3, wherein a distance measuring sensor (18) is installed outside the shielding protection body (17), vertically irradiates the surface of the potassium salt material, is used for measuring the distance of the surface of the potassium salt material relative to the X fluorescence measuring mechanism in real time, feeds back the change of the material quantity, and is used for distance compensation correction of the X fluorescence intensity; the on-line moisture meter (19) is arranged outside the shielding protection body (17) and is arranged on a central line with the measuring window body (10) to vertically irradiate the surface of the sylvite material.
10. The device for on-line detection of potassium salt according to claim 3, wherein helium gas injection means is added to the space between the probe of the X-ray fluorescence detector and the measurement window and to the space between the potassium salt and the measurement window.
11. The potassium salt component online detection device according to claim 3, wherein the front end of the X-ray collimator, the probe of the X-ray fluorescence detector and the measuring window are sealed in a chamber of an acrylic structure, sealing rings are arranged at the joints, and a vacuum cylinder and a vacuum pump are sequentially connected in the chamber to vacuumize the chamber.
12. The device for on-line detection of potassium salt according to claim 1, wherein a roller structure is added to the material shaping structure to roll the surface of the potassium salt.
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| CN114951023B (en) * | 2022-05-24 | 2024-07-12 | 广东冠电科技股份有限公司 | Device for analyzing metal surface components by utilizing X rays |
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