CN102305811B - Device and method for testing mass transfer coefficient of anion resin dynamic performance index SO4<2-> - Google Patents

Device and method for testing mass transfer coefficient of anion resin dynamic performance index SO4<2-> Download PDF

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CN102305811B
CN102305811B CN 201110136295 CN201110136295A CN102305811B CN 102305811 B CN102305811 B CN 102305811B CN 201110136295 CN201110136295 CN 201110136295 CN 201110136295 A CN201110136295 A CN 201110136295A CN 102305811 B CN102305811 B CN 102305811B
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resin
water
mixed bed
test
column
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CN102305811A (en
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王罗春
傅洁琦
陈英
丁桓如
付毅
王英俊
郑黎明
曾郁楠
周振
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Shanghai University of Electric Power
University of Shanghai for Science and Technology
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Shanghai University of Electric Power
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Abstract

The invention discloses a device and a method for testing the mass transfer coefficient of an anion resin dynamic performance index SO4<2-> in a condensation water refined processing high-speed mixed bed. The device comprises a high pressure pump, a rotameter, a hydrogen exchange column, a conductivity meter A, a conductivity meter B, a washing solution inlet box, a testing solution inlet box, a constant temperature water bath box, a resin testing column mixed bed with a clamping sleeve, and a switching valve. The method comprises the following seven steps of: preparing mixed bed cation resin; preparing mixed bed anion resin; mixing the mixed bed cation resin and the mixed bed anion resin and loading to a column; preparing hydrogen exchange column resin; washing a mixed bed testing column; testing the mass transfer coefficient of the SO4<2->; and calculating the mass transfer coefficient K of the anion resin dynamic performance index SO4<2-> according to a Harries model. A testing result in the testing method is slightly influenced by CO2 in air and the temperature of testing solution, and testing cost is relatively low.

Description

A kind of negative resin dynamic performance index-SO 42-Determinator and the method for coefficient of mass transfer
Technical field
The present invention relates to negative resin dynamic performance index-SO in a kind of condensation water refined processing high-speed mixing bed 4 2-Determinator and the method for coefficient of mass transfer.
Background technology
The steam that boiler of power plant produces, after being used for steam turbine (turbine) work done, the water that is condensed at condenser (condenser) through chilled water is condensate water.Condensate water is generally mixed with make-up water as the feedwater of boiler and is recycled.Due to bringing into of Steam Condenser Leak and some metallic corrosion products of boiler circuit e-quipment and pipe, in condensate water, metal oxide particle and various other ion concentrations often can not reach the requirement of boiler feed water, and need with carry out precision processing before make-up water mixes.
Precision processing device of condensation water mainly contains two kinds at present: (1) fore filter+high flow rate mixed bed+post-filter; (2) high flow rate mixed bed+post-filter.
Often can find the high flow rate mixed bed that is comprised of new resin in condensate fine is processed, water outlet conductivity is very low, and after operation a period of time, due to negative resin exchange kinetics hydraulic performance decline, water outlet conductivity rises, and its physicochemical property of resin is also unchanged.Therefore the anion exchange resins dynamic test is the indispensable means of precision processing device of condensation water fault detect.As far back as about 1980, and the people such as Ray Ball and Coates [International Water Conference(IWC), 1985-2003] begin the detection research of anion exchange resins dynamic performance, by detecting the SO of negative resin 4 2-Coefficient of mass transfer realized accurate judgement to the running status of negative resin, and successfully its achievement in research is applied to the supervision of negative resin performance change in condensation water refined processing high-speed mixing bed.On this basis, the U.S. has formulated relevant standard [Standard Practice for Evaluating the Kinetic Behavior of Ion Exchange Resins, Designation:D 6302 – 98 (Reapproved 2009)].The principal feature of Unite States Standard (USS) method is that whole proving installation is in complete closed state when test; Two the molten medicine-chests that are placed in before simultaneously the sodium sulphate in test fluid and ammonia are measured, during mensuration, passing ratio volume pump and mixing chamber mix again.This method of testing, during due to test, whole proving installation is in complete closed state, has eliminated CO in air fully 2On the impact of conductance measurement, accuracy of measurement is higher; Simultaneously, in test fluid, the mixing of sodium sulphate and ammonia is that passing ratio volume pump and mixing chamber are completed, and testing expense is more expensive.
The present invention, with reference to U.S. ASTM standard, designed, designed and processing obtain negative resin SO in a high flow rate mixed bed 4 2-The determinator of coefficient of mass transfer, and successfully use it for the dynamic supervision of negative resin performance change in condensation water refined processing high-speed mixing bed.
Summary of the invention
The present invention provides negative resin dynamic performance index S O in a kind of condensation water refined processing high-speed mixing bed in order to solve above-mentioned technical matters 4 2-Determinator and the assay method of coefficient of mass transfer.
Know-why of the present invention
The negative resin dynamic performance generally characterizes with the mass transfer coefficient of negative ion, and negative ion common in the boiler of power plant condensate water has SO 4 2-And Cl -Deng, wherein with SO 4 2-Ionic radius maximum, so negative resin absorb that the caused negative resin dynamic performance of the sulfate ion of identical molal quantity changes will be much larger than chlorion.Draw SO in water outlet by the variation that detects water conductivity 4 2-Concentration, recycling Harries model calculates the SO of negative resin 4 2-Mass transfer coefficient, last SO according to negative resin 4 2-The mass transfer coefficient size judges its running status.
The present invention is take ultrapure water as contrast liquid, with SO 4 2-Solution is test fluid, take the yin and yang resin mixed bed as test pole, connects a hydrogen exchange column after test pole.
When test fluid was flowed through test pole, the negative resin in the test pole mixed bed was with part SO in test fluid 4 2-To be replaced into OH -, the hydrogen exchange column is with the kation (Na in the test fluid water outlet +And NH 4 +) the unified H that is replaced into +, OH -With H +Water generation reaction changes the reading of the conductivity meter after the hydrogen exchange column and can reflect SO in the test fluid water outlet 4 2-Concentration change.
When in the test pole mixed bed, the negative resin dynamic performance changes, negative resin exchange SO when test fluid is passed through test pole 4 2-Amount also occur, so the reading of the conductivity meter after the hydrogen exchange column also changes.Changing value according to the conductivity meter reading after the hydrogen exchange column obtains SO in the test fluid water outlet 4 2-Concentration, then according to the Harries model ((ASTM International. D 6302-98(Reapproved 2009) [S]. United States:2009)) draw the SO of negative resin 4 2-Mass transfer coefficient.Last SO according to negative resin 4 2-The mass transfer coefficient size judges its running status.
Technical scheme of the present invention
Negative resin dynamic performance index S O in a kind of condensation water refined processing high-speed mixing bed 4 2-Coefficient of mass transfer measure device used, comprise high-pressure pump, spinner-type flowmeter, hydrogen exchange column and conductivity meter A and conductivity meter B, also comprise resin test pole mixed bed and the transfer valve of washing fluid inlet water tank, test fluid inlet water tank, constant water bath box, jacketed;
Described transfer valve can be replaced with other devices that can realize arbitrarily washing fluid test fluid handoff functionality;
The outlet of the outlet of described washing fluid inlet water tank and test fluid inlet water tank is connected with the inlet duct of high-pressure hydraulic pump by a transfer valve after joining by pipeline;
Be provided with stainless-steel tube in described constant water bath box, an end of stainless-steel tube is connected with the water under high pressure delivery side of pump, and the other end passes through resin test pole mixed bed, conductivity meter A, hydrogen exchange column and the conductivity meter B of spinner-type flowmeter, jacketed successively.
Negative resin dynamic performance index S O in a kind of condensation water refined processing high-speed mixing bed 4 2-Coefficient of mass transfer measure the process route of equipment therefor, namely install resin test pole mixed bed, conductivity meter A, hydrogen exchange column and the conductivity meter B of Stainless Steel Coil in transfer valve, constant water bath box of power that washing fluid and test fluid provide by high-pressure pump by different inlet water tanks with cover plate respectively, spinner-type flowmeter, jacketed, the final outflow.Wherein, in water bath and test pole chuck, water keeps circulation and constant temperature, its effect is that the temperature of regulating test fluid by test fluid coil pipe and test pole is 25 ± 0.5 ℃, guarantees that the test fluid temperature perseverance that conductivity meter shows is 25 ± 0.5 ℃, makes the not impact of tested person liquid temp of conductivity meter reading;
Hydrogen exchange column in above-mentioned device all transforms hydrogen ion with ammonium ion and sodion remaining in the resin test pole mixed bed water outlet of jacketed.
Negative resin dynamic performance index S O in a kind of condensation water refined processing high-speed mixing bed 4 2-The assay method of coefficient of mass transfer, comprise the steps:
(1), the preparation of mixed bed sun resin
Get 150mL sun resin, make it be immersed in tap water and leach immediately, get water logging sun resin, water logging sun resin is loaded in the glass actifier column, be that the 4%HCl of 13～14 times of water logging sun resin volume is with the approximately flow velocity regeneration of 10mL/min with volume again, the HCl regenerated liquid goes out water concentration when consistent with influent concentration, and regeneration ending is led to going out water power＜0.5 μ s/cm with the pure water rinsing of 50 ~ 60 ℃;
Described HCl regenerated liquid is 4% HCl aqueous solution;
Described positive resin is the new resin of Tao Shi 650C type;
Above-mentioned glass actifier column used is that volume is greater than the glass column of 150mL;
(2), the preparation of mixed bed negative resin
Get 75mL 28～30 order negative resins, it is immersed in tap water, and leaches immediately; Then clean water logging sun resin 2 times with 4%HCl, negative resin after hydrochloric acid cleaning is loaded in the glass actifier column, be that the 26-27 NaOH regenerated liquid doubly of the negative resin volume after pickling is with the approximately flow velocity regeneration of 10mL/min with volume again, the NaOH regenerated liquid goes out water concentration when consistent with influent concentration, regeneration ending is led to going out water power＜0.5 μ s/cm with the pure water rinsing of 50～60 ℃;
Described NaOH regenerated liquid is that concentration is the NaOH aqueous solution of 2mol/L;
Described negative resin is the new resin of CPA02 type of Tao Shi 550A type resin or Mitsubishi;
Above-mentioned glass actifier column used is that volume is greater than the glass column of 75mL;
(3), the mixed bed yin and yang resin mixes the dress post
Step (1) and the good yin, yang resin of (2) flushing are poured in a 500mL large beaker of cleaning, pour out the upper strata excessive moisture, mix, resin test pole mixed bed with deionized water cleaning tape chuck, after having cleaned, seal the lower end rising pipe, pour 10～20mL pure water into, the resin that mixes is poured in test pole mixed bed with chuck, avoid producing bubble and layering;
(4), the preparation of hydrogen exchanging column resin
1L sun resin is immersed in tap water and leaches immediately, get water logging sun resin, water logging sun resin is loaded in the glass actifier column, be that the 4%HCl regenerated liquid of 2 times of water logging sun resin volume is with the approximately flow velocity regeneration of 10mL/min with volume again, when the HCl regenerated liquid goes out water concentration when consistent with influent concentration, regeneration ending is led to going out water power＜0.5 μ s/cm with the pure water rinsing of 50-60 ℃;
Described HCl regenerated liquid is 4% HCl aqueous solution;
Described positive resin is the new resin of Tao Shi 650C type;
Above-mentioned glass actifier column used is that volume is greater than the glass column of 1L;
(5), the flushing of mixed bed test pole
Deionized water is got ultrapure water used by the ultrapure water resin;
After the test pole mixed bed of jacketed and hydrogen exchange column are respectively charged into corresponding resin, the regulating thermostatic bath temperature is 30 ℃ of left and right, guarantee that the conductivity meter temperature is 25 ± 0.5 ℃, the opening high pressure pump, with test pole and the hydrogen exchange column of ultrapure water as washing fluid flushed zone chuck, flushing speed is controlled at 1 ~ 1.2L/min, makes water outlet conductivity＜0.07 μ s/cm, and stablizes at least 10min;
If be shorter than 10min stabilization time, illustrate that the resin regeneration effect is bad or it is inhomogeneous to mix, need again to regenerate, to mix resin and fill post;
(6), SO 4 2-The test of coefficient of mass transfer
With the 0.0900g anhydrous Na 2SO 4Be dissolved in and make Na used in the 1L ultrapure water 2SO 4Solution;
With 27.3g NH 3Be dissolved in and make ammoniacal liquor used in the 1L pure water;
In situ preparation 25L ultrapure water adds the Na of gained immediately 2SO 4The ammoniacal liquor 50mL of solution 12.5mL and gained makes test fluid;
Test fluid is packed in test fluid immersion case, and control with the flow velocity of 1L/min resin test pole, conductivity meter A, hydrogen exchange column and the conductivity meter B through the stainless-steel tube in transfer valve, high-pressure pump, constant water bath box, spinner-type flowmeter, jacketed, measure and record the reading of conductivity meter B, remain unchanged in 1min to reading, test finishes, with the ultrapure water flushing line, to the conductivity meter reading be 0.07 μ s/cm;
(7), negative resin dynamic performance index-SO 4 2-The calculating of coefficient of mass transfer
According to Harries model (ASTM International. D 6302-98(Reapproved 2009) [S]. United States:2009), calculate SO 4 2-Coefficient of mass transfer
The Harries model is:
Figure 2011101362951100002DEST_PATH_IMAGE001
（2-1）
In formula, K:SO 4 2-Coefficient of mass transfer, m/s;
ε: bed voidage;
R: resinoid volume ratio,
F: the flow velocity of test fluid, m/s;
A: the test pole bed sectional area of jacketed, m 2
L: the test pole bed of jacketed is dark, i.e. resin height, m;
D: resin-like harmonic average diameter, m
P wherein iBe the percentage composition of the resin of a certain diameter section,
Figure 2011101362951100002DEST_PATH_IMAGE004
d 1, d 2Be mesh size, cm;
C: the test fluid sulfate radical goes out water concentration, μ g/L;
C=ΔDD/8.768×10 -3
The conductivity difference of Δ DD conductivity meter B when intaking take ultrapure water and test fluid as device respectively wherein;
C 0Be the test fluid sulfate concentration, μ g/L, concentration 300 μ g/L in test.
According to above-mentioned assay method, finally calculate the SO of gained negative resin 4 2-Coefficient of mass transfer, and associative list 1[International Water Conference(IWC), 1985-2003] draw negative resin state and condensed water precision processing system operation conditions in mixed bed;
Table 1 SO 4 2- The corresponding relation of coefficient of mass transfer, mixed bed negative resin state and condensed water precision processing system operation conditions
SO 4 2- Coefficient of mass transfer scope (* 10 -4 m/s） Resin state System operation situation
1.5 ～ 2.0 Satisfied Normal operation
1.0 ～ 1.5 Transition state The sulfate radical washing water quantity increases
0.5 ～ 1.0 Chronic fault Often defective in quality
< 0.5 Lost efficacy and upgraded The a large amount of leakage
Be in the coefficient of mass transfer corresponding to resin of " satisfaction " state〉1.5 * 10 -4M/s, its performance is worked as with new resin-phase; Coefficient of mass transfer corresponding to resin that is in " transition " state is 1.0 ~ 1.5 * 10 -4M/s, the resin that at this moment rinses after regenerating with ultrapure water is larger to the qualified required water yield of water outlet sulfate radical; Coefficient of mass transfer corresponding to resin that is in " chronic fault " state is 1.0 ~ 1.5 * 10 -4M/s although this moment, resin can use, make its water outlet reach required time of feedwater quality requirement and increases greatly of expense; Coefficient of mass transfer corresponding to resin that is in " lost efficacy and upgrade " state is＜0.5 * 10 -4M/s, this moment, resin can not use.
Generally in the precision processing device, the resin operating condition reaches " chronic fault " or " lost efficacy and upgrade " stage, and resin just must be changed.Resin can readjust amount of resin and add new resin from the top as in " transition " operating mode, can return to " satisfaction " operating mode.
Beneficial effect of the present invention
Proving installation of the present invention, when measuring, adopt manual method that the sodium sulphate in test fluid and ammonia are mixed, and then add the test fluid inlet water tank, inlet water tank is with cover plate, the water delivering orifice of inlet water tank is near the bottom of water tank, and test fluid is built cover plate after adding inlet water tank immediately, reduces CO in air as far as possible 2Impact on conductance measurement;
Simultaneously, proving installation of the present invention adopts water bath and test pole chuck to carry out the water-bath temperature adjustment to test fluid, make the water in water bath and test pole chuck keep circulation and constant temperature, the temperature of regulating test fluid by test fluid coil pipe and test pole is 25 ± 0.5 ℃, the test fluid temperature substantially constant that guarantees the conductivity meter demonstration is constant, makes the impact of conductivity meter reading tested person liquid temp very little.
In addition, negative resin SO in condensation water refined processing high-speed mixing bed of the present invention 4 2-The coefficient of mass transfer method of testing, can be in the situation that the resin physical property may not change, whether state easy, that in time judge resin good, guarantee operation condition in site and water quality situation, and testing cost is lower.
Description of drawings
Fig. 1, be negative resin dynamic performance index S O in a kind of condensation water refined processing high-speed mixing bed of the present invention 4 2-Coefficient of mass transfer measure device schematic diagram used, in figure 1 be with cover plate the washing fluid inlet water tank, 2 for the test fluid inlet water tank of cover plate, 3 for transfer valve, 4 for high-pressure pump, 5 for the stainless-steel tube in constant water bath box, 6 for constant water bath box, 7 for spinner-type flowmeter, 8 for the resin test pole of jacketed, 9 for conductivity meter A, 10 be that hydrogen exchange column and 11 is conductivity meter B.
Embodiment
Below by embodiment, the present invention is further set forth, but do not limit the present invention.
Negative resin dynamic performance index S O in a kind of condensation water refined processing high-speed mixing bed in the embodiment of the present invention 1 4 2-Coefficient of mass transfer measure in device used used:
High-pressure pump is DP100 type high-pressure diaphragm pump, voltage 24V, maximum current 1.1A, maximum flow 1.2L/min, top pressure 0.69Mpa;
The test pole mixed bed of jacketed is for being the stainless steel column with heating interlayer, and its column internal diameter is φ 25 * 580mm;
The hydrogen exchange column is stainless steel, and internal diameter is φ 50 * 500mm;
Conductivity meter A is the higher difficult to understand sharp imperial 3-Star portable 320C-06 type pure water conductivity instrument (electrode constant J=0.1) of sensitivity, and effect is to detect developing result;
Conductivity meter B is the higher thunder magnetic DDG-5205A type industry electrical conductivity instrument (electrode constant J=0.0993) of stability.
Constant water bath box is 501BS type thermostatic water-circulator bath pot, and its specification is: supply voltage AC220V ± 10%, and heating power 1000W controls RT-100 ℃ of temperature, temperature-controlled precision ± 0.5 ℃;
The connecting tube material is high pressure polyethylene;
The LZB-10 type glass rotameter that spinner-type flowmeter provides for revitalizing flow-meter plant, range is 0 ~ 100L/h.
Embodiment 1
In order to realize the present invention, negative resin dynamics in a kind of condensation water refined processing high-speed mixing bed of assembling voluntarily
Performance index SO 4 2-Coefficient of mass transfer measure device used, as shown in Figure 1, comprise high-pressure pump 4, spinner-type flowmeter 7, hydrogen exchange column 10 and conductivity meter A9 and conductivity meter B11, characterized by further comprising resin test pole mixed bed 8 and the transfer valve 3 of washing fluid inlet water tank 1 with cover plate, the test fluid inlet water tank 2 with cover plate, constant water bath box 6, jacketed;
The outlet of described washing fluid inlet water tank 1 with cover plate and joins by pipeline with the outlet of the test fluid inlet water tank 2 of cover plate after pass through a transfer valve 3 and be connected with the inlet duct of high-pressure pump 4;
Be provided with stainless-steel tube 5 in described constant water bath box 6, an end of stainless-steel tube 5 is connected with the outlet of high-pressure pump 4, and the other end passes through resin test pole mixed bed 8, conductivity meter A9, hydrogen exchange column 10 and the conductivity meter B11 of spinner-type flowmeter 7, jacketed successively.
Its process route, be the Stainless Steel Coil 5 of power in transfer valve 3, constant water bath box 6 that washing fluid and test fluid are provided by high-pressure pump 4 by different inlet water tanks respectively, by resin test pole mixed bed 8, conductivity meter A9, hydrogen exchange column 10 and the conductivity meter B11 of spinner-type flowmeter 7, jacketed, finally flow out successively.
Wherein, in the chuck of the test pole mixed bed 8 of constant water bath box 6 and jacketed, water keeps circulation and constant temperature, namely the temperature by test fluid coil pipe and test pole adjusting test fluid is 25 ± 0.5 ℃, guarantee that the test fluid temperature perseverance that conductivity meter shows is 25 ± 0.5 ℃, make the impact of conductivity meter reading tested person liquid temp very little.
Application Example 1
Utilize negative resin dynamic performance index S O in 1 one kinds of condensation water refined processing high-speed mixing beds of embodiment 4 2-Coefficient of mass transfer measure device used, test Dow Chemical is without the dynamic performance index S O of the new 550A type strong basic anion-exchange resin that uses 4 2-Coefficient of mass transfer.Its method of testing is as follows:
(1), the preparation of mixed bed sun resin
Get 150mL sun resin, make it be immersed in tap water and leach immediately, get water logging sun resin, water logging sun resin is loaded in the glass actifier column, be that the 4%HCl of 13～14 times of water logging sun resin volume is with the approximately flow velocity regeneration of 10mL/min with volume again, the HCl regenerated liquid goes out water concentration when consistent with influent concentration, and regeneration ending is led to going out water power＜0.5 μ s/cm with the pure water rinsing of 50 ~ 60 ℃;
Described HCl regenerated liquid is 4% HCl aqueous solution;
Described positive resin is the new resin of Tao Shi 650C type;
Above-mentioned glass actifier column used is that volume is greater than the glass column of 150mL;
(2), the preparation of mixed bed negative resin
Get 75mL 28～30 order negative resins, it is immersed in tap water, and leaches immediately; Then clean water logging sun resin 2 times with 4%HCl, negative resin after hydrochloric acid cleaning is loaded in the glass actifier column, be that the 26-27 NaOH regenerated liquid doubly of the negative resin volume after pickling is with the approximately flow velocity regeneration of 10mL/min with volume again, the NaOH regenerated liquid goes out water concentration when consistent with influent concentration, regeneration ending is led to going out water power＜0.5 μ s/cm with the pure water rinsing of 50～60 ℃;
Described NaOH regenerated liquid is that concentration is the NaOH aqueous solution of 2mol/L;
Described negative resin is that Dow Chemical is without the new resin of 550A type that uses;
Above-mentioned glass actifier column used is that volume is greater than the glass column of 75mL;
(3), the mixed bed yin and yang resin mixes the dress post
Step (1) and the good yin, yang resin of (2) flushing are poured in a 500mL large beaker of cleaning, pour out the upper strata excessive moisture, mix, with washed with de-ionized water test pole mixed bed, after having cleaned, seal the lower end rising pipe, pour 10～20mL pure water into, the resin that mixes is poured in test pole mixed bed with chuck, avoid producing bubble and layering;
(4), the preparation of hydrogen exchanging column resin
1L sun resin is immersed in tap water and leaches immediately, get water logging sun resin, water logging sun resin is loaded in the glass actifier column, be that the 4%HCl regenerated liquid of 2 times of water logging sun resin volume is with the approximately flow velocity regeneration of 10mL/min with volume again, when the HCl regenerated liquid goes out water concentration when consistent with influent concentration, regeneration ending is led to going out water power＜0.5 μ s/cm with the pure water rinsing of 50-60 ℃;
Described HCl regenerated liquid is 4% HCl aqueous solution;
Described positive resin is the new resin of Tao Shi 650C type;
Above-mentioned glass actifier column used is that volume is greater than the glass column of 1L;
(5), the flushing of mixed bed test pole
Deionized water is got ultrapure water used by the ultrapure water resin;
After the resin test pole mixed bed of jacketed and hydrogen exchange column are respectively charged into corresponding resin, the regulating thermostatic bath temperature is 30 ℃ of left and right, guarantee that the conductivity meter temperature is 25 ± 0.5 ℃, the opening high pressure pump, with test pole and the hydrogen exchange column of ultrapure water as washing fluid flushed zone chuck, flushing speed is controlled at 1 ~ 1.2L/min, makes water outlet conductivity＜0.07 μ s/cm, and stablizes at least 10min;
Described positive resin is Tao Shi 550A type resin;
If be shorter than 10min stabilization time, illustrate that the resin regeneration effect is bad or it is inhomogeneous to mix, need again to regenerate, to mix resin and fill post;
(6), SO 4 2-The test of coefficient of mass transfer
With the 0.0900g anhydrous Na 2SO 4Be dissolved in and make Na used in the 1L ultrapure water 2SO 4Solution;
With 27.3g NH 3(top grade pure " 25～28% ") are dissolved in and make ammoniacal liquor used in the 1L pure water;
In situ preparation 25L ultrapure water adds 12.5mL Na immediately 2SO 4Solution and 50mL NH 3Solution makes test fluid, passes into test fluid with the flow velocity of 1L/min, measures and record the reading of conductivity meter B, remains unchanged in 1min to reading, and test finishes, with the ultrapure water flushing line, to the conductivity meter reading be 0.07 μ s/cm;
(7), negative resin dynamic performance index-SO 4 2-The calculating of coefficient of mass transfer K
According to the Harries model, calculate SO 4 2-Coefficient of mass transfer
The Harries model is:
Figure 2011101362951100002DEST_PATH_IMAGE005
In formula: ε: bed voidage.
Figure 2011101362951100002DEST_PATH_IMAGE006
M is heavy for the oven dry filtrate ,=resin volume * wet pseudodensity
=0.785×150 + 0.657×75 = 166.525；
ρ is average wet true density;
Figure 122291DEST_PATH_IMAGE007
V is the resin cumulative volume ,=150mL+75mL=225mL.
Top concrete numerical value is brought in formula calculated, draw the value of concrete ε
Figure 2011101362951100002DEST_PATH_IMAGE008
R: resinoid volume ratio,
F: test fluid flow velocity, 1L/min;
A: test pole bed sectional area, A=π r 2(r is the test pole internal diameter ,=12.5mm)=4.9cm 2
L: the test pole bed is dark, i.e. test pole resin height, 0.46m;
D: resin-like harmonic average diameter, 0.615 * 10 -3m
Figure 234921DEST_PATH_IMAGE003
P wherein iBe the percentage composition of the resin of a certain diameter section,
Figure 49293DEST_PATH_IMAGE004
d 1, d 2Be mesh size, d 1=0.63mm, d 2=0.60mm;
C: sulfate radical goes out water concentration, μ g/L;
C leads to convert according to the survey electricity and tries to achieve,
ΔDD=8.768×10 -3×C
The conductivity difference of Δ DD conductivity meter B when intaking take ultrapure water and test fluid as device respectively;
C 0Be the test fluid sulfate concentration, μ g/L is configuration concentration 300 μ g/L in test.
The conductivity difference of conductivity meter B when measuring and recording ultrapure water and test fluid and be the device water inlet, SO 4 2-The result of calculation of coefficient of mass transfer as shown in table 2.
Application Example 2
Utilize negative resin dynamic performance index S O in 1 one kinds of condensation water refined processing high-speed mixing beds of embodiment 4 2-Coefficient of mass transfer measure device used, the dynamic performance index S O in the 550A type strong basic anion-exchange resin of test used Dow Chemical 4 2-Coefficient of mass transfer.Its method of testing is as follows:
Negative resin described in step (2) be Dow Chemical use the 550A type strong basic anion-exchange resin of a year in Waigaoqiao of Shaihai power plant, other are with Application Example 1, the conductivity difference of conductivity meter B when finally measuring and recording ultrapure water and test fluid and be the device water inlet, SO 4 2-The result of calculation of coefficient of mass transfer as shown in table 2.
Application Example 3
Utilize negative resin dynamic performance index S O in 1 one kinds of condensation water refined processing high-speed mixing beds of embodiment 4 2-Coefficient of mass transfer measure device used, the dynamic performance index S O of the new exchange resin of CPA02 type strong alkali anion of test MIT 4 2-Coefficient of mass transfer.Its method of testing is as follows:
Negative resin described in step (2) is that MIT is without the new new exchange resin of CPA02 type strong alkali anion that uses, other are with Application Example 1, the conductivity difference of conductivity meter B when finally measuring and recording ultrapure water and test fluid and be the device water inlet, SO 4 2-The result of calculation of coefficient of mass transfer as shown in table 2.
Test result and the table 1 of table 2 are compared, can find out, no matter new resin is the 550A type strong basic anion-exchange resin of Dow Chemical, or the CPA02 type strong basic anion-exchange resin of MIT, SO 4 2-Coefficient of mass transfer be 1.91 and 1.86, resin all is in satisfactory state, can guarantee water quality condition, guarantees on-the-spot normal operation.
The dynamic performance test result of three kinds of negative resins of table 2
New 550A type The on-the-spot 550A type that uses New CPA02 type
SO 4 2-Coefficient of mass transfer K/10 -4m/s 1.91 1.44 1.86
The 550A type strong basic anion-exchange resin SO of on-the-spot used Dow Chemical 4 2-Coefficient of mass transfer only have 1.44, resin is in " transition state ".
Above said content is the basic explanation under conceiving for the present invention only, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.

Claims (2)

1. negative resin dynamic performance index S O in a condensation water refined processing high-speed mixing bed 4 2-Coefficient of mass transfer measure device used, comprise high-pressure pump, spinner-type flowmeter, hydrogen exchange column and conductivity meter A and conductivity meter B, characterized by further comprising resin test pole mixed bed and the transfer valve of washing fluid inlet water tank, test fluid inlet water tank, constant water bath box, jacketed;
The outlet of the outlet of described washing fluid inlet water tank and test fluid inlet water tank is connected with the inlet duct of high-pressure pump by a transfer valve after joining by pipeline;
Be provided with stainless-steel tube in described constant water bath box, an end of stainless-steel tube is connected with the high pressure delivery side of pump, and the other end passes through resin test pole mixed bed, conductivity meter A, hydrogen exchange column and the conductivity meter B of spinner-type flowmeter, jacketed successively.
2. one kind is adopted device claimed in claim 1 to carry out negative resin dynamic performance index S O in condensation water refined processing high-speed mixing bed 4 2-The assay method of coefficient of mass transfer, it is characterized in that comprising the steps:
(1), the preparation of mixed bed sun resin
Get 150mL sun resin, make it be immersed in tap water and leach immediately, get water logging sun resin, water logging sun resin is loaded in the glass actifier column, be that the 4%HCl of 13～14 times of water logging sun resin volume is with the approximately flow velocity regeneration of 10mL/min with volume again, the HCl regenerated liquid goes out water concentration when consistent with influent concentration, regeneration ending, with the pure water rinsing of 50～60 ℃ to water outlet conductivity＜0.5 μ s/cm;
Described HCl regenerated liquid is 4% HCl aqueous solution;
Described positive resin is the new resin of Tao Shi 650C type;
Above-mentioned glass actifier column used is that volume is greater than the glass column of 150mL;
(2), the preparation of mixed bed negative resin
Get 75mL 28～30 order negative resins, it is immersed in tap water, and leaches immediately; Then clean the water logging negative resin 2 times with 4%HCl, negative resin after hydrochloric acid cleaning is loaded in the glass actifier column, be that the 26-27 NaOH regenerated liquid doubly of the negative resin volume after pickling is with the approximately flow velocity regeneration of 10mL/min with volume again, the NaOH regenerated liquid goes out water concentration when consistent with influent concentration, regeneration ending, with the pure water rinsing of 50～60 ℃ to water outlet conductivity＜0.5 μ s/cm;
Described NaOH regenerated liquid is that concentration is the NaOH aqueous solution of 2mol/L;
Described negative resin is the new resin of CPA02 type of Tao Shi 550A type resin or Mitsubishi;
Above-mentioned glass actifier column used is that volume is greater than the glass column of 75mL;
(3), the mixed bed yin and yang resin mixes the dress post
Step (1) and the good yin, yang resin of (2) flushing are poured in a 500mL large beaker of cleaning, pour out the upper strata excessive moisture, mix, with washed with de-ionized water test pole mixed bed, after having cleaned, sealing lower end rising pipe is poured 10～20mL pure water into, the resin that mixes is poured in the resin test pole mixed bed of jacketed;
(4), the preparation of hydrogen exchanging column resin
1L sun resin is immersed in tap water and leaches immediately, get water logging sun resin, water logging sun resin is loaded in the glass actifier column, be that the 4%HCl regenerated liquid of 2 times of water logging sun resin volume is with the approximately flow velocity regeneration of 10mL/min with volume again, when the HCl regenerated liquid goes out water concentration when consistent with influent concentration, regeneration ending uses the pure water rinsing of 50-60 ℃ to water outlet conductivity＜0.5 μ s/cm;
Described HCl regenerated liquid is 4% HCl aqueous solution;
Described positive resin is the new resin of Tao Shi 650C type;
Above-mentioned glass actifier column used is that volume is greater than the glass column of 1L;
(5), the flushing of test pole mixed bed
Deionized water is got ultrapure water used by the ultrapure water resin;
After the resin test pole mixed bed of jacketed and hydrogen exchange column are respectively charged into corresponding resin, regulating thermostatic water bath temperature is 30 ℃ of left and right, guarantee that conductivity meter A temperature is 25 ± 0.5 ℃, the opening high pressure pump, with resin test pole mixed bed and the hydrogen exchange column of ultrapure water as washing fluid flushed zone chuck, flushing speed is controlled at 1 ~ 1.2L/min, makes water outlet conductivity＜0.07 μ s/cm, and stablizes at least 10min;
(6), SO 4 2-The test of coefficient of mass transfer
With the 0.0900g anhydrous Na 2SO 4Be dissolved in and make Na used in the 1L ultrapure water 2SO 4Solution;
With 27.3g NH 3Be dissolved in and make ammoniacal liquor used in the 1L pure water;
In situ preparation 25L ultrapure water adds the Na of gained immediately 2SO 4The ammoniacal liquor 50mL of solution 12.5mL and gained makes test fluid;
Test fluid is packed in the test fluid inlet water tank, and control with the flow velocity of 1L/min resin test pole mixed bed, conductivity meter A, hydrogen exchange column and the conductivity meter B through the stainless-steel tube in transfer valve, high-pressure pump, constant water bath box, spinner-type flowmeter, jacketed, measure and record the reading of conductivity meter B, remain unchanged in 1min to reading, test finishes, with the ultrapure water flushing line, to conductivity meter A reading be 0.07 μ s/cm;
(7), negative resin dynamic performance index-SO 4 2-The calculating of coefficient of mass transfer K
According to the Harries model, calculate SO 4 2-Coefficient of mass transfer:
Figure 2011101362951100001DEST_PATH_IMAGE002
In formula, K is top SO 4 2-Coefficient of mass transfer, m/s;
ε: bed voidage;
R: resinoid volume ratio,
Figure 2011101362951100001DEST_PATH_IMAGE004
F: the flow velocity of test fluid, m/s;
A: the resin test pole mixed bed sectional area of jacketed, m 2
L: the resin test pole mixed bed of jacketed is dark, i.e. resin height, m;
D: resin-like harmonic average diameter, m
Figure 2011101362951100001DEST_PATH_IMAGE006
P wherein iBe the percentage composition of the resin of a certain diameter section, d 1, d 2Be mesh size, cm;
C: the test fluid sulfate radical goes out water concentration, μ g/L;
C =ΔDD/（8.768×10 -3）
Wherein, the conductivity difference of Δ DD conductivity meter B when intaking take ultrapure water and test fluid as device respectively;
C 0Be test fluid sulfate radical influent concentration, 300 μ g/L.
CN 201110136295 2011-05-25 2011-05-25 Device and method for testing mass transfer coefficient of anion resin dynamic performance index SO4<2-> Expired - Fee Related CN102305811B (en)

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