CN210572079U - Strong-basicity anion exchange resin Mass Transfer Coefficient (MTC) measuring device - Google Patents
Strong-basicity anion exchange resin Mass Transfer Coefficient (MTC) measuring device Download PDFInfo
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- CN210572079U CN210572079U CN201920933765.9U CN201920933765U CN210572079U CN 210572079 U CN210572079 U CN 210572079U CN 201920933765 U CN201920933765 U CN 201920933765U CN 210572079 U CN210572079 U CN 210572079U
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Abstract
The utility model relates to a strong basic anion exchange resin Mass Transfer Coefficient (MTC) survey device belongs to steam power system chemistry water treatment technical field. The main circulation loop of the device comprises a constant temperature water tank, a circulating pump, an MB fine processing column, a booster pump, a static pipeline mixer, a float flowmeter, a test column, an RH exchange column, an online conductivity meter, a corresponding pipeline and a valve; a heat-insulating interlayer is arranged outside the test column, and backflow water of the circulating pump returns to the constant-temperature water tank through the test column heat-insulating interlayer to keep the test column at a constant temperature; and the main circulation loop is also connected with an injection branch, and test medium sulfate radicals enter the main circulation loop through the injection branch. Utilize the utility model discloses a survey device can survey out anion exchange resin's mass transfer coefficient fast, accurately, can provide the basis for anion exchange resin dynamic performance aassessment, ion exchange resin reactor's design and operation.
Description
Technical Field
The utility model relates to a steam power system chemistry water treatment technical field especially relates to a steam power system condensate water fine treatment such as thermal power factory, nuclear power plant, large-scale naval vessel is with strong alkaline anion exchange resin dynamics performance evaluation index-sulfate radical medium Mass Transfer Coefficient (MTC) survey device.
Background
The mixed ion exchange resin reactor for the condensate polishing of the steam power system is a high-speed mixed bed. Taking a power plant as an example, the height of a typical mixed bed for condensate polishing is 0.9m-1.2m, and the running flow speed is 100m/h-120 m/h. Kinetic leakage occurs because of the short contact time of the condensate with the resin bed, some ions may not be able to exchange thoroughly (HUSSEY, D F, PANDEY, A K, FOUTH, G L. Amass transfer coefficient for radial flow and exchange [ J ]. Industrial & Engineering Chemistry Research,2012,51(3): 1429-1434.). Even with new resins or resins that have just been regenerated, kinetic leakage can occur due to differences in resin properties and changes therein. If the dynamic performance of the ion exchange resin is not good, the problems of poor quality of effluent of the high-speed mixed bed, short operation period, frequent regeneration, long cleaning period and the like are caused, so that the operation safety and the economical efficiency of the generator set are influenced. Anion exchange resins are of interest for their performance in the treatment of concentrated hydroxide anion, condensate and/or condensate kinetics, since anion exchange resins have much less heat, oxidation and contamination resistance than cation exchange resins (SIMISTER C, CARON F, GEDYE R. determination of the thermal degradation rate of polystyrene-based catalysts in exchange resins in ultra-pure water and service temperature [ J ]. Journal of radical and nuclear chemistry,2004,261(3): 523-531; UASHNG C, WANG J, LI H, et al. effect of the chemical structure of ion exchange resin in the condensate of the condensate and/or reaction [ J ]. Journal of viscosity & surface, 437-163-169).
Mass Transfer Coefficient (MTC) is a key index for characterizing the dynamic performance of ion exchange resins. MTC is a sensitive parameter that characterizes the average rate of migration of the ions to be exchanged from the host solution to the exchange sites. When the kinetic properties of the anionic resin deteriorate, MTC decreases to a large extent, while other indices of the resin such as exchange capacity, water content, etc. do not change much (HUSSEY, D F, PANDEY, AK, FOTCH, G L.A mass transfer coeffefficientfor radial flow adsorption and ion exchange [ J ]. Industrial & Engineering Chemistry Research,2012,51(3): 1429-1434.). The change in MTC also characterizes the extent of resin contamination, since contaminated resins can develop more severe kinetic leakage (HASAN M, RAHMAN M, KABIRA, et al. Mass-transfer synergistic as an indicator of resin performance: phenomena of film-forming and storage time on condensation polymerization-exchange resins [ J ]. Industrial & Engineering Chemistry Research,2018,57(31): 10601-10608.).
Sulfate radicals are often selected as test media for the determination of the strongly basic anion exchange resin MTC for condensate polishing. When the anion resin is polluted by organic matters, the organic matters occupy the liquid film on the surface of the resin and the internal mass transfer channels or consume the exchange capacity of the resin, and further influence the exchange reaction between the ions to be exchanged and the exchangeable ions on the active groups of the resin. The radius of sulfate hydrate ions is larger than that of other common anions such as chloride ions, and the mass transfer is more seriously influenced by organic pollutants. In addition, sulfate carries two negative charges and the exchange requires two exactly adjacent exchange sites (LEE, G.C., FOUCH, G.L., ARUNACHALAM, A.an evaluation of mass-transfer coefficients for new and use-exchange resins, 1997,35(1-2), 55-73.). Therefore, the decrease of the ability of anion exchange reaction with sulfate of anion resin with poor kinetic performance is more obvious. Therefore, the sulfate medium Mass Transfer Coefficient (MTC) is a characteristic index for characterizing the dynamic performance of the anion resin for condensate polishing.
Various negative resin MTC measuring devices have been internationally established, such as the United kingdom Central Power office CEGB (Harries, R.R., Anion Exchange dynamics in condensed purity concrete and Performance pressure in Fine ingredient Research Workshop, Richmond, VA, USA,1985.), the American Power Research EPRI (Field optimization of the EPRI Research tester: protocol Development and Initial Field Usage; EPRI Technical report No.1008084[ R ], Electric Power Research Institute: Pakis Alto, CA,2004.) and the American society for testing and materials ASTM (ASTM) for evaluating negative resin MTC devices, PA 20102, Condensate analysis of the national center of Electrical Research Workshop, Inc. [ 2019 ] and the American society for testing and materials Research Institute [ ASTM ] PA 02. However, two conductivity meters are selected as the measuring device constructed by the mechanisms. In fact, the determination of the concentration of the medium can be achieved by only a single conductivity meter. Meanwhile, the measuring devices do not calibrate the working curve of the actual ion concentration and hydrogen conductivity, and impurities, flow velocity and the like in the measuring devices can influence the measurement of the conductivity. In addition, temperature affects the ion exchange reaction in the test column, and the test column of the above-mentioned measuring apparatus is not designed with a heat-insulating member.
There are also reports on resin MTC assay devices in China. Van Sheng Ping et al established a shallow bed apparatus for determining total MTC in resin (Van Sheng Ping, Cao shuan, Hu Xin Rong, et al. shallow bed for measuring total mass transfer coefficient of resin 201520860458.4[ P].2016-04-27). When the device is used for determining the total MTC of the resin, the test needs to be carried out until the ion exchange reaction reaches the equilibrium. At this point, the test ion leak in the resin thin layer effluent comes from an equilibrium leak of the resin sample, not a kinetic leak. Kinetic leakage of anion resins with sufficient exchange capacity and unbalanced ion exchange reactions can also occur due to differences and variations in resin properties (LEE, G.C., FOUTCH, G.L., ARUNACHALAAM, A.an evaluation of mass-transfer coefficients for new and used ion-exchange resins [ J.].Reactive&Functional Polymers,1997,35(1-2), 55-73.). A female resin sulfate MTC measuring device (Wangchun, Fujie Qi, Chenying, etc.) is constructed by Wangchun, etc. a female resin dynamic performance index-SO4 2-The device and method for measuring a mass transfer coefficient of (1): 201110136295.1[ P ]].2013-05-08). The device has simple structure and low test cost. However, the device is not designed with a mixed ion exchange resin (MB) fine treatment column, so that the effluent can not be recycled, and the water consumption is high. The test solution of the device adopts an ammonia-containing sodium sulfate solution. Ammonia has peculiar smell, which brings inconvenience to the preparation of the test solution and the determination of the negative resin MTC. Meanwhile, the alkaline test solution can absorb CO in the air2And further introduces interference factors for the determination of MTC. In addition, the assayThe device also does not calibrate the working curve of the actual sulfate radical concentration and the hydrogen conductivity, and impurities, flow velocity and the like in the device can influence the determination of the conductivity.
At present, resin MTC measuring devices designed and built by various institutions at home and abroad have certain defects. Designing a device capable of rapidly and accurately measuring the strong-base anion exchange resin MTC is a key for evaluating the dynamic performance of the anion exchange resin and further guiding the production practice.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a strong basic anion exchange resin Mass Transfer Coefficient (MTC) survey device to above-mentioned technical problem, adopt the device, can survey strong basic anion exchange resin's mass transfer coefficient fast, accurately.
The utility model provides a technical scheme is:
a strong basic anion exchange resin Mass Transfer Coefficient (MTC) measuring device is characterized in that a main circulation loop of the device comprises a constant temperature water tank, a circulation pump, an MB fine processing column, a booster pump, a static pipeline mixer, a float flowmeter, a test column, an RH exchange column, an online conductivity meter, a corresponding pipeline and a valve; a heat-insulating interlayer is arranged outside the test column, and backflow water of the circulating pump returns to the constant-temperature water tank through the test column heat-insulating interlayer to keep the test column at a constant temperature; and the main circulation loop is also connected with an injection branch, and test medium sulfate radicals enter the main circulation loop through the injection branch.
The RH exchange column is arranged in front of the online conductivity meter, the effluent liquid of the test column returns to the constant temperature water tank through the RH exchange column and the online conductivity meter, and the hydrogen conductivity of the effluent liquid of the test column is measured by using a single online conductivity meter.
Injection branch road is including injection pump, syringe, luer joint ball valve, syringe needle tube, rubber buffer, the three-way valve for the injection that connects gradually, the test medium sulfate radical is equipped with in the syringe, the test medium sulfate radical flows through luer joint ball valve, syringe needle tube, rubber buffer, the three-way valve for the injection in proper order through the injection pump horizontal migration, merges into the main circulation circuit, passes through static pipeline mixer misce bene with the pure water in the main circulation circuit.
Preferably, the apparatus is selected from the following instruments and materials:
the constant temperature water tank is made of stainless steel, the temperature control precision is +/-0.1 ℃, and the volume is 30L;
circulating pump PcThe flow range (20-40) L/min and the lift (12-14) m;
the MB fine processing column is made of organic glass, and has an inner diameter of 50mm and a length of 600 mm;
syringe pump PiThe flow range (0-2.3) mL/min is matched with 30mL multiplied by 2 of an injector;
booster pump PbThe flow range (42-52) L/min and the lift (4-6) m;
a static pipeline mixer with an outer diameter of 12mm and a length of 250 mm;
a tubular float flowmeter, wherein the metering range is (0.5-2.0) L/min;
the test column is a sandwich glass column, the bottom of the inner tube is filled with a G1 sand core, and the outer diameter is 40mm, the inner diameter is 25mm and the length is 600 mm;
the RH exchange column is made of organic glass, the inner diameter is 50mm, and the length is 600 mm;
the electrode constant K of the online conductivity meter is 0.01, the resolution is 0.001 mu S/cm, and the temperature measurement resolution is 0.1 ℃;
the steps for calibrating the hydrogen conductivity of the trace sulfate solution are as follows:
dissolving the baked sodium sulfate with pure water to prepare sulfate radical solution of 1mg/L, 2mg/L, 5mg/L, 10mg/L, 20mg/L, 40mg/L, 60mg/L, 80mg/L and 100 mg/L;
calibrating the flow rate of the injection pump to 0.5 mL/min;
adjusting the flow of the main circulation loop to be 1L/min, circularly purifying and automatically keeping the temperature of the measuring system constant until the conductivity is stable and the outlet water temperature of the RH exchange column is (25.0 +/-0.5) DEG C;
pure water was injected at a rate of 0.5mL/min to measure the blank hydrogen conductivity κ0；
1mg/L sulfate solution was injected into the main circulation loop at a rate of 0.5mL/min to measure the hydrogen conductivity κ1；
The hydrogen conductivity was measured by changing the injection solutions with different sulfate radical concentrations from low to high.
The utility model discloses following beneficial effect has:
the utility model discloses not filling resin, directly on former survey device at the test column, actually measured the hydrogen conductivity of different concentration sulfate radical solutions, demarcated the relation of sulfate radical concentration and hydrogen conductivity, offset the influence of impurity, velocity of flow etc. in the device to the conductivity survey; the hydrogen conductivity of the effluent liquid of the test column can be measured by using a single conductivity meter, and the composition is simpler; a test column heat-insulating part is designed, the temperature can be controlled to be (25.0 +/-0.5) DEG C, and the influence of the temperature on the ion exchange reaction and the conductivity measurement is reduced; the determination of one resin sample MTC can be completed within 1h, and the precision of the test result is higher than that of the existing report;
the utility model discloses can survey out strong alkaline anion exchange resin's sulfate radical medium mass transfer coefficient fast, accurately, can provide the basis for resin dynamic performance aassessment, resin reactor's design and operation.
Drawings
FIG. 1 is a schematic structural diagram of a Mass Transfer Coefficient (MTC) measuring device for strongly basic anion exchange resin according to the present invention;
fig. 2 is a schematic view of the structure of the syringe pump assembly of the present invention.
The figures in the drawings are labeled as:
1. a constant temperature water tank; 2. a circulation pump; MB fine processing column; 4. an injection branch; 41. an injection pump; 42. an injector; 43. a luer fitting ball valve; 44. an injector needle tube; 45. a rubber plug; 46. a tee for injection; 5. a booster pump; 6. a static pipeline mixer; 7. a float flow meter; 8. a test column; RH exchange column; 10. an on-line conductivity meter; 11. a drain valve at the bottom of the constant temperature water tank; 12. a water outlet valve of the constant-temperature water tank; 13. a water inlet valve of the test column heat-insulating jacket; a MB exchange column water inlet primary valve; 15, feeding a water secondary valve into the MB exchange column; MB exchange column exhaust valve; an MB exchange column water outlet valve; 18. a test column water inlet primary valve; 19. a test column water inlet secondary valve; 20. a test column exhaust valve; 21. a test column outlet valve; 22, a primary water inlet valve of the RH exchange column; 23, a RH exchange column water inlet secondary valve; an RH exchange column exhaust valve; and 25, an outlet valve of the RH exchange column.
Detailed Description
In order to facilitate understanding of the present invention, the present invention will be described in further detail with reference to the following embodiments.
Example 1
Assembling a measuring device:
as shown in fig. 1, a constant temperature water tank 1, a circulating pump 2, a MB fine treatment column 3 filled with water, an injection branch 4, a booster pump 5, a static pipeline mixer 6, a float flowmeter 7, a test column 8 filled with water, an RH exchange column 9 filled with water, and an online conductivity meter 10 are sequentially connected by pipelines to form a main circulation loop. The structure of the injection pump branch 4 is shown in fig. 2, and the test medium sulfate enters the main circulation loop through an injection pump 41, an injector 42, a luer joint ball valve 43, an injector needle tube 44, a rubber plug 45 and an injection three-way valve 46; in the connection process, the RH exchange column 9 and the float flowmeter 7 should be kept vertically fixed, and the outlet pipe orifice of the electrode pool of the online conductivity meter 10 is preferably higher than the outlet of the RH exchange column exhaust valve 24.
The bottom of the constant-temperature water tank 1 is provided with a bottom discharge valve 11 of the constant-temperature water tank, a water outlet valve 12 of the constant-temperature water tank is arranged between the constant-temperature water tank 1 and the circulating pump 2, an MB exchange column water inlet primary valve 14 and an MB exchange column water inlet secondary valve 15 are arranged between the circulating pump 2 and the MB fine treatment column 3, and in addition, pipelines between the MB exchange column water inlet primary valve 14 and the MB exchange column water inlet secondary valve 15 are also connected with an MB exchange column exhaust valve 16. An MB exchange column water outlet valve 17 is arranged between the MB fine processing column 3 and a booster pump 55 of the booster pump 5, a test column water inlet primary valve 18 is arranged between the static pipeline mixer 6 and the float flowmeter 7, a test column water inlet secondary valve 19 is arranged between the float flowmeter 7 and the test column 8, and a test column exhaust valve 20 is connected on a pipeline between the float flowmeter 7 and the test column water inlet secondary valve 19. A test column water outlet valve 21, an RH exchange column water inlet primary valve 22 and an RH exchange column water inlet secondary valve 23 are sequentially connected between the test column 8 and the RH exchange column 9, and a RH exchange column exhaust valve 24 is also connected on a pipeline between the RH exchange column water inlet primary valve 18 and the RH exchange column water inlet secondary valve 23. An RH exchange column water outlet valve 25 is connected between the RH exchange column 9 and the on-line conductivity meter 10.
Checking the sealing condition of each connecting part of the measuring device to eliminate water leakage;
backwashing ROH reference resin and RH reference resin according to GB/T5476, mixing the negative resin and the positive resin according to the volume ratio of 2:1, filling an MB fine processing column 3, wherein the bed height is not less than 350 mm;
filling the backwashed RH reference resin into an RH exchange column 9, wherein the height of a bed layer is not less than 300 mm;
the measuring device is cleaned until the conductivity is stable.
In-situ calibration of the relationship between sulfate concentration and hydrogen conductivity:
dissolving the baked sodium sulfate with pure water to prepare sulfate radical solution of 1mg/L, 2mg/L, 5mg/L, 10mg/L, 20mg/L, 40mg/L, 60mg/L, 80mg/L and 100 mg/L;
calibrating the flow rate of the injection pump 41 to 0.5 mL/min;
adjusting the flow of the main circulation loop to be 1L/min, circularly purifying and automatically keeping the temperature of the measuring system constant until the conductivity is stable and the temperature of the outlet water of the RH exchange column 9 is (25.0 +/-0.5) DEG C;
pure water was injected at a rate of 0.5mL/min to measure the blank hydrogen conductivity κ0；
1mg/L sulfate solution was injected into the main circulation loop at a rate of 0.5mL/min to measure the hydrogen conductivity κ1；
The hydrogen conductivity was measured by changing the injection solutions with different sulfate radical concentrations from low to high.
When the ratio is 0 ≦ (κ)1-κ0) When the concentration is less than or equal to 0.070 mu S/cm, [ SO ]4 2-]＝139.54×(κ1-κ0)+0.27(R＝0.996)；
When 0.070. mu.S/cm < (. kappa.)1-κ0) When the concentration is less than or equal to 0.435 mu S/cm, [ SO ]4 2-]＝111.31×(κ1-κ0)+1.60(R＝0.998)。
Measuring the mass transfer coefficient of a sulfate medium of a negative resin sample:
calibrating the flow rate of the injection pump 41 to 0.5 mL/min;
backwashing 200mL of OH type resin sample to be detected according to GB/T5476;
determining the weighted harmonic average particle size of the resin to be measured by adopting a laser diffraction scattering method;
uniformly mixing 75mL of negative resin sample and 150mL of RH reference resin, and filling a test column 8;
adjusting the flow of the main circulation loop to be 1L/min, circularly purifying and automatically keeping the temperature of the measuring system constant until the conductivity is stable and the temperature of the outlet water of the RH exchange column 9 is (25.0 +/-0.5) DEG C;
pure water was injected at a rate of 0.5mL/min to measure the blank hydrogen conductivity κ0；
0.9g/L sodium sulfate solution was injected into the main circulation loop at a rate of 0.5mL/min, and the hydrogen conductivity κ of the effluent of the test column 8 was measured1；
Measuring and recording the height H of the resin bed layer of the test column 8;
according to the calibrated relation, the concentration of sulfate radical in the effluent liquid of the test column 8 is calculated, and the mass transfer coefficient of the sulfate radical medium of the strong-base anion exchange resin is calculated through the following formula.
In the formula:
dp-equivalent diameter of resin, mm;
f-flow, m3/s；
Epsilon-porosity, dimensionless;
a-cross sectional area of test column 8, m2；
H-height of resin bed layer, mm;
(FR) -proportion of anionic resin in the mixed bed, dimensionless;
Four typical strongly basic hydroxide anion exchange resins were selected, 3 samples of each resin sample were taken, and the measurement was repeated 4 times for each sample, and the measurement results and precision were shown in table 1.
TABLE 1 measurement of mass transfer coefficient of sulfate medium and precision
Through the method steps, the utility model discloses can survey out strong alkaline anion exchange resin's sulfate radical medium mass transfer coefficient fast, accurately, can provide the basis for resin dynamic performance aassessment, resin reactor's design and operation.
The above description is only an example of the present invention, and the common general knowledge of the operation steps and features of the schemes is not described herein. It should be noted that, for those skilled in the art, variations and modifications can be made without departing from the spirit of the present invention, and these should be considered as the scope of the present invention. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (3)
1. A strong basic anion exchange resin Mass Transfer Coefficient (MTC) measuring device is characterized in that a main circulation loop of the device comprises a constant temperature water tank, a circulation pump, an MB fine processing column, a booster pump, a static pipeline mixer, a float flowmeter, a test column, an RH exchange column, an online conductivity meter, a corresponding pipeline and a valve; a heat-insulating interlayer is arranged outside the test column, and backflow water of the circulating pump returns to the constant-temperature water tank through the heat-insulating interlayer of the test column and is used for keeping the test column at a constant temperature; and the main circulation loop is also connected with an injection branch, and test medium sulfate radicals enter the main circulation loop through the injection branch.
2. The apparatus of claim 1, wherein the RH exchange column is installed before the on-line conductivity meter, the effluent of the test column is returned to the constant temperature water tank through the RH exchange column and the on-line conductivity meter, and the hydrogen conductivity of the effluent of the test column is measured by using a single on-line conductivity meter.
3. The device of claim 1, wherein the injection branch comprises an injection pump, an injector, a luer joint ball valve, an injector needle tube, a rubber plug and a three-way valve for injection which are connected in sequence, test medium sulfate radicals are filled in the injector, and the test medium sulfate radicals flow through the luer joint ball valve, the injector needle tube, the rubber plug and the three-way valve for injection in sequence by horizontal pushing of the injection pump, are merged into the main circulation loop and are uniformly mixed with pure water in the main circulation loop through a static pipeline mixer.
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| CN113960116A (en) * | 2021-10-21 | 2022-01-21 | 常州博瑞电力自动化设备有限公司 | Device and method for testing dynamic performance of ion exchange resin of converter valve cooling system |
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| CN113960116A (en) * | 2021-10-21 | 2022-01-21 | 常州博瑞电力自动化设备有限公司 | Device and method for testing dynamic performance of ion exchange resin of converter valve cooling system |
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