CN105242032A - Apparatus for determining maximum regeneration capacity of hydrogen-oxygen type anion exchange resin - Google Patents

Apparatus for determining maximum regeneration capacity of hydrogen-oxygen type anion exchange resin Download PDF

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Publication number
CN105242032A
CN105242032A CN201510623776.3A CN201510623776A CN105242032A CN 105242032 A CN105242032 A CN 105242032A CN 201510623776 A CN201510623776 A CN 201510623776A CN 105242032 A CN105242032 A CN 105242032A
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China
Prior art keywords
resin
hydrogen
scavenge trunk
anion exchange
type anion
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CN201510623776.3A
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CN105242032B (en
Inventor
周少玲
许立国
张永
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State Grid Corp of China SGCC
Electric Power Research Institute of State Grid Shandong Electric Power Co Ltd
Maintenance Branch of State Grid Shandong Electric Power Co Ltd
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State Grid Corp of China SGCC
Electric Power Research Institute of State Grid Shandong Electric Power Co Ltd
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Priority to CN201510623776.3A priority Critical patent/CN105242032B/en
Publication of CN105242032A publication Critical patent/CN105242032A/en
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Abstract

The present invention discloses an apparatus for determining the maximum regeneration capacity of a hydrogen-oxygen type anion exchange resin. The apparatus comprises a device B and a device C, wherein the device B is an opening container, the device C comprises a filter, the outlet pipeline of the device C is provided with a flow rate control device, the opening of the device B is connected to the inlet end of the device C, a closed chamber is formed between the device C and the device B and the unchanged volume of the chamber is maintained when the flow rate control device is closed, the device C is provided with a ventilation pipe, the bottom end of the ventilation pipe extends inside the device B, the top end of the ventilation pipe extends out of the external of the device B, the top end of the ventilation pipe is provided with a gas flow rate control device, and in a stationary state, the bottom end of the ventilation pipe is positioned above the liquid level of a reaction solution. With the apparatus of the present invention, the problems that the three factors such as the cooling time difference between the resin and the soaking liquid, the cooling way difference between the resin and the soaking liquid, and the resin sucking during the soaking liquid shifting-out affect the determination of the maximum regeneration capacity of the hydrogen-oxygen type anion exchange resin, and the bottle cork breaking is avoided are solved.

Description

A kind of device measuring hydrogen-oxygen type anion exchange resins maximum regeneration capacity
Technical field
The invention belongs to power grid construction field, particularly a kind of device measuring hydrogen-oxygen type anion exchange resins maximum regeneration capacity.
Technical background
Anion exchange resins is widely used in generating plant, pharmaceutical factory, electron trade, plays an important role purifying water, except in negative ion, organism etc. in anhydrating.Maximum regeneration capacity is the important performance indexes of hydrogen-oxygen type anion exchange resins, it is related to naval stores quality and the water yield processed, be related to the price between supplier and user and interests, so Accurate Determining hydrogen-oxygen type anion exchange resins maximum regeneration capacity important in inhibiting.
Ion exchange resin exchange capacity refers to that Board Lot (weight or volume) resin can carry out the total amount of the chemical group of ion-exchange reactions, and the temperature of reaction of ion exchange resin and soak solution, equilibration time are the key factors affecting exchange capacity.In standard GB/T/T5760-2000 " hydrogen-oxygen type Determination of Capacity of Basic Anion Exchange Resin method " 8.1 " mensuration of hydrogen-oxygen type anion exchange resins maximum regeneration capacity " its to the effect that: get a certain amount of resin after treatment and proceed in tool plug triangular flask, add 100mL hydrochloric acid standard solution, cover tightly bottle stopper, put and soak 2 hours to 40 DEG C of water-soluble pots, be cooled to room temperature, soak solution 25mL in tool plug triangular flask (must not sucking-off resin) is shifted out with transfer pipet, put into another erlenmeyer flask, add appropriate reagent water and indicator, titration is carried out with standard solution of sodium hydroxide, volumescope according to consuming NaOH titer calculates hydrogen-oxygen type anion exchange resins maximum regeneration capacity.
Defect and the deficiency of 8.1 these methods and operation existence 4 aspects in GB/T5760-2000 is proved through test of many times:
A.GB/T5760-2000 method regulation " soak solution is put and soaked 2 hours to 40 DEG C of water-soluble pots; be cooled to room temperature ", the method weak point is: soak solution takes out and is cooled to room temperature from 40 DEG C of water-soluble pots, and in cooling procedure, required cool time depends on ambient temperature.But room temperature is variable element, in same region, room temperature is different throughout the year; Even if different geographical on the same day, room temperature is also different, and thus soak solution is also different because of the change of room temperature parameter from 40 DEG C of times being cooled to room temperature, and the time causing resin and soak solution to be cooled to room temperature, with season, geographical diversity and changing, is a underrange.So soak solution is during being cooled to room temperature, the adsorption equilibrium that the hydrochloric acid solution in hydrogen-oxygen type anion exchange resins and soak solution is set up, because equilibration time difference creates the error at measurment of ion exchange resin maximum regeneration capacity.
B. soak solution is cooled to its type of cooling of room temperature is that variable element (1) cools naturally; (2) water quench is used.The type of cooling is different, and the time that soak solution is cooled to room temperature is different, produces ion exchange resin maximum regeneration volumetric determination error.
C. this operating conditions of soak solution 25mL in tool plug triangular flask (must not sucking-off resin) is shifted out with transfer pipet harsh, should not grasp, especially when resin wet true density is less, at the top of soak solution, middle part, bottom resin all adrift, resin will be inhaled into transfer pipet accidentally, cause test titration error, produce ion exchange resin maximum regeneration volumetric determination error.
D. in water-bath, in order to prevent bottle stopper tripping, the weight that need add 500g heavy is pushed down, and this regulation is difficult.Due to taper stopper band point, with weight push down band point object because of contact point too little, weight is pressed on bottle stopper insecure.Because bottle internal gas pressure is high in test, bottle stopper is backed down and is slipped to the accident broken into pieces on the ground and happens occasionally, cause test to stop on the way, can not carry out smoothly by warranty test.
Summary of the invention
In order to solve resin and soak solution difference cool time, type of cooling difference, when shifting out soak solution, 3 kinds of factors such as sucking-off resin affect the mensuration of capacity hydrogen-oxygen type anion exchange resins maximum regeneration capacity, and avoid bottle stopper in test to break a difficult problem into pieces, invent a kind of device measuring hydrogen-oxygen type anion exchange resins maximum regeneration capacity, this device can make resin soak in 40 DEG C of water-soluble pots after 2 hours and hightail soak solution, during soak solution is cooled to room temperature, the equilibration time of soak solution and equilibrium concentration do not limit by room temperature and the type of cooling, and suck a difficult problem for resin when avoiding transfer pipet to shift out soak solution completely.The bottle stopper of this device not only sternly stitches with reaction bulb plying and bottle stopper weight is large, avoids the difficult problem that in process of the test, bottle stopper is broken into pieces by jack-up, guarantees the accuracy of hydrogen-oxygen type anion exchange resins maximum regeneration volumetric determination, guarantees that test is carried out smoothly.
The object of this invention is to provide a kind of device measuring hydrogen-oxygen type anion exchange resins maximum regeneration capacity, described device (device A) is made up of device B and device C, device B is open containers, device C comprises filtrator, scavenge trunk, volume control device, the outlet conduit of described device C is provided with volume control device, and the opening of described device B is connected with the entrance point of described device C; When volume control device closes, form airtight cavity between described device C and device B and keep cavity constancy of volume; Described device C is provided with scavenge trunk, and the bottom of described scavenge trunk extends to device B inside, and the top of described scavenge trunk extends to device B outside, and described scavenge trunk top is provided with gas flow control device; Under static state, the bottom of described scavenge trunk is in more than reactant liquor liquid level.
Preferably, described device B is the container with outer grinding port, and described device C is the filtrator with interior ground, and the internal diameter of described interior ground is identical with outer grinding port external diameter.
Preferably, described device B is the container with interior ground, and described device C is the filtrator with outer grinding port, and the internal diameter of described interior ground is identical with outer grinding port external diameter.
At present, ion exchange resin bead footpath requires generally to be greater than 0.315 millimeter, but finds in experimentation: resin or impurity inevitably doped with part small particle diameter in reaction solution, therefore, in multiple preferred embodiment of the present invention, the aperture of preferred filter plate is less than 0.2 millimeter.
Preferred, described filtrator is provided with filter plate, and the aperture of described filter plate is 0.192-0.193 millimeter.
Preferably, the level height on the top of described scavenge trunk is lower than scavenge trunk bottom.When avoiding device A is inverted filter liquor, filtrate is run out of from tongs.
Preferably, when volume control device closes, described device C is positioned at the top of device B.
Preferably, described device B is flat conical vessel.
Preferably, described volume control device is piston or valve.
Preferably, the bottom surface of the inside of described device B has roughly conical shape, the thickness of the thick in the roughly conical shape of the described bottom surface of the inside of described device B is set to a ratio with the ratio of the thickness of most thin section, under this ratio, when described device B at the uniform velocity shakes, in the interface of described resin to be measured and described soak solution, the size resulting from the shear strain of described resin to be measured is the same.
The object of this invention is to provide a kind of method measuring hydrogen-oxygen type anion exchange resins maximum regeneration capacity, the ion exchange resin reacting the schedule time under predetermined condition is separated with reactant liquor, using the reactant liquor after separation as solution to be measured, measure the exchange capacity of ion exchange resin according to corresponding national regulations.
Concrete steps are as follows:
1) ion exchange resin and reactant liquor are reacted the schedule time under predetermined temperature in device A, obtain soak solution;
2) inverted device A, the flow controller of device for opening A and gas flow controller, filtration step 1) soak solution that obtains, obtain filtrate, filtrate is measured the exchange capacity of ion exchange resin according to corresponding national regulations.
Beneficial effect of the present invention:
Feature 1. as shown in Figure 1, the effect of the piston 1 on C device is: valve function, this piston is opened during filter infusion liquid, soak solution is separated automatically with the resin in device B, resin is stayed in device B, after soak solution is leached by device C, soak solution filtrate proceeds in another clean, dry tool plug erlenmeyer flask, for future use.
Feature 2. as shown in Figure 1, when filter liquor, open, play gas exchange action by the scavenge trunk 2 on C device by the tongs 5 on flexible pipe 4, and the degree of depth that scavenge trunk 2 inserts conical flask is conical flask 150mL scale mark 3 place.
As shown in Figure 1, the inwall of C device inlays a filter plate 10 to feature 3., and material is core or pottery, and its aperture is less than 0.2 millimeter;
As shown in Figure 1, piston on A device 1 and scavenge trunk 2, in the same side, are conducive to resin and flow out along same direction and easy to operate feature 4..
Design concept
This device A is made up of device B and device C, and device B and device C complete set, device C is enclosed within the outside forming apparatus A of device B.Device B is the 250mL erlenmeyer flask with outer grinding port; Device C has interior ground and device B is supporting, and device C is furnished with piston, scavenge trunk, filter core.The weight of the device C of design is large and sternly stitch with the plying of device B ground, avoids in bottle stopper experimentation by a difficult problem that jack-up is broken into pieces.Soak solution containing resin soaked after 2 hours in 40 DEG C of water-soluble pots, use device A that resin is separated rapidly with soak solution, the soak solution obtained is not resinous, thus 3 kinds of factors such as sucking-off resin affect the error at measurment of the hydrogen-oxygen type anion exchange resins maximum regeneration capacity caused by cooling time difference, type of cooling difference, when shifting out soak solution to avoid resin and soak solution, ensure that the accuracy of hydrogen-oxygen type anion exchange resins maximum regeneration capacity.
Accompanying drawing explanation
Fig. 1 device A wherein, 1-glass piston; 2-glass scavenge trunk; 3-conical flask 150mL scale mark; 4-flexible pipe; 5-tongs; 6-resin; 7-soak solution; 8-conical flask outer grinding port; Ground in 9-conical flask; 10-filter
Fig. 2 device B
Fig. 3 device C
The inverted A device of Fig. 4
Concrete embodiment
Embodiment 1
Apparatus of the present invention A is made up of device B and device C, and device B and device C complete set, device C is enclosed within the outside forming apparatus A of device B.Device B is the 250mL erlenmeyer flask with outer grinding port; Device C has interior ground and device B is supporting, and device C is furnished with piston, scavenge trunk, filter core.The weight of the device C of design is large and sternly stitch with the plying of device B ground, avoids in bottle stopper experimentation by a difficult problem that jack-up is broken into pieces.Soak solution containing resin soaked after 2 hours in 40 DEG C of water-soluble pots, use device A that resin is separated rapidly with soak solution, the soak solution obtained is not resinous, thus 3 kinds of factors such as sucking-off resin affect the error at measurment of the hydrogen-oxygen type anion exchange resins maximum regeneration capacity caused by cooling time difference, type of cooling difference, when shifting out soak solution to avoid resin and soak solution, ensure that the accuracy of hydrogen-oxygen type anion exchange resins maximum regeneration capacity.
As shown in Figure 1, the effect of the piston 1 on C device is: valve function, this piston is opened during filter infusion liquid, soak solution is separated automatically with the resin in device B, resin is stayed in device B, after soak solution is leached by device C, soak solution filtrate proceeds in another clean, dry tool plug erlenmeyer flask, for future use.
As shown in Figure 1, the tongs 5 on flexible pipe 4, when filter liquor, is opened, is played gas exchange action by the scavenge trunk 2 on C device, and the degree of depth that scavenge trunk 2 inserts conical flask is conical flask 150mL scale mark 3 place.
As shown in Figure 1, the inwall of C device inlays a filter plate 10, and material is core or pottery, and its aperture is less than 0.2 millimeter;
As shown in Figure 1, piston on A device 1 and scavenge trunk 2, in the same side, are conducive to resin and flow out along same direction and easy to operate.
Detailed operating procedures
The mensuration of 1 hydrogen-oxygen type anion exchange resins maximum regeneration capacity
1.1 take two increment product with Subtraction method, and the every increment product of strong-base anion-exchange resin are about 2.5g; Weakly-basic anion is handed over
Change the every increment product of resin and be about 2.0g; Be accurate to 0.1mg, be placed in dry device B respectively.
1.2 put in the device B of sample to each, and add 0.1mol/L hydrochloric acid standard solution 100.00mL with transfer pipet, shake up, device C is enclosed within forming apparatus A on device B, piston 1, tongs 5 are in closed condition.Device A is put into 40 DEG C of water-baths to soak 2 hours, take out, device A is inverted as shown in Figure 4, opens piston 1, open tongs 5, in inverted device A lower end with the soak solution filtrate 11 that clean, a dry erlenmeyer flask then filters out, till the filtrate in device A has been filtered.
1.3 take out 25mL soak solution filtrate with transfer pipet from erlenmeyer flask is placed in another erlenmeyer flask, adds 50mL pure water and 2 instructions phenolphthalein solutions.
1.4 are titrated to blush with the Standard Volumetric Solutions for Sodium Hydroxide of 0.1mol/L keeps 15s colour-fast, is terminal.
Embodiment 2
Be with the difference of embodiment 1, described device B is the container with outer grinding port, and described device C is the filtrator with interior ground, and the internal diameter of described interior ground is identical with outer grinding port external diameter.
Embodiment 3
Be with the difference of embodiment 1, described device B is the container with interior ground, and described device C is the filtrator with outer grinding port, and the internal diameter of described interior ground is identical with outer grinding port external diameter.
Embodiment 4
Be with the difference of embodiment 1, the level height on the top of described scavenge trunk is lower than scavenge trunk bottom.
Embodiment 5
Be with the difference of embodiment 1, the bottom surface of the inside of described device B has roughly conical shape, the thickness of the thick in the roughly conical shape of the described bottom surface of the inside of described device B is set to a ratio with the ratio of the thickness of most thin section, under this ratio, when described device B at the uniform velocity shakes, in the interface of described resin to be measured and described soak solution, the size resulting from the shear strain of described resin to be measured is the same.
Embodiment 6
Be with the difference of embodiment 1, described filtrator is provided with filter plate, and the aperture of described filter plate is less than 0.2 millimeter.
Embodiment 7
Be with the difference of embodiment 1, described filtrator is provided with filter plate, and the aperture of described filter plate is 0.192-0.193 millimeter.
Although above-mentioned, the specific embodiment of the present invention is described; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.

Claims (10)

1. one kind measures the device of hydrogen-oxygen type anion exchange resins maximum regeneration capacity, it is characterized in that, described device is made up of device B and device C, device B is open containers, device C comprises filtrator, scavenge trunk, volume control device, the outlet conduit of described device C is provided with volume control device, and the opening of described device B is connected with the entrance point of described device C; When volume control device closes, form airtight cavity between described device C and device B and keep cavity constancy of volume; Described device C is provided with scavenge trunk, and the bottom of described scavenge trunk extends to device B inside, and the top of described scavenge trunk extends to device B outside, and described scavenge trunk top is provided with gas flow control device; Under static state, the bottom of described scavenge trunk is in more than reactant liquor liquid level.
2. device as claimed in claim 1, it is characterized in that, described device B is the container with outer grinding port, and described device C is the filtrator with interior ground, and the internal diameter of described interior ground is identical with outer grinding port external diameter.
3. device as claimed in claim 1, it is characterized in that, described device B is the container with interior ground, and described device C is the filtrator with outer grinding port, and the internal diameter of described interior ground is identical with outer grinding port external diameter.
4. device as claimed in claim 1, it is characterized in that, be provided with filter plate in described filtrator, the aperture of filter plate is less than 0.2 millimeter.
5. device as claimed in claim 1, it is characterized in that, the level height on the top of described scavenge trunk is lower than scavenge trunk bottom.
6. device as claimed in claim 1, it is characterized in that, when volume control device closes, described device C is positioned at the top of device B.
7. device as claimed in claim 1, it is characterized in that, described volume control device is piston or valve.
8. device as claimed in claim 1, it is characterized in that, the bottom surface of the inside of described device B has roughly conical shape, the thickness of the thick in the roughly conical shape of the described bottom surface of the inside of described device B is set to a ratio with the ratio of the thickness of most thin section, under this ratio, when described device B at the uniform velocity shakes, in the interface of described resin to be measured and described reactant liquor, the size resulting from the shear strain of described resin to be measured is the same.
9. the device described in any one of claim 1-8 is measuring the application in hydrogen-oxygen type anion exchange resins maximum regeneration capacity.
10. one kind measures the method for hydrogen-oxygen type anion exchange resins maximum regeneration capacity, it is characterized in that, the ion exchange resin reacting the schedule time under predetermined condition is separated with reactant liquor, using the reactant liquor after separation as solution to be measured, measure the exchange capacity of ion exchange resin according to corresponding national regulations.
CN201510623776.3A 2015-09-25 2015-09-25 A kind of device for determining hydrogen-oxygen type anion exchange resin maximum regeneration capacity Expired - Fee Related CN105242032B (en)

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US5621163A (en) * 1995-12-20 1997-04-15 Johnson; David H. Apparatus for testing resin flow
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CN204395563U (en) * 2014-12-15 2015-06-17 中国原子能科学研究院 A kind of grournd glass Flange filter
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Inventor after: Zhou Shaoling

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