CN102471098B - Ion-exchange device, process and equipment for producing same, and method and device for forming ion-exchange resin layer - Google Patents
Ion-exchange device, process and equipment for producing same, and method and device for forming ion-exchange resin layer Download PDFInfo
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- CN102471098B CN102471098B CN201080029277.7A CN201080029277A CN102471098B CN 102471098 B CN102471098 B CN 102471098B CN 201080029277 A CN201080029277 A CN 201080029277A CN 102471098 B CN102471098 B CN 102471098B
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- ion
- exchange resin
- interchange unit
- container
- ion exchange
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- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 title claims abstract description 160
- 239000003456 ion exchange resin Substances 0.000 title claims abstract description 160
- 229920003303 ion-exchange polymer Polymers 0.000 title claims abstract description 160
- 238000000034 method Methods 0.000 title claims abstract description 47
- 238000005342 ion exchange Methods 0.000 title abstract description 44
- 230000008569 process Effects 0.000 title abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 125
- 239000000428 dust Substances 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 238000000746 purification Methods 0.000 claims abstract description 15
- 238000011049 filling Methods 0.000 claims description 66
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 32
- 239000012498 ultrapure water Substances 0.000 claims description 32
- 238000002360 preparation method Methods 0.000 claims description 20
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 238000007670 refining Methods 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims 2
- 239000003957 anion exchange resin Substances 0.000 abstract description 32
- 239000003729 cation exchange resin Substances 0.000 abstract description 28
- 230000003749 cleanliness Effects 0.000 abstract description 6
- 238000003860 storage Methods 0.000 abstract description 6
- 150000002500 ions Chemical class 0.000 description 92
- 239000011347 resin Substances 0.000 description 92
- 229920005989 resin Polymers 0.000 description 92
- 239000002002 slurry Substances 0.000 description 63
- 239000012530 fluid Substances 0.000 description 46
- 239000000203 mixture Substances 0.000 description 42
- 230000008676 import Effects 0.000 description 32
- 230000008929 regeneration Effects 0.000 description 24
- 238000011069 regeneration method Methods 0.000 description 24
- 238000000926 separation method Methods 0.000 description 17
- 230000015572 biosynthetic process Effects 0.000 description 15
- 239000000945 filler Substances 0.000 description 12
- 239000007788 liquid Substances 0.000 description 11
- 230000004888 barrier function Effects 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 230000001276 controlling effect Effects 0.000 description 9
- 239000012528 membrane Substances 0.000 description 7
- 230000008520 organization Effects 0.000 description 7
- 239000003814 drug Substances 0.000 description 5
- 238000011068 loading method Methods 0.000 description 5
- 229920006395 saturated elastomer Polymers 0.000 description 5
- 230000007246 mechanism Effects 0.000 description 4
- 230000001172 regenerating effect Effects 0.000 description 4
- 238000004062 sedimentation Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000013467 fragmentation Methods 0.000 description 3
- 238000006062 fragmentation reaction Methods 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- 238000011001 backwashing Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229920001429 chelating resin Polymers 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 229910017518 Cu Zn Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000007726 management method Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004457 water analysis Methods 0.000 description 1
- 238000013316 zoning Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/02—Loose filtering material, e.g. loose fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/02—Non-contaminated water, e.g. for industrial water supply
- C02F2103/04—Non-contaminated water, e.g. for industrial water supply for obtaining ultra-pure water
Abstract
A process for producing an ion-exchange device is provided in which ion-exchange resins are prevented from being fouled by airborne dust. An anion-exchange resin and a cation-exchange resin are purified and metered respectively through receiving tanks (11, 21), purification columns (14, 24), storage tanks (16, 26), and metering tanks (19, 29), mixed together in a mixing tank (30), and then filled into a vessel (33). The metering tanks (19, 29), the mixing tank (30), and the vessel to be filled (33) are disposed in a clean room (41) having a degree of cleanliness of 10,000 or higher. The produced ion-exchange device is subjected to a water-passing test, and the effluent water is analyzed in a high-cleanliness clean room (42) having a degree of cleanliness of 1,000 or higher.
Description
Technical field
The present invention relates to a kind of filling ion-exchange resin in container and make the method and apparatus of ion interchange unit, particularly relating to a kind of preparation method and equipment of ion interchange unit of the making that is applicable to the ion interchange unit that ultra-pure water manufacturing process etc. uses.The present invention relates to a kind of by the ion interchange unit of the method and equipment made.In addition, the present invention relates to a kind of filling ion-exchange resin in container and form method and the device of resinbed.The present invention relates to a kind ofly have by the method and install the ion interchange unit of formed resinbed.
Background technology
In the past, as ion interchange unit, to adopt following ion interchange unit mostly, fixed ion interchange unit particularly, wherein, it is configured to: cationic ion-exchange resin, anion exchange resin, these hybrid resin or the hybrid resin of these and other resin are filled in container and form resinbed, allow processed liquid by carrying out ion-exchange treatment.And, after resinbed is saturated, stop allowing processed liquid pass through, then, allow regenerated liquid by and resinbed is regenerated, then allow detergent remover by after cleaning, start once again to allow processed liquid by and start once again to carry out ion-exchange treatment.
Yet, like this alternately and the ion interchange unit that repeatedly carries out ion-exchange treatment and regeneration, when carrying out the regeneration of resinbed, have the shortcoming that cannot carry out ion-exchange treatment.Therefore, as the replacement of this ion interchange unit and there is a kind of ion interchange unit of elements exchange formula, it is the ion exchange resin filler cells that adopts the reassembling type of filling ion-exchange resin in movable main body container, after being carried to scene, being installed on ion interchange unit and carrying out ion-exchange treatment, after resinbed is saturated, from ion interchange unit, ion exchange resin filler cells is unloaded, the unit more renewing and proceed ion-exchange treatment, the ion exchange resin filler cells unloading is on the other hand recovered, by the use of regenerating as required of used ion exchange resin.
The ion interchange unit of this elements exchange formula comprises does not regenerate the ion exchange resin filler cells unloading from ion interchange unit and direct discarded non-renewable type ion interchange unit and ion exchange resin being regenerated and the regeneration use type ion interchange unit that re-used.Situation the latter, comprises: to the unit of each recovery respectively by the mode of ion exchange resin regeneration; From unit collection of ions exchanger resin, regenerated, the ion exchange resin after regeneration is filled in to unit and is carried to after on-the-spot standby, be installed on ion interchange unit and carry out the mode etc. of ion-exchange treatment.
In patent documentation 1 (Japanese kokai publication hei 9-70546 communique), recorded a kind of ion-exchange unit, be filling ion-exchange resin and forming in main body container, and allow and be connected in raw water tubes, process water pipe etc. and use from the outstanding pipe of container.Fig. 2 is the ion-exchange unit U that the document is recorded.This ion-exchange unit U is the ion exchange resin 2 after the interior filling of the container 1 with peristome 1a is adjusted.In peristome 1a installing, cover 6.On lid 6, be provided with the introducing port 3 of ion exchange resin, and former water ingress pipe 5 and processing water take-off pipe 4 are arranged to connect shape.It is the bottoms that are inserted in container 1 that former water imports path 4, in its lower end, filter 5a is set.
The filter 4a that is arranged on the lower end of processing water taking-up path 5 is the top that is positioned at container 1.
Ion exchange resin 2 is to see through resin introducing port 3 to be filled in container 1.Introducing port 3, is sealed after this.Resin introducing port 3, is when connecting, to be used for carrying out draining, discharge air etc., and normally airtight when ion-exchange treatment.
This ion-exchange unit is that the state that cut off with the position at connector 4b, 5b imposes and seals and be carried to scene and install.And, utilize this connector 4b, 5b to be connected with expansion joint 7,8, to carry out the importing of former water and the taking-up (paragraph 0021～0022) of processing water (ultra-pure water).
As ion exchange resin, be to comprise: by cationic ion-exchange resin or the independent situation of filling of anion exchange resin and situations with the ratio mixing filling of 1: 3～3: 1 left and right of Capacity Ratio by both.(paragraph 0018)
Being installed on the ion-exchange unit U of ion exchange system, is that former water is imported to container 1 from the former current road (not shown) of ion interchange unit by former water ingress pipe the 4, the 1st filter 4a, through carrying out ion-exchange by resinbed 2; Processing water is that from processing water take-off pipe 5, the processing current road (not shown) by ion interchange unit is removed after the 2nd filter 5a collects.After ion exchange resin 2 is saturated, utilize connector 4b, 5b to unload and be replaced with new unit ion-exchange unit U, to proceed ion-exchange treatment.
Used ion-exchange unit U, that the state unloading is carried and reclaimed, as required ion exchange resin taken out and regenerated, the ion exchange resin after regeneration is filled in once again container 1 and forms ion interchange unit, to supply once again ion-exchange treatment.
For main body container 1 filling ion-exchange resin at above-mentioned ion-exchange unit U, be to allow ion exchange resin be scattered in water and import with slurry shape, the water of carrying under one's arms is discharged by filter 4a, 5a are separated.According to the method, in main body container 1, fill the ion exchange resin of ormal weight and can have any problem.
In patent documentation 4 (No. 2002-28501, TOHKEMY), record following example: be to be carried to scene accommodate ion exchange resin in ion exchange resin mobile containers after, be filled at the scene ion interchange unit and supply to carry out ion-exchange, from ion interchange unit, ion exchange resin is taken out after saturated and after being contained in ion exchange resin mobile containers, be carried to the place that arranges of regenerating unit, the ion exchange resin after regeneration is contained in once again to ion exchange resin mobile containers and is carried to scene.As this ion exchange resin mobile containers, possesses the pipe arrangement being connected with filter element (being equivalent to filter) in container, ion exchange resin is be scattered in water and import with slurry shape, the water of carrying under one's arms is discharged by filter element is separated, thus, carry out filling ion-exchange resin, still, and the unexposed ion exchange resin loading that makes becomes ormal weight.
Ion exchange resin, the amount of resin that will measure regulation under drying regime is easy.But when ion-exchange, because ion exchange resin is to be filled in liquid phase to use, being again to take the volume of resinbed carry out characterization and process as benchmark, being therefore filled in the amount of resin of container, is to require to become specified volume to be present under the state of liquid phase.In this situation, ion exchange resin is to be scattered in slurry shape in water to import and be filled in container, but owing to cannot making the amberlite lipid concentration in slurry become setting, even if measure slurry, still cannot fill the resin of ormal weight.
With regard to the method for filling ormal weight resin, measure in advance the method that the resin that will fill is filled again, must measure in advance the resin after the regeneration of ormal weight, then allow it in water, be dispersed into slurry shape and import, therefore the combination of complex steps must be adopted and in fact the trouble that becomes can have any problem.In addition, each container is measured to the method for weight resin, because the existing water yield can affect the instrumentation of weight, be in fact difficult to carry out correct metering.Moreover, utilize the visual method of carrying out instrumentation resin filling amount, must repeatedly stop logical liquid and visual instrumentation, in addition, if container maximizes and makes resin filling quantitative change many, there is the problem that is difficult to carry out correct instrumentation.
Generally speaking, till filling if content is filled in the container of specified volume, the capacity of its filler can become setting.In patent documentation 1,4, the resinbed being filled in container is not filled, and remains the space that does not form resinbed on the top of container.As so, have in the container of enough and to spare, though be difficult to fill the ion exchange resin of specified volume, but by by container and be disposed at filter wherein and structure of pipe arrangement etc., configuration etc. give regularization, its capacity becomes specified volume, therefore, till filling if ion exchange resin is filled in the container of this specified volume, the capacity of resinbed should become setting.
If import ion exchange resin in generic container with slurry shape, useless water also can be imported into.Owing to being difficult to make the concentration of the ion exchange resin in slurry become setting, therefore, it is difficult making the capacity of filled ion exchange resin become setting.With respect to this, as one, in Patent Document 2, possesses the pipe arrangement being connected with filter in container, ion exchange resin is imported with the slurry shape being scattered in water, the water of carrying under one's arms is discharged by filter is separated, thus, carrys out the method for filling ion-exchange resin, if while filling, the capacity of the ion exchange resin of filling should become setting.
Yet the situation that ion exchange resin slurry is carried by pump, if still carry by pump after filling, the packed density of resin becomes too high and becomes and cannot carry out water flowing, or it is broken that resin occurs, or filter and pipe arrangement easily stop up, and have problems.In the case, though can consider the ion exchange resin detecting in container according to the pressure rise of supply slurry has filled with stop supplies slurry, but in order correctly to detect pressure rise with stop supplies slurry, must adopt complicated device and controlling organization etc., and be difficult to the ion exchange resin in slurry to form the uniform packed layer of packed density from carrying under one's arms water separation, therefore exist many problems.
In patent documentation 5 (No. 2002-221160, TOHKEMY), recorded a kind of air pressure drive-type membrane pump as fluid pressure drive-type pump.This air pressure drive-type membrane pump is the pump that belongs to two diaphragm types, at two pump chambers, is respectively equipped with barrier film, is engaged in the front end of main shaft (run through midfeather and slidably) and forms integratedly, thus, can move back and forth.Yet, and the unexposed ion exchange resin loading that makes becomes ormal weight.
In patent documentation 6 (No. 2007-305019, TOHKEMY), recorded a kind of controlling organization, in air pressure drive-type pump etc., when driving the air pressure of use, pump arrives the time point of authorized pressure, remove acting on the air pressure of pump and stop driving pump.Yet, this controlling organization, be result from barrier film etc. damage and dally, cause the situation that for driving, air pressure rises, be used for detecting the rising of this air pressure and stop driving pump, itself and the unexposed ion exchange resin loading that makes become ormal weight.
In following patent documentation 2,3, recorded and be used for the medicament of method and refining use of refinement treatment ion exchange resin.
Patent documentation
Patent documentation 1: Japanese kokai publication hei 9-70546 communique
Patent documentation 2: Japanese kokai publication hei 5-15789 communique
Patent documentation 3: Japanese kokai publication hei 9-201539 communique
Patent documentation 4: TOHKEMY 2002-28501 communique
Patent documentation 5: TOHKEMY 2002-221160 communique
Patent documentation 6: TOHKEMY 2007-305019 communique
In semiconductor industry, in clean and other purposes of semiconductor article, can use ultra-pure water, to the water quality requirement of this ultra-pure water, be more and more stricter, for example, metal concentration is below 1ppt, optionally also has the situation of the superelevation water quality requiring below 0.1ppt.
In this case, in order to prevent the seepage of metal from ion interchange unit etc., must be in ion interchange unit the refining ion exchange resin of packed height.
Yet, be, in atmosphere, highly refined ion exchange resin is filled in to container in the past, therefore airborne dust can be sneaked into, and may make ion exchange resin that micro-pollution occurs.
Summary of the invention
The problem that invention will solve
The 1st object of the present invention is, a kind of preparation method and equipment that prevents the ion interchange unit of airborne dust pollution ion exchange resin is provided, and uses the method and the produced ion interchange unit of equipment.
The 2nd object of the present invention is, providing a kind of can correctly be filled in container by the ion exchange resin of ormal weight in the short time by simple mechanism and shirtsleeve operation and form resinbed, and can prevent formation method and the device of the ion exchange layer of the high density filling of ion exchange resin and the obstruction of fragmentation or pipe arrangement etc., and there is the ion interchange unit that uses the method and install formed resinbed.
Solve the method for problem
The preparation method of the ion interchange unit of the 1st technical scheme and equipment, it is that the ion exchange resin after refinement treatment is filled in to the method that container is made ion interchange unit, it is characterized in that, the filling step that ion exchange resin is filled in to this container is to carry out in dust free room.
The preparation method of the ion interchange unit of the 2nd technical scheme and equipment, it is in the 1st technical scheme, and ion exchange resin is carried out after refinement treatment not contact the state of atmosphere, via pipe arrangement, not contact the state of atmosphere, to aforementioned filling step, transfers.
The preparation method of the ion interchange unit of the 3rd technical scheme and equipment, it is in the 1st or the 2nd technical scheme, be set up in parallel the purification apparatus that carries out refinement treatment is a plurality of, the ion exchange resin of only processing one species by a purification apparatus, different types of ion exchange resin is processed by different purification apparatus.
The preparation method of the ion interchange unit of the 4th technical scheme and equipment, it is in the 3rd technical scheme, and the ion exchange resin of plural kind respectively after different purification apparatus is refined, is measured by different measuring tanks, then, in mixing channel mixing, be filled in aforementioned container.
The preparation method of the ion interchange unit of the 5th technical scheme and equipment, it is in arbitrary technical scheme of the 1st to 4, the cleaniliness classs of aforementioned dust free room is below 10000.
The preparation method of the ion interchange unit of the 6th technical scheme and equipment, it is in arbitrary technical scheme of the 1st to 5, for the ion interchange unit after filling ion-exchange resin, in aforementioned dust free room, carry out the water flowing of ultra-pure water, analyze outflow water from ion interchange unit to check ion interchange unit.
The preparation method of the ion interchange unit of the 7th technical scheme and equipment, it is in the 6th technical scheme, the analysis of aforementioned outflow water is to carry out in cleaniliness classs is the high-cleanness, high dust free room below 1000.Wherein, the cleanliness factor of dust free room of the present invention, means 1 cubic feet of (1ft
3) volume space in the number of the more than 0.3 μ m particulate that swims, grade 10000 has 10000 particulates in representing 1 cubic feet, grade 1000 has 1000 particulates in representing 1 cubic feet.
In the preparation method and equipment of the ion interchange unit of 1st～7 technical schemes, owing to ion exchange resin being filled in to the filling step of container, be to carry out in dust free room, can prevent from allowing airborne dust sneak in ion interchange unit at this filling step.Therefore,, by using the method and the produced ion interchange unit of equipment, can produce the good ultra-pure water of water quality.The present invention is in Ultrapure Water Purifiers, is specially adapted to preparation method and the equipment of the ion-exchange refining treatment apparatus (Ion Exchange Polisher, non-renewable type ion interchange unit) as subsystem (second pure water system).The present invention is specially adapted to as the Ultrapure Water Purifiers of manufacturing highly purified ultra-pure water, such as manufacturing wafer, manufacture preparation method and the equipment of the ion interchange unit of the Ultrapure Water Purifiers that semiconductor etc. uses.According to the Ultrapure Water Purifiers with the ion interchange unit of method and apparatus made of the present invention, easily produce the ultra-pure water of metal concentration 1ppt following (further for 0.1ppt is following).
According to the method and apparatus of the 2nd technical scheme, owing to not contacting atmosphere in purification step and subsequent handover step intermediate ion exchanger resin, therefore can prevent that airborne dust is sneaked into ion exchange resin in these steps.
According to the method and apparatus of the 3rd technical scheme, because different types of ion exchange resin is to carry out refinement treatment by different purification apparatus mutually, therefore can prevent that different types of ion exchange resin from sneaking in ion exchange resin.
According to the method and apparatus of the 4th technical scheme, because measuring tank is also to arrange respectively according to the kind of ion exchange resin, even mixed bed type ion interchange unit still can mix and fill ion exchange resin up to specification.
As described in the 5th technical scheme, the cleaniliness classs of dust free room is preferably below 10000.
Method and apparatus according to the 6th technical scheme, carries out water flowing to the ion interchange unit after filling ion-exchange resin, after the water quality of inspection outflow water, carries out shipment again, therefore can guarantee the quality of ion interchange unit.In the 7th technical scheme, because this examination of water is to carry out, therefore check that precision is high in cleaniliness classs is the dust free room of the high-cleanness, high below 1000.
Formation method and the device of the resinbed of the 8th technical scheme, it is that the mixture slurry of ion exchange resin and water is imported to container, water is discharged from the container after by filter separation, thus, filling ion-exchange resin in container and form method and the device of resinbed, it is characterized in that
The mixture slurry of ion exchange resin and water is to be supplied to container by fluid pressure drive-type pump,
When aforementioned pump drives the fluid pressure of use, arrive the time point of authorized pressure, releasing acts on the fluid pressure of pump and stops driving pump.
Formation method and the device of the resinbed of the 9th technical scheme, it is in the 8th technical scheme, the time point releasing that drives the fluid pressure of use to arrive authorized pressure when pump acts on the fluid pressure of pump and stops after driving pump, start once again driving pump, when pump drives the fluid pressure of use, arrive once again the time point of authorized pressure, releasing acts on the fluid pressure of pump and stops driving pump.
Formation method and the device of the resinbed of the 10th technical scheme, it is in the 8th or 9 technical schemes, container possesses that the former water that is connected in the 1st filter imports path, the processing water that is connected in the 2nd filter takes out path and resin imports path; By resin, import path the mixture slurry of ion exchange resin and water is imported to container, by the 1st and/or the 2nd filter, by discharging from former water importing path and/or processing water taking-up path after water separation, thus, in container, form resinbed.
Formation method and the device of the resinbed of the 11st technical scheme, it is in 8th～10 technical schemes, fluid pressure drive-type pump is air pressure drive-type pump, and possess: when pump drives the air pressure of use, arrive the time point of authorized pressure, remove the controlling organization that acts on the air pressure of pump and stop driving pump.
In 8th～11 technical schemes, as fluid pressure drive-type pump, be more preferably air pressure drive-type membrane pump.
In 8th～11 technical schemes, ion exchange resin is more preferably the hybrid resin of cationic ion-exchange resin and anion exchange resin.
Accompanying drawing explanation
Fig. 1 is the preparation method of ion interchange unit and the flow chart of device of an explanation technical scheme of the present invention.
Fig. 2 is the profile of ion interchange unit.
Fig. 3 is the formation method of resinbed of embodiment and the flow chart of device.
The specific embodiment
The embodiment of 1st～7 technical schemes is described with reference to Fig. 1 below.In the present embodiment, be that anion exchange resin and cationic ion-exchange resin respectively after refining and metering, are mixed and are filled in container.
Anion exchange resin is from flexible container bag etc., to deliver to special-purpose accepting groove 111 to store.Anion exchange resin in this accepting groove 111 is to deliver to treating column (adjustment tower) 114 by pump 112 and pipe arrangement 113.In this treating column, by ultra-pure water and adjustment, with medicine, carry out the refining of ion exchange resin.As adjustment medicine, the various medicines such as medicine that can use aforementioned patent document 1～3 grade to record.Refinement treatment draining is sent to recovery system (not shown), after processing with the form recycling of ultra-pure water.In addition, the treating column of cationic ion-exchange resin described later also carries out same processing, processes water vent and similarly reclaims.
Anion exchange resin after refinement treatment, is sent to measuring tank 119 by pipe arrangement 115, storage tank 116, pump 117, pipe arrangement 118.
Cationic ion-exchange resin, is stored in special-purpose accepting groove 121, via pump 122, pipe arrangement 123, is sent to treating column 124, after refinement treatment, by pipe arrangement 125, storage tank 126, pump 127, pipe arrangement 128, is sent to measuring tank 129.
The mixing channel 130 of these measuring tanks 119,129 and its rear class etc. is to be arranged in the dust free room 141 of cleanliness factor below 10000.In measuring tank 119,129, with anion exchange resin and cationic ion-exchange resin after ormal weight metering, by special-purpose pipe arrangement 119a, 129a, import mixing channel 130 respectively and mix.Mixed ion exchange resin, is sent to container 133 and is filled by pump 131, pipe arrangement 132.As container 133, be the container that uses structure identical with earlier figures 2, ion exchange resin is that the resin introducing port from container 133 is filled in container 133 and formation ion interchange unit.
After filling completes, resin introducing port is airtight.Then, ion interchange unit is sent to the inspection step in dust free room 141.At this, check in step, from being arranged at the former water introducing port of container 133, by pipe arrangement 135, import ultra-pure water, the analytic engine 137 that the processing water taking out from processing water conveying end is sent in analysis room 142 by pipe arrangement 136 carries out water analysis.Inspection draining is discharged to recovery system by pipe arrangement 138.If check result is qualified, the former water introducing port of container 133 and processing water conveying end is airtight, by dust free room gateway 143, outside dust free room 1141, send.Underproof ion interchange unit is also from gateway 143 taking-up to dust free room 141.Above-mentioned analysis room 142 is cleanliness factor high-cleanness, high dust free rooms below 1000.
In the preparation method of the ion interchange unit of this Fig. 1; owing to ion exchange resin being filled in to the filling step of container 133, be to carry out in the dust free room below 10,000 141 at cleanliness factor, can prevent from allowing airborne dust sneak in ion interchange unit at this filling step.Therefore,, by using the ion interchange unit of so producing, can manufacture the good ultra-pure water of water quality.
In the present embodiment; in treating column 114,124 not contact after the state of atmosphere imposes refinement treatment by anion exchange resin, cationic ion-exchange resin; ion exchange resin is transferred by pipe arrangement 115,118,125,128 not contact the state of atmosphere; at measuring tank 119,129 and mixing channel 130, not contact the state of atmosphere, measure and mix; therefore, can prevent that airborne dust is sneaked into ion exchange resin in these handovers, metering and blend step.
In addition, in the present embodiment, anion exchange resin and cationic ion-exchange resin use respectively special-purpose accepting groove 111,121, treating column 114,124, storage tank 116,126, measuring tank 119,129 and each pipe arrangement and pump is transferred, refining and metering, therefore, can prevent from allowing ion exchange resin not of the same race sneak into ion exchange resin in these steps.In addition, because being does not measure and mixes and be filled in container 133 sneaking into the pure anion exchange resin only consisting of single kind of ion exchange resin of the same race not and cationic ion-exchange resin, therefore, can make the mixed bed type ion interchange unit that mixing up to specification is filled with anion exchange resin and cationic ion-exchange resin.
In the present embodiment, the ion interchange unit after filling ion-exchange resin is carried out to the water flowing of ultra-pure water, carry out again shipment after check flowing out the water quality of water, therefore can positively allow high-quality ion interchange unit shipment.Because this examination of water is to carry out in the dust free room 142 of the high-cleanness, high below 1000 at cleaniliness classs, therefore check that precision is high.
In the above-described embodiment, anion exchange resin and cationic ion-exchange resin are processed, transferred by special-purpose accepting groove 111～measuring tank 119 and accepting groove 121～measuring tank 129 respectively, but be while using the resin of different model at anion exchange resin, each model is arranged to the pipeline of special-purpose accepting groove～measuring tank, by the pipeline of each model specific, process anion exchange resin.Cationic ion-exchange resin is also same, when using the resin of different model, each model is arranged to special-purpose pipeline, and each model is processed by special-purpose pipeline.So, can prevent that the anion exchange resin of different model from sneaking in anion exchange resin, or the cationic ion-exchange resin of different model is sneaked in cationic ion-exchange resin.
In the above-described embodiment, anion exchange resin and cationic ion-exchange resin are passed through after measuring tank 119,129 meterings, at mixing channel 136, mix and be filled in container 133, but also can be only the anion exchange resin of self-measuring groove 119 or be filled in container 133 and make anion exchange device or cation exchange device from the cationic ion-exchange resin of measuring tank 129 in the future.
In the present invention, preferably on container, set up bar code with management progress and origin.
Below, embodiment and the comparative example of 1st～7 technical schemes are described.
Embodiment 1
Use the ion interchange unit making apparatus shown in Fig. 1, in the container (72L) of the structure shown in Fig. 2, anion exchange resin and cationic ion-exchange resin are produced to ion interchange unit with mixing in 1: 1.To this ion interchange unit, the ultra-pure water of concentration of metal ions shown in table 1 is carried out to the water flowing of 24 hours with the state of SV=60/h.The water quality that the ion interchange unit of taking for the 24th hour flows out water is shown in table 1.
Comparative example 1
In Fig. 1, except using the ion interchange unit making apparatus of the structure that dust free room 141 is not set, be to produce similarly to Example 1 ion interchange unit, carry out water test.The water quality that the ion interchange unit of taking for the 24th hour flows out water is shown in table 1.
Table 1 (unit: ppt)
| No. | Cu | Zn | Fe | Ca | Na |
| Former water (ultra-pure water) | 0.01 | 0.01 | 0.01 | 0.02 | 0.01 |
| Embodiment 1 | 0.01 | 0.01 | 0.01 | 0.01 | 0.01 |
| Comparative example 1 | 0.45 | 0.3 | 0.01 | 0.2 | 0.01 |
As known from Table 1, the ion interchange unit of the application of the invention method and apparatus made, can produce the ultra-pure water of high water quality.
8th～11 technical schemes are then described.
In 8th～11 technical schemes, resinbed is the resinbed that is formed at the ion interchange unit of Water Purifiers, Ultrapure Water Purifiers, wastewater treatment equipment, ionic adsorption device etc., wherein, have be arranged at fixed ion interchange unit, elements exchange formula ion interchange unit, make the resinbed etc. of ion interchange unit etc. of the resins exchange formula of spent ion exchange resin mobile containers.In addition, its object also comprises the resinbed etc. of the container of ion exchange resin mobile containers that the ion interchange unit of the ion exchange resin filler cells that is formed at the ion interchange unit of said units switch type and uses, resins exchange formula uses or resin storage tank etc.In these, as its object, be preferably the resinbed that is formed at the ion exchange resin filler cells that the ion interchange unit of elements exchange formula uses.
Form the ion exchange resin of resinbed, can enumerate: the resin in pelletized form of cationic ion-exchange resin, anion exchange resin, chelating resin, other Selective adsorption resin, these hybrid resin or the hybrid resin of these and inactive resin, other resins etc.These resins no matter be brand-new resin or re-use resin all can, no matter but be which situation, be preferably the resin importing of regenerate be filled in container and formation resinbed.
The container of filling ion-exchange resin is not particularly limited, and can directly be filled in the container that requires to form resinbed.As this container, can enumerate: fixed, resins exchange formula, the ion exchange tower of other ion interchange units, the ion exchange resin mobile containers that the ion interchange unit of the ion exchange resin filler cells that the ion interchange unit of elements exchange formula uses, resins exchange formula uses, resin storage tank, other containers etc.Particularly suitable be the container of specified volume, also the resin of specified volume can be filled with the packed density of regulation, when filling, can form the resinbed of specified volume.As this container, can enumerate: the ion exchange resin filler cells that the ion interchange unit of elements exchange formula uses.
As the container of filling ion-exchange resin, more preferably for possessing resin, import the container of the filling device of path (being used for the mixture slurry of ion exchange resin and water to import container), filter (water of carrying under one's arms gives separated) and Separation of Water drain passageway (Separation of Water is discharged from the container) etc. in container.More preferably for possessing the container of internal volume for stipulating under the state of these filling devices.In addition, the container that does not possess these filling devices also can, still, in the case, by these filling devices are installed, allow to carry out the filling of resin.As ion exchange tower, ion exchange resin filler cells, as ion-exchange treatment with and in the situation that container possesses, the former water that is connected in the 1st filter imports path, the processing water that is connected in the 2nd filter takes out path and resin imports path, these a side or two can use as aforementioned filling device.As filter, preferably there is the opening of 0.1～0.3mm to avoid the ion exchange resin of particle diameter 0.4～0.5mm to flow out.
In 8th～11 technical schemes, the mixture slurry of ion exchange resin and water is imported to container with filling ion-exchange resin, and water is discharged from the container after by filter separation, thus, in container, form resinbed.In the case, the mixture slurry of ion exchange resin and water is supplied to container by fluid pressure drive-type pump, and Separation of Water is discharged, if fill ion exchange resin in container, the pressure that spues of pump uprises, corresponding therewith, and pump drives the fluid pressure of use also to uprise.Therefore, when pump drives the fluid pressure of use, arrive the time point of authorized pressure, the fluid pressure that will act on pump is removed, and thus, stops driving pump and can in container, form the resinbed of specified volume.
In 8th～11 technical schemes, the capacity of ion exchange resin, being in pure water (ultra-pure water), to drop into ion exchange resin, until resin bed do not change, is generally speaking standing 10～20 minutes and make the capacity measured under the state of its sedimentation.As ion exchange resin, be the situation of using the hybrid resin of cationic ion-exchange resin and anion exchange resin etc., the capacity of ion exchange resin is input hybrid resin and capacity that the state of its standing sedimentation is measured in pure water (ultra-pure water).Ion exchange resin, because being fills mixture slurry with pressurized state, the packed density that is formed at the resinbed in container uprises, therefore, the resin capacity that forms resinbed, has than the more situation of the resin capacity that is equivalent to vessel volume.In the present invention, be to make the capacity of the ion exchange resin that pressurized state fills become setting.
The mixture slurry of ion exchange resin and water, it is the slurry that mixes above-mentioned ion exchange resin and water, if the mixed proportion of resin uprises, the mobility step-down of slurry and resin become and easily stop up, if again the mixed proportion step-down of resin the separated water yield become many and hinder operability.Therefore, the preferred mixed proportion of ion exchange resin and water, being preferably ion exchange resin under the state that forms around water (not yet standing sedimentation and make the state of water separation) and the Capacity Ratio of water is (70: 30)～(90: 10).
In 8th～11 technical schemes, the mixture slurry of ion exchange resin and water is by importing and be filled in container after the pressurization of fluid pressure drive-type pump, at this moment mixture slurry is supplied to the supply pressure (being also the pressure that spues of pump) of container, be preferably and easily carry out the padding of resin and can avoid resin fragmentation and the pressure of uniform filling, generally speaking, can set the pressure within the scope of 0.2～0.7MPa for.As such stuffing pressure, if identical with the pressure of logical hydraulic pressure that puts on resinbed in ion interchange unit, the situation of the ion exchange resin filler cells using at the ion interchange unit of elements exchange formula, after ion interchange unit installation unit, the adjustment that need not implement resinbed before logical liquid just can start to lead to liquid, therefore comparatively preferred.
In said pump, spue to depress mixture slurry is supplied to container, when time the name a person for a particular job fluid pressure that acts on pump that pump drives the fluid pressure of use to arrive authorized pressure is removed and stopped driving pump, thus, though can form the resinbed of specified volume in container, but have the inhomogeneous situation of packed density, have by initial padding and be difficult to form the packed density situation of resinbed completely uniformly.Therefore in padding once and after stopping driving pump, start driving pump once again and supply slurry, when pump drives the fluid pressure of use, arrive once again the time point of authorized pressure, releasing acts on the fluid pressure of pump and stops driving pump, can form thus the resinbed of uniform filling density.In the case, be preferably in initial padding and after stopping driving pump, the placement stipulated time, for example 1～20 minute, after more preferably 5～10 minutes, start once again driving pump.So, repeatedly carry out stopping and driving as long as once of pump, but more repeatedly its uniformity is higher, and can fills equably the resin of ormal weight.
Fluid pressure drive-type pump, can use possess when pump drive the fluid pressure of use arrive authorized pressure time name a person for a particular job and act on the fluid pressure drive-type pump of the controlling organization that the fluid pressure of pump removed.Thus, in container, be filled with the ion exchange resin of ormal weight and become the time point of filling, along with slurry pushes the rising of pressure and makes pump drive the fluid pressure of use to rise, therefore when driving the fluid pressure of use, pump arrives the time point of authorized pressure, can automatically terminate the fluid pressure that acts on pump.Thus, can under the ion exchange resin loading without too much or not enough, allow the driving of pump stop.
Detect spuing of pump and press and allow controlling organization that pump stops or press the time point uprising automatically to stop the mechanism etc. of pump spuing of pump, the hybrid system of resin and water be difficulty and must use complicated mechanism and operation, but in this system, corresponding to the rising of filling the formed pump of resin and spuing and pressing, pump drives the fluid pressure of use to rise sensitively, therefore as long as control pump drives the fluid pressure of use, just can corresponding to filling of resin, allow pump stop.In this situation, because pump drives the fluid of the use solid matter as not resinous, the structure of its machine and operation running etc. can simplification.If particularly use air to drive the fluid of use as pump, the more simplification that can become such as the structure of machine and running operation, with respect to system, carry out be taken into, discharge etc. becomes easily, can correctly control according to the rules.
As fluid pressure drive-type pump, be preferably air pressure drive-type pump, by adopting the advantage that air pressure possesses as fluid pressure to comprise: its produce, process and discarded etc. easily, again to do the used time compressed and can reduce resin the occurred breakage etc. that is hit.In addition, be preferably and possess: when pump drives the air pressure of use, arrive the time point of authorized pressure, can remove the air pressure that acts on pump and the controlling organization that stops driving pump, thus, make to control and become easy, unlikely damage resin and filling with correct packed density, can form the resinbed of specified volume.As air pressure drive-type pump, can move reciprocating pump etc. for reciprocal, but be preferably air pressure drive-type membrane pump.By adopting air pressure drive-type membrane pump, can reduce the impact to resin, and can further reduce the damage of resin, and control easily, can fill and form the resinbed of specified volume with correct packed density.
As container, when use possesses former water, import path (being connected in the 1st filter), process the container that water takes out path (being connected in the 2nd filter) and resin importing path, it is for example the situation of the ion exchange resin filler cells that uses of the ion interchange unit of elements exchange formula, by resin, import path the mixture slurry of ion exchange resin and water is imported to container, water is given to separation by the 1st and/or the 2nd filter, from former water, import path and/or process the discharge of water taking-up path again, thus, can in container, form resinbed.So carry out, form the container of resinbed, can directly be installed on ion interchange unit, thus, allow the logical liquid of processed liquid and carry out ion-exchange treatment, container is reclaimed after saturated and allow filling once again after resin regeneration, and can use repeatedly.
In 8th～11 technical schemes, as the resinbed that forms object, according to the ion interchange unit of the different objects of Water Purifiers, Ultrapure Water Purifiers, wastewater treatment equipment, ionic adsorption device etc., when the restricted situation of imported impurity level, the water using as carrying, be preferably to use corresponding to the pure water that requires purity, ultra-pure water etc. and form resinbed, and carry out padding under the less environment such as dust of dust free room etc.
According to 8th～11 technical schemes, the mixture slurry of ion exchange resin and water is imported to container, water is discharged from the container by filter is separated, thus, filling ion-exchange resin in container and forming in the method for resinbed, that the mixture slurry of ion exchange resin and water is supplied to container by fluid pressure drive-type pump, when driving the fluid pressure of use, aforementioned pump arrives the time point of authorized pressure, releasing acts on the fluid pressure of pump and stops driving pump, form thus resinbed, therefore, utilize simple mechanism and shirtsleeve operation, can correctly the ion exchange resin of ormal weight be filled in to container at short notice and form resinbed and there is the ion interchange unit of this resinbed, and the high density that can prevent ion exchange resin is filled and is broken, or the obstruction of pipe arrangement etc.
Below, the embodiment of 8th～11 technical schemes is described with Fig. 3.In Fig. 3, container 1 is the container of the ion-exchange unit U that uses of the ion interchange unit of Component units switch type, and it has identical structure with the container in Fig. 2.Also, ion-exchange unit U, is to form the resinbed 2 after regeneration in the inside of the container 1 of reassembling type.On the top of container 1, form peristome 1a, and be provided with and cover 6 (by resin import path 3, former water imports path 4 and processes water taking-up path 5 and gives integrated).At former water, import path 4 and process the bottom that water takes out path 5, the leading section in extending to container 1 is provided with respectively the 1st filter 4a and the 2nd filter 5a.In addition, at former water, import path 4 and process the top that water takes out path 5, connector 4b, 5b being installed respectively, and forming the expansion joint 7,8 that can be connected in resin filling device.Expansion joint 7,8 is to be connected in outside stream 11,12 by joint 9,10.
In Fig. 2, resinbed 2 is not filled in all of container 1, and on the top of container 1, is formed with water layer; In Fig. 3, resinbed 2 is that the state of filling is filled in all of container 1.In addition as resinbed 2, be the hybrid resin of filling male ion-exchange resin and anion exchange resin.The structure of other ion-exchange unit U and to basic operation of container 1 potting resin etc. is identical with the situation essence illustrated in fig. 2.
The ion-exchange unit U that is formed with resinbed 2 of manufacturing, with the illustrated situation of Fig. 2 similarly, that the state that cut off with the position at connector 4b, 5b imposes and seals and be carried to scene, be installed on after ion interchange unit, by connector 4b, 5b be equivalent to outside stream 11,12 ion interchange unit former current road and process current road (all not shown) to be connected and ion-exchange is carried out in confession.At this moment resin imports path 3, is for carrying out Bas Discharged etc.
In Fig. 3, in order to fill hybrid resin in container 1, be provided with cationic ion-exchange resin regeneration tank 21, anion exchange resin regeneration tank 22, mixing channel 23, in these grooves, carry out separation, regeneration, mixing of ion exchange resin etc., then, the resin after regeneration is imported to the container 1 that is filled in ion-exchange unit U by pump 30.
Then explanation gives used ion exchange resin to mix the situation of filling separation, regeneration from the ion-exchange unit U reclaiming, from the container 1 of reclaimed ion-exchange unit U, the hybrid resin that forms resinbed 2 is imported to cationic ion-exchange resin regeneration tank 21 from pipeline L1, from pipeline L2, carry pure water and resin is imposed to back washing separation, the anion exchange resin after separation is imported to anion exchange resin regeneration tank 22 from pipeline L5.Then from pipeline L3, cationic ion-exchange resin regeneration tank 21 is carried out the logical liquid of regenerative agent (acid), from pipeline L4, discharge regeneration discharge opeing and by cationic ion-exchange resin regeneration, the cationic ion-exchange resin after regeneration is transferred to mixing channel 23 from pipeline L6.In addition, from pipeline L7, pure water is sent to anion exchange resin groove 22 and resin is imposed back washing, from pipeline L8, carry out the logical liquid of regenerative agent (alkali), from pipeline L9, regeneration discharge opeing discharged and make anion exchange resin regeneration, the anion exchange resin after regeneration is transferred to mixing channel 23 from pipeline L11.
In mixing channel 23, from pipeline L12 supply air and pure water, and from pipeline L13 supply pure water and and mixed with resin, to form the mixture slurry of resin and water.This mixture slurry, be from pipeline L14 by pump 30 suck, pressurization and the resin by ion-exchange unit U imports path 3 and imports containers 1 from pipeline L15, carry under one's arms water by after the 1st filter 4a and the 2nd filter 5a separation, by expansion joint 7,8, joint 9,10, from outside stream 11,12, discharge, fills thus formation resinbed 2.
At the opposition side of barrier film 33a, the 33b of pump chamber 32a, 32b, form and drive air chamber 36a, 36b (be communicated in respectively and drive air flue 37a, 37b).In the bottom of pump chamber 32a, 32b, check- valves 38a, 38b are set, by slurry, suck path 41 respectively and be communicated in pipeline L14.In addition, on the top of pump chamber 32a, 32b, check- valves 39a, 39b are set, by slurry feed path 42, are communicated in pipeline L15 respectively. Drive air flue 37a, 37b not to be linked to across transfer valve 43 with slurry feed path 42.Transfer valve 43 is to be communicated in air feed path 44 and Bas Discharged path 45.
The time point that drives the air pressure of use to arrive authorized pressure when pump is set in pump 30 and can removes the air pressure that acts on pump and the control device 50 that stops driving pump.As this control device 50, for example, adopt disclosed control device in patent documentation 6 (No. 2007-305019, TOHKEMY).This control device 50 is consisted of control valve 51, three-way valve 52 and control valve 53.Control valve 51, by valve body 54 (regulating by adjuster 55) zoning Cheng 1 56 He 2 fluid chamber 57 of fluid chamber.1 fluid chamber 56 arranges and drives air intake 58 and drive air outlet slit 59, from air compressor 60 and by thering is the compressed air of the pipeline L16 of valve 61, from driving air intake 58 to enter, from driving air outlet slit 59 to be supplied to the air feed path 44 of transfer valve 43 by pipeline L17.
In addition, 1 fluid chamber 56 is provided with and controls air outlet slit 62, by pipeline L18, is communicated in three-way valve 52, further by pipeline L19, is communicated in control valve 53.2 fluid chamber 57 arrange and control air intake 63, by pipeline L21, are communicated in control valve 53.Adjuster 55, by adjusting the position of valve body 54, the adjustable flow that passes through the mobile driving air of the 1st fluid chamber 56.At control valve 53, adjuster 64 is set, the operating pressure of adjustable control valve 53.At three-way valve 52, switch 65 is set, the stream of changeable three-way valve 52 and discharge control air, and control valve 51 can be reset (reset).
In above-mentioned structure, compressed air from air compressor 60, by valve 61, carry out Flow-rate adjustment, by pipeline L16, import the driving air intake 58 of control valve 51, from driving air outlet slit 59 to be supplied to the air feed path 44 of the transfer valve 43 of pump 30 by pipeline L17.In transfer valve 43, will drive air flue 37a, 37b to switch alternately, will drive air to import alternately, drive air chamber 36a, 36b, at this moment from the opposing party's driving air flue 37b, 37a, will drive air to discharge towards Bas Discharged path 45.Thus, make barrier film 33a, 33b pass through main shaft 35 towards equidirectional movement, from pipeline L14, mixture slurry is sucked pressurization, the resin that passes through ion-exchange unit U from pipeline L15 imports path 3 importing containers 1.
In Fig. 3, demonstrate, pump 30 will drive air to be imported and driven air chamber 36b by driving air flue 37b from transfer valve 43, and will drive the driving air of air chamber 36a from driving air flue 37a to pass through the state that Bas Discharged path 45 is discharged toward system.Now, drive the driving air of air chamber 36a to be discharged from, and make barrier film 33a toward midfeather 34 side shiftings, make thus the slurry that the mixture slurry of mixing channel 23 enters pump 30 from pipeline L14 suck path 41, by check-valves 38a, be inhaled into pump chamber 32a.Barrier film 33b can thus by the mixture slurry pressurization in pump chamber 32b, and enter slurry feed path 42 from check-valves 39b toward pump chamber 32b side shifting at the same time, and the resin importing path 3 that passes through ion-exchange unit U from pipeline L15 imports container 1.At this moment due to check-valves 39a is closed, the mixture slurry of slurry feed path 42 can not enter pump chamber 32a.
Then transfer valve 43 switches, and will drive air to drive air chamber 36a from driving air flue 37a to import, and will drive the driving air of air chamber 36b by driving air flue 37b to discharge toward system by Bas Discharged path 45 from transfer valve 43.Make thus barrier film 33a, 33b toward the right-hand movement of Fig. 1, from mixing channel 23, enter the mixture slurry of the slurry suction path 41 of pump 30, by check-valves 38b, be inhaled into pump chamber 32b.By the mixture slurry pressurization in pump chamber 32a, from check-valves 39a, enter slurry feed path 42 at the same time, from pipeline L15, import the container 1 of ion-exchange unit U.So, by the mutual stream that drives air and mixture slurry that switches of transfer valve 43, can proceed mixture slurry towards the importing of container 1.
Ion exchange resin from the mixture slurry of pipeline L15 importing container 1 is filled in container 1, the water of carrying under one's arms is separated by the 1st filter 4a and the 2nd filter 5a, by expansion joint 7,8, joint 9,10, from outside stream 11,12, discharge, form thus ion exchange resin packed layer 2.At the filling initial stage of ion exchange resin, the ion exchange resin packed layer 2 in container 1 is few, under the state existing in water layer volume, owing to carrying under one's arms, water can be separated and discharged, mixture slurry can be imported successively, therefore, the switching by transfer valve 43 is repeatedly to carry out the supply of mixture slurry.
Along with the progress of the filling of ion exchange resin, when in container 1 all fill ion exchange resin packed layer 2 time, mixture slurry becomes and cannot enter in container 1.Thus, the pressure that spues of pump 30 uprises, corresponding therewith, and the load that puts on barrier film 33a, 33b becomes large, therefore drives air pressure to uprise.In control valve 51, a part for driving air in the 1st fluid chamber 56 is as controlling air, from controlling air outlet slit 62, by pipeline L18, be supplied to three-way valve 52, further by pipeline L19, be supplied to control valve 53, driving air pressure to arrive the time point of authorized pressure, control valve 53 can be opened.
By opening control valve 53, control air and by pipeline L21, control air intake 63, enter the 2nd fluid chamber 57 from control valve 53, make valve body 54 toward the right-hand movement of Fig. 1,56 sealings of Jiang 1 fluid chamber.Stop thus 30 supplies to pump and drive air, releasing acts on the driving air pressure of pump 30 and stops driving pump 30.Thus, pump 30 stops container 1 supply mixture slurry.In this stage, because container 1 is the state of filling, at the ion exchange resin packed layer 2 of the interior formation specified volume of container 1.
So carry out, at the driving air pressure of pump 30, arrive the time point of authorized pressure, releasing acts on the driving air pressure of pump 30 and stops driving pump 30, though thus can be at the resinbed 2 of the interior formation specified volume of container 1, but still have the inhomogeneous situation of packed density, therefore in padding once and after stopping driving pump 30, for example, after placing the stipulated time (1～10 minute), start once again driving pump 30 and supply mixture slurry, when driving air pressure to arrive once again the time point of authorized pressure, releasing acts on the air pressure of pump 30 and stops driving pump 30, can form thus the ion exchange resin packed layer 2 of uniform filling density.
When starting driving pump 30 once again, by being arranged at the switch 65 of three-way valve 52, switch the stream of three-way valve 52, with the control Bas Discharged in Jiang 2 fluid chamber 57, make thus the valve body 54 of control valve 51 reset and control valve 51 is reset.By allowing pump 30 stop and placing, can remove the filling strain of the ion exchange resin packed layer 2 in container 1, to form uniform ion exchange resin packed layer 2, and by water layer separation and at the interior formation resin of container 1 inflow space, at this moment control valve 51 is reset and started once again driving pump 30, to start once again the interior supply mixture slurry of container 1.Driving air pressure to arrive once again the time point of authorized pressure, control valve 53 to be opened, releasing acts on the air pressure of pump 30 and stops driving pump 30.Can form thus the more uniform ion exchange resin packed layer 2 of packed density.
After so carrying out forming ion exchange resin packed layer 2, or the situation of not being strict with for the loading of ion exchange resin packed layer 2, omit padding repeatedly, then, container 1 is changed and carried out the formation of ion exchange resin packed layer 2 for next container 1.The replacing of container 1, be at connector 4b, 5b from expansion joint 7,8 separation, be replaced with new container 1.After being replaced with new container 1, by switch 65, switch the stream of three-way valve 52 and control valve 51 is reset, thus the 1st fluid chamber 56 supplies of control valve 51 are driven to air, start once again by 30 pairs of new containers of pump, 1 supply mixture slurry, with aforementioned similarly filling ion-exchange resin, and carry out the formation of ion exchange resin packed layer 2.
The operating pressure of control valve 53, driving air pressure while also allowing control valve 53 open is the pressure of setting within the scope of 0.2～0.7MPa, by adjuster 64, this pressure can be adjusted to and easily carry out the padding of resin and can avoid resin fragmentation and the pressure of uniform filling.In this situation, need not measure or adjust the pressure that spues of pump 30, as long as regulate the operating pressure of control valve 53, can closed control valve 51 and remove the air pressure that acts on pump 30, to stop driving pump 30.
Below, embodiment and the comparative example of 8th～11 technical schemes are described.
Embodiment 2～6
In the device shown in Fig. 3, in container 1 (volume 70L), setting pressure at pump 30 is to fill mixture slurry under 0.294MPa, to form ion exchange resin packed layer 2, this mixture slurry is by cationic ion-exchange resin CRM (Kurita Water Industries Ltd's system, trade mark) and the hybrid resin that mixes at 1: 1.6 with Capacity Ratio of anion exchange resin KR (Kurita Water Industries Ltd's system, trade mark) to be formed with around the hybrid resin of state (not yet standing sedimentation and allow the state of water separation) of water and the mixture slurry mixing at 80: 20 with Capacity Ratio of water.When pump 30 arrives 0.294MPa and after stopping, placing 10 minutes, at pump 30, set pressure once again and drive under 0.294MPa, and fill.Five containers 1 are sequentially changed, filling the results are shown in table 1.
Table 2
| Layer capacity (L) | Too much or in shortage (L) | |
| Embodiment 2 | 70.5 | 0.5 |
| |
72.0 | 2.0 |
| |
71.5 | 1.5 |
| |
71.0 | 1.0 |
| |
70.5 | 0.5 |
According to the result of table 2, the mean value too much or in shortage of the resinbed 2 in container 1 is+1.1L, with respect to the Capacity Ratio of datum quantity (70L), is 1.57%, is all belong to too much situation and there is no not enough example, and it is qualified to be judged to be.
Comparative example 2～4
Use container and the mixture slurry identical with embodiment 2～6, at the resin of the container 1 shown in Fig. 3, import path 3 funnel is set, use beaker that mixture slurry is poured into until fill container 1, at container 1, form resinbed 2.Three containers 1 are sequentially changed and filled, and it the results are shown in table 3.
Table 3
| Layer capacity (L) | Too much or in shortage (L) | |
| Comparative example 2 | 65 | -5 |
| Comparative example 3 | 60 | -10 |
| Comparative example 4 | 63 | -7 |
According to the result of table 3, in each comparative example, the capacity of the resinbed 2 in container 1 all presents the deficiency within the scope of 5～10L, and deviation is very large.
8th～11 technical schemes, can be used in the container that the ion interchange unit at Water Purifiers, Ultrapure Water Purifiers, wastewater treatment equipment, ionic adsorption device etc. uses, the hybrid resin of the hybrid resin of cationic ion-exchange resin, anion exchange resin, these resins or these resins and other resins is filled in container to form in the method for resinbed.
Though be to use specific technical scheme to understand the present invention, those skilled in the art can understand, can carry out various changes not departing under the intent of the present invention and scope.
In addition, the application makes according to the Japanese application for a patent for invention (No. 2009-266401, Japanese Patent Application) of the Japanese application for a patent for invention (No. 2009-155660, Japanese Patent Application) of application on June 30th, 2009 and application on November 24th, 2009, at this, its integral body is applied to the present invention.
Claims (12)
1. the preparation method of an ion interchange unit, this ion interchange unit is in the Ultrapure Water Purifiers of the ultra-pure water for the manufacture of below metal concentration 0.1ppt, and be the ion exchange resin after refinement treatment to be filled in to container be made, it is characterized in that
Ion exchange resin is carried out to refinement treatment and to filling step, transfers not contact the state of atmosphere via pipe arrangement not contact the state of atmosphere,
The filling step that ion exchange resin after refinement treatment is filled in to this container is to carry out in cleaniliness classs is the dust free room below 10000.
2. the preparation method of ion interchange unit as claimed in claim 1, wherein, be set up in parallel the purification apparatus that carries out refinement treatment is a plurality of, the ion exchange resin of only processing one species by a purification apparatus, different types of ion exchange resin is processed by different purification apparatus.
3. the preparation method of ion interchange unit as claimed in claim 2, wherein, after the ion exchange resin of plural kind is refined by different purification apparatus respectively, by different measuring tanks, measure, then, in mixing channel mixing, be filled in aforementioned container.
4. the preparation method of ion interchange unit as claimed any one in claims 1 to 3, wherein, for the ion interchange unit after filling ion-exchange resin, in aforementioned dust free room, carry out ultra-pure water water flowing, analyze outflow water from ion interchange unit to check ion interchange unit.
5. the preparation method of ion interchange unit as claimed in claim 4, wherein, the analysis of aforementioned outflow water is to carry out in cleaniliness classs is the high-cleanness, high dust free room below 1000.
6. the making apparatus of an ion interchange unit, this ion interchange unit is in the Ultrapure Water Purifiers of the ultra-pure water for the manufacture of below metal concentration 0.1ppt, and be the ion exchange resin after refinement treatment to be filled in to container be made, it is characterized in that, it possesses:
Ion exchange resin is carried out not contact the state of atmosphere refinement treatment refining plant,
By the refining ion exchange resin of this refining plant via pipe arrangement with the transfer device that do not contact the state of atmosphere and transfer to filling step and
The cleaniliness classs that is used for carrying out the ion exchange resin after refinement treatment is filled in the filling step of this container is the dust free room below 10000.
7. the making apparatus of ion interchange unit as claimed in claim 6, wherein, be set up in parallel the purification apparatus that carries out refinement treatment is a plurality of, the ion exchange resin of only processing one species by a purification apparatus, different types of ion exchange resin is processed by different purification apparatus.
8. the making apparatus of ion interchange unit as claimed in claim 7, wherein, the ion exchange resin of plural kind respectively after different purification apparatus is refined, is measured by different measuring tanks, then, in mixing channel mixing, be filled in aforementioned container.
9. the making apparatus of the ion interchange unit as described in any one in claim 6 to 8, wherein, it possesses testing fixture,
This testing fixture for the ion interchange unit after filling ion-exchange resin, carries out ultra-pure water water flowing in aforementioned dust free room, analyzes outflow water from ion interchange unit to check ion interchange unit.
10. the making apparatus of ion interchange unit as claimed in claim 9, wherein, it possesses: the cleaniliness classs that is used for carrying out the analysis of aforementioned outflow water is the high-cleanness, high dust free room below 1000.
11. 1 kinds of ion interchange units, is characterized in that, it is the ion interchange unit of manufacturing by the method described in any one in claim 1 to 5.
12. 1 kinds of ion interchange units, is characterized in that, it is by the ion interchange unit of the device fabrication described in any one in claim 6 to 10.
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2009-155660 | 2009-06-30 | ||
| JP2009155660A JP5391874B2 (en) | 2009-06-30 | 2009-06-30 | Manufacturing method of ion exchanger |
| JP2009266401A JP5407801B2 (en) | 2009-11-24 | 2009-11-24 | Method for forming ion exchange resin layer |
| JP2009-266401 | 2009-11-24 | ||
| PCT/JP2010/060649 WO2011001871A1 (en) | 2009-06-30 | 2010-06-23 | Ion-exchange device, process and equipment for producing same, and method and device for forming ion-exchange resin layer |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310252891.5A Division CN103342404B (en) | 2009-06-30 | 2010-06-23 | Ion-exchange device, process for producing same and equipment, and method for forming layer of ion-exchange resin and device thereof |
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| Publication Number | Publication Date |
|---|---|
| CN102471098A CN102471098A (en) | 2012-05-23 |
| CN102471098B true CN102471098B (en) | 2014-01-29 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201310252891.5A Active CN103342404B (en) | 2009-06-30 | 2010-06-23 | Ion-exchange device, process for producing same and equipment, and method for forming layer of ion-exchange resin and device thereof |
| CN201080029277.7A Active CN102471098B (en) | 2009-06-30 | 2010-06-23 | Ion-exchange device, process and equipment for producing same, and method and device for forming ion-exchange resin layer |
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| CN201310252891.5A Active CN103342404B (en) | 2009-06-30 | 2010-06-23 | Ion-exchange device, process for producing same and equipment, and method for forming layer of ion-exchange resin and device thereof |
Country Status (4)
| Country | Link |
|---|---|
| KR (2) | KR101682874B1 (en) |
| CN (2) | CN103342404B (en) |
| TW (2) | TWI551336B (en) |
| WO (1) | WO2011001871A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP5413587B2 (en) * | 2009-10-22 | 2014-02-12 | 栗田工業株式会社 | Ultrapure water production method and production apparatus for ion exchange resin purification equipment |
| CN111068361B (en) * | 2018-10-22 | 2022-02-11 | 中国石油化工股份有限公司 | Caprolactam ion exchange device and regeneration method thereof |
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|---|---|---|---|---|
| CN2540405Y (en) * | 2002-04-29 | 2003-03-19 | 昝保真 | Ion exchanger for producing ultrapure water |
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| JP3221001B2 (en) * | 1991-07-12 | 2001-10-22 | 三菱化学株式会社 | Purification method of basic anion exchange resin for water treatment |
| JPH0920505A (en) * | 1995-07-03 | 1997-01-21 | Sumitomo Chem Co Ltd | Purification of hydrogen peroxide aqueous solution |
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| JP3994210B2 (en) * | 1996-01-30 | 2007-10-17 | 三菱化学株式会社 | Purification method of ion exchange resin |
| JP2000203811A (en) * | 1999-01-06 | 2000-07-25 | Sumitomo Chem Co Ltd | Packed column and purification of aqueous hydrogen peroxide using the same packed column |
| JP2001286770A (en) * | 2000-04-04 | 2001-10-16 | Idemitsu Petrochem Co Ltd | Preparation method of fixed bed of acidic cation exchange resin for bisphenol production |
| JP3961199B2 (en) * | 2000-07-14 | 2007-08-22 | 日本電工株式会社 | Ion exchange resin transfer container and ion exchange resin transfer device |
| JP2002221160A (en) * | 2001-01-26 | 2002-08-09 | Yamada Corporation | Pump device |
| US6883222B2 (en) * | 2002-10-16 | 2005-04-26 | Bioject Inc. | Drug cartridge assembly and method of manufacture |
| JP2004299738A (en) * | 2003-03-31 | 2004-10-28 | Daiwa Can Co Ltd | Environmental monitoring apparatus of aseptic molding/filling system |
| JP4508701B2 (en) * | 2004-04-05 | 2010-07-21 | オルガノ株式会社 | Water treatment system for electronic component parts manufacturing equipment |
| JP4587694B2 (en) * | 2004-04-07 | 2010-11-24 | 旭化成ケミカルズ株式会社 | Method for separating and recovering amino acid and iminodicarboxylic acid |
| JP2007083132A (en) * | 2005-09-21 | 2007-04-05 | Dow Global Technologies Inc | Method for reducing elution of organic material from anion exchange resin |
| KR100741417B1 (en) * | 2005-11-30 | 2007-07-23 | 한국원자력연구원 | Loading machines for ion exchange resin |
| CN2860612Y (en) * | 2005-12-31 | 2007-01-24 | 深圳市水苑水工业技术设备有限公司 | Ion exchanging resin nondestructive transportation, loading and unloading, regenerating device |
| JP4195896B2 (en) | 2006-05-15 | 2008-12-17 | 株式会社ヤマダコーポレーション | Fluid pressure control device for pump device |
| US8476324B2 (en) * | 2007-04-19 | 2013-07-02 | Kurita Water Industries Ltd. | Method for manufacturing anion exchange resin, anion exchange resin, method for manufacturing cation exchange resin, cation exchange resin, mixed bed resin, and method for manufacturing ultrapure water for washing electronic component material |
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| CN2540405Y (en) * | 2002-04-29 | 2003-03-19 | 昝保真 | Ion exchanger for producing ultrapure water |
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Also Published As
| Publication number | Publication date |
|---|---|
| WO2011001871A1 (en) | 2011-01-06 |
| KR101794500B1 (en) | 2017-11-07 |
| CN102471098A (en) | 2012-05-23 |
| CN103342404B (en) | 2015-01-28 |
| TW201127491A (en) | 2011-08-16 |
| TW201501770A (en) | 2015-01-16 |
| CN103342404A (en) | 2013-10-09 |
| KR20160073428A (en) | 2016-06-24 |
| TWI551336B (en) | 2016-10-01 |
| KR20120039524A (en) | 2012-04-25 |
| TWI494166B (en) | 2015-08-01 |
| KR101682874B1 (en) | 2016-12-06 |
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