JP3197199B2 - Resin outflow prevention device for adsorption tower - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a resin tower (adsorption tower) for filtering treatment liquids and the like of various plants, a filtration tower, and the like. It relates to a prevention device.

[0002]

2. Description of the Related Art FIG. 6 is a block diagram of a conventional filtering apparatus for processing an etching solution or the like.
Shows an example of net layer filtration, and (c) shows an example of slit layer filtration.
In the figure, (a) shows that the liquid 4 passes through the upper sand filtration layer 20,
After the filtration, the resin enters the adsorption tower 21, and the resin 22 and the sand layer 2 in the tower.
3 and is discharged as a processed liquid 24. (B)
The liquid 4 passes through the upper net layer 30, and the liquid after passing through the net enters the adsorption tower 31, passes through the resin 32 and the net layer 33 in the tower, and is discharged as a treated liquid 34. (C) is liquid 4
Through the upper slit layer filtration 40, and after filtration, the adsorption tower 41
Then, it passes through the resin 42 and the slit layer 43 in the tower, and is discharged as a treated liquid 44.

Conventionally, sand filtration, net filtration, and filtration of dispersed solids using fine slits have been carried out to prevent outflow from the system. However, the sand filtration layer increases the weight of the apparatus and causes strong corrosive liquids. In the case of, sand components may elute and impurities may be mixed into the product liquid.In addition, since the sand particles are fixedly filled, the pressure drop increase due to the solid dispersion deposited between the particles is large. Become.

In the case of mesh filtration and slit filtration, the thickness of the filtration layer cannot be increased, and flat filtration is performed, so that the pressure loss tends to increase, and there is no method for preventing membrane breakage. FIG.
As shown in (1), the liquid flow is basically in one direction, and in order to flow an alternating current, it is necessary to provide upper and lower filtration devices, which is extremely disadvantageous in a cycle operation such as adsorption / desorption.

[0005] Adsorption proceeds from the upper layer to the lower layer, and an adsorption zone is formed. Therefore, it is reasonable to desorb the resin by an upward flow. However, efficient measures can be taken unless measures are taken to prevent resin from flowing out. Absent. However, it is preferable to prevent the consolidation by the upstream / downstream operation with respect to the increase in the pressure loss and the like. The upper surface cannot be restrained due to resin expansion and contraction.

[0006]

SUMMARY OF THE INVENTION The aforementioned conventional sand filtration,
In the case of using a highly corrosive, high-viscosity, high-density liquid such as an etchant in a net filtration or slit filtration apparatus, there are the following problems.

(1) The resin flows out of the tower due to the flow of the liquid, and the particles secondarily adversely affect instruments and the like.

(2) Outflow of the resin not only results in loss of the resin, but also causes a reduction in the adsorption capacity, which leads to a reduction in performance.

(3) As in the case of conventional filtration, the pressure loss rises due to the formation of dispersed solids deposited on the surface of the filter membrane,
Good filtration characteristics cannot be obtained.

[0010]

The present invention provides the following means in order to solve such a problem.

(1) an upper liquid inflow / outflow pipe through which liquid flows in and out of the upper part of the tower; a liquid separation pipe communicating with the upper liquid inflow / outflow pipe; A bag-like net wrapped around the mesh with a mesh-woven net;
An ion-exchange resin filled in the tower below the bag-like net; and a lower liquid inlet / outlet pipe through which liquid flows in and out of the lower part of the tower. At the time of adsorption, a treatment containing metal chloride ions is performed. The liquid to be flowed in from the lower liquid inflow / outflow pipe, the ion component is adsorbed by the ion exchange resin, and the liquid flows from the outer periphery of the bag-like net toward the center, and the bag-like net and the synthetic resin pellet The solids dispersed in the liquid are filtered and flowed out of the upper liquid inflow / outflow pipe through the liquid separation pipe, and at the time of desorption, the liquid is flowed in from the upper liquid inflow / outflow pipe, and the synthesis is performed from the liquid separation pipe. Pass the resin pellets and the bag-shaped net, flow into the ion exchange resin while separating the solids attached to the outer periphery of the bag-shaped net,
A resin outflow prevention device for an adsorption tower, wherein an adsorption capture component is collected and discharged from the lower liquid inflow / outflow pipe.

(2) In the above (1), the mesh woven net is made of any one of Saran, polyethylene and polypropylene, and the line distance of the net is 50 μm to 2 μm.
An apparatus for preventing resin from flowing out of an adsorption tower, which has a range of 50 μm.

(3) In the above (1) or (2),
The average particle diameter of the ion exchange resin is 450 μm to 500 μm.
The synthetic resin pellets have a diameter of 1 to 10 times the average particle diameter of the ion-exchange resin, and the resin pellets are prevented from flowing out of the adsorption tower.

(4) The resin outflow prevention device for an adsorption tower according to (1) or (2), wherein a large number of pleats are provided around the mesh woven net bag.

According to the present invention, in the method (1), first, in the adsorption step, the treatment liquid first flows in from the lower liquid inflow / outflow pipe, enters the ion exchange resin as an ascending flow, and enters the liquid. The contained metal ions, etc. are adsorbed and captured by this resin, and then the solid dispersion (ion exchange resin particles) in the liquid is filtered through a bag-like net made of a mesh woven net having a large outer surface. While passing through the particle space of the synthetic resin pellets filled in the bag, the solid matter is further filtered, separated and purified, and the purified treated water flows out of the upper liquid inflow / outflow pipe through the liquid separation pipe.

In this device, the filtration surface can be regenerated by the desorption process. That is, in the adsorption step, the liquid becomes an upward flow from the outer periphery of the bag-shaped net toward the center of the bag, but in the desorption step, the liquid flows in from the upper liquid inflow pipe, and the synthetic resin pellets are separated from the liquid separation pipe. After passing, the flow becomes a downward flow that changes from the central portion of the bag-shaped net to the outer periphery, and the solid particles trapped on the outer peripheral surface of the bag-shaped net fall off to regenerate the filtration surface. The treated liquid passes through the ion exchange resin again to desorb and recover the adsorbed components, and flows out of the column from the lower liquid outflow / inlet pipe.

On the other hand, in the adsorption step, even if the resin particles or crushed pieces smaller than the interline diameter of the bag-like net pass through the net, the synthetic resin pellet layer is not removed while passing through the synthetic resin pellet gap filled in the bag. Is trapped and removed as a filtration layer and purified, so that no resin flows out of the tower system.

In (2), the mesh net is made of Saran, polyethylene or polypropylene, the distance between the lines is in the range of 50 μm to 250 μm, and the particle size distribution of the ion exchange resin is as large as about 250 μm to 800 μm. And does not flow out through the minimum particle size of the resin. Even if the ion exchange resin tries to flow out, this mesh net prevents this, so that the effect of (1) is ensured.

In (3), the particle size of the synthetic resin pellet is 1 to 10 times the value of the ion exchange resin. According to the experimental results, when the synthetic resin pellet having a particle size in this range is used, The pressure loss rise is small, and the amount of the ion exchange resin flowing out from the packed bed of synthetic resin pellets is also small. This effect and the effect of preventing the resin from flowing out of the system are ensured by both of the effect of the mesh net.

Further, in (4), the operation of (1)
In addition to the effect, the area through which the liquid passes increases because there are many folds around the mesh woven net bag,
This reduces the filtration surface speed during liquid passage to prevent an increase in pressure loss and disperses the accumulation of dispersed solids, thereby increasing the effect of filtration.

[0021]

Embodiments of the present invention will be specifically described below with reference to the drawings. FIG. 1 is a longitudinal sectional view of a resin outflow prevention device for an adsorption tower according to an embodiment of the present invention, FIG. 2 is a sectional view taken along line AA, and FIG.
It is B sectional drawing. In these figures, 1 is an adsorption tower,
Inside thereof is a bag-like net 13 composed of a mesh layer 10, in which synthetic resin pellets 9 are filled.
As shown in FIGS. 2 and 3, the bag-like net 13 has a pillow shape having a large number of pleats 11 around the periphery in order to increase the filtration area and suppress pressure loss and clogging of the ion exchange resin. ing.

A liquid separating pipe 8 is provided at the center of the bag-shaped net 13, and the liquid separating pipe 8 has a large number of outflow / inflow holes 7, and allows liquid to flow into and out of the tower. The liquid inlet / outlet pipe 5 communicates with the liquid separating pipe 8, and the liquid 4 flows in from the outside at the time of desorption and the liquid 4 flows out at the time of adsorption, as described later. Further, an inner ring resin pellet layer 12 is arranged around the separation pipe 8,
The inner layer resin pellet 12 and the synthetic resin pellet 9 constitute the mesh layer 10.

Reference numeral 2 denotes an ion exchange resin provided in the lower part of the adsorption tower 1 having such a structure, reference numeral 3 denotes a net layer (multi-layer filtration layer) thereunder, and reference numeral 6 denotes a processing liquid flowing into and out of the lower part of the vessel 15. is there. Note that the synthetic resin pellets 9 are made of a bag-like net 13.
And between the bag-like net 13 and the container 15.

In such a configuration, a net layer 3 serving as a multilayer filtration layer is provided at the bottom of the vessel 15 of the adsorption tower 1, and the ion exchange resin 2 is filled thereon. In the adsorption step, as shown by the white arrow in FIG. 1, the processing liquid 6 flows upward from the lower part of the tower in an upward flow, and while passing through the layer of the ion exchange resin 2, the processing liquid 6 After the components are adsorbed and captured, they are discharged from the liquid separation layer 8 and the liquid inflow / outflow pipe 5 through the outflow / inflow hole 7 through the bag-like net 13 and the resin pellet 9.

In the desorption step (downward flow) following the adsorption, the desorption liquid is supplied from the liquid inflow / outflow pipe 5 as indicated by the black arrow in the drawing, and is supplied to the separation pipe 8 in the opposite manner to the adsorption step. From the outflow / inflow holes 7, through the resin pellet layer 9, through the eyes of the bag-like net 13, the fine particles are gradually supplied to the layer of the ion exchange resin 2, and the components to be treated that have been adsorbed and captured are desorbed. Collected and discharged from the bottom of the tower.

In the desorption step, the mesh layer 10 filters solids in the desorption liquid (work water) to prevent the solids from flowing into the ion exchange resin 2 layer. It functions to prevent the ion exchange resin 2 from flowing out of the tower, which is the main object of the invention.

This function is to prevent expensive resin from flowing out of the system and to keep the resin layer at a constant height. It is important to prevent coming.

For this reason, as shown in FIG. 3, the mesh layer 10 has a large filtering area to reduce pressure rise caused by clogging of the ion exchange resin 2 and solids.
With a structure.

Further, in the adsorption step, the processing liquid 6 is short-circuited from the mesh layer 10 to the liquid separating pipe 8, and the liquid is discharged.
An inner ring resin pellet 12 surrounding the separation pipe 8 is arranged so that the ion exchange resin 2 contained in the liquid is not discharged. In the adsorption step (upward flow), the inner ring resin pellets 12 are important for capturing resin particles contained in the highly viscous treatment liquid 6 and preventing the resin particles from flowing out.

In particular, when the ion exchange resin 2 is crushed for some reason and a large number of fragments are contained in the treatment liquid 6, the inner ring resin pellets 12 are very important for preventing the resin from flowing out. . This inner ring resin pellet 12 is
Proceeding to the desorption step, when the liquid flow reverses and the liquid flows downward, the solids floating in the working water are filtered as described above, and the solids flow into the layer of the ion exchange resin 2. The main purpose is to prevent this from happening.

On the other hand, in the conventional apparatus, even if various measures are taken, it is necessary to improve crushing, increase in pressure loss, apparatus weight, maintenance and the like, and it is difficult to suppress outflow of resin.

FIG. 4 shows the results of the effect of suppressing the outflow of the ion exchange resin 2 depending on the diameter of the resin pellet 9. FIG. 4 shows the test results performed to determine the optimum diameter of the resin pellet 9.
A predetermined resin pellet was filled to 80 mm, the ion-exchange resin was filled to 600 mm, and the liquid was allowed to flow upward from below. The pressure loss of the five glass columns after the lapse of time and the amount of ion-exchange resin in the effluent were measured. Things.

This result cannot be compared as it is because the test conditions are slightly different from the data of the experimental result 1 to be described later. However, as shown in the figure, the resin pellet has a small increase in pressure drop when the ion exchange resin diameter is 1 to 10 times the diameter of the ion exchange resin. It can be seen that the outflow of the grains is also small.

In FIG. 4, when the pellet diameter is small, the pressure loss of the ion-exchange resin packed bed increases with time, and the
It reaches 4000 mm at 00Hr. On the other hand, the ion exchange resin outflow increases when the particle size ratio exceeds 10, and initially exceeds 10 mg / Hr, and the ion exchange resin gradually stays in the pellet space, and the outflow decreases, but cannot be reduced effectively. It is shown that. From these relations, the diameter of the pellet can be optimally selected to be 1 to 10 times the diameter of the ion exchange resin.

On the other hand, the line-to-line distance of the net is also important for suppressing the outflow of the ion exchange resin. FIG. 5 shows the test results of the net conditions and the pressure loss rise. Since the net condition is particularly related to the increase in pressure drop due to clogging of the ion exchange resin particles, this point was tested. It is known that in a test with a mesh of 32 μm between lines, the pressure loss sharply increased in a test of only 264 Hr, and the fine particles and crushed pieces coexisting in the ion exchange resin particles were clogged, causing the pressure loss to increase.

Based on the results shown in FIG. 5, it is preferable to select an optimal net line distance between 50 and 250 μm. Up to 2
The reason for setting the particle size to 50 μm is to prevent the resin from having a particle size distribution of about 250 to about 800 μm and having the minimum particle size flowing out.

Next, an experiment was conducted on the resin outflow prevention device of the adsorption tower having such a configuration under the following conditions.

[Experimental result 1]; The filtration layer was compared with the conventional sand filtration, net filtration and the method of the present invention.
m, mesh bag diameter 300mm cylindrical, resin pellet 2.5
Filling 3.5 liters of polypropylene (pp) pellets with a diameter of mm, number of folds in the mesh bag, liquid passage surface area about 0.5 m ² , liquid inflow / outflow pipe 30 mmφ, length 200 mm, outflow / inflow hole diameter 2 mm Approximately 150 inlet / outlet pipes were provided.

An anion exchange resin (representative diameter: 463 μm, maximum: 861 μm, minimum: 214 μm) is 500 mm high, 35 mm
The resin was packed in a 0 mmφ tower, and upstream and downstream were generated at a liquid flow rate of 2.5 m / sec, and the resin outflow was measured. A 10% ammonium sulfate solution was used as a simulated adsorption component.

Under these conditions, adsorption / desorption was performed 100 cycles, and the amount of resin flowing out and the pressure loss were measured. The results are shown in Table 1 below.

[0041]

[Table 1]

From the results shown in Table 1, the sand filtration method has a small resin outflow, but has a disadvantage that the pressure loss increases with time and impurities are eluted from the sand component. In the net filtration method, the pressure loss is small, but the resin outflow is remarkably large.

[Experimental Result 2]; Condition comparison was performed based on the data of Experimental Result 1. Table 2 shows the results.

[0044]

[Table 2]

In Table 2, regarding the resin diameter, the crushing and abrasion of the ion-exchange resin were slight in the method of the present invention together with the results of microscopic observation. However, in the sand filtration, numerous surface scratches and surface abrasion were observed. , And refined.

In Table 2 above, the planned apparatus weight ratio is the apparatus weight ratio obtained in the actual apparatus planned example of the processing liquid of 50 L / Hr, and is the ratio when the apparatus of the present invention is set to 1. From this weight ratio, it can be seen that the size of the apparatus is increased by the sand filtration method. The operability is also inferior to the sand filtration method compared to the method of the present invention. In addition, investigations after the experimental results showed that the method of the present invention was sound without clogging of a large amount of particles between mesh fibers.

[0047]

As specifically described above, the present invention relates to an upper liquid inflow / outflow pipe for inflow / outflow of liquid from the upper part of a column, a liquid separation pipe communicating with the upper inflow / outflow pipe, and a liquid separation pipe. A bag-like net filled with synthetic resin pellets around the periphery and wrapped around with a mesh-woven net, an ion-exchange resin filled in the tower below the bag-like net, and a lower liquid inlet / outlet pipe at the bottom of the tower were provided. The mesh woven net is made of Saran, polyethylene or polypropylene, and the distance between the lines is 50
μm to 250 μm range, the synthetic resin pellet diameter is 1 to 10 times the ion exchange resin,
Since the configuration in which the folds are provided around the mesh woven net is also provided, the following effects can be obtained.

(1) Even if the ion-exchange resin leaks from the mesh-woven net of the bag-like net, the synthetic resin pellets inside the net trap the ion-exchange resin particles and suppress the outflow from the system. Further, by arranging a large number of liquid flow holes smaller than the diameter of the synthetic resin pellet in the liquid separating pipe, it is possible to prevent resin outflow, pressure loss rise, and the like.

(2) Set the distance between the lines of the mesh woven net to 50
By setting the thickness in the range of ~ 250 µm, outflow of the ion exchange resin out of the system can be reliably prevented by the mesh woven net.

(3) By making the diameter of the synthetic resin pellet 1 to 10 times the particle diameter of the ion exchange resin, the effect of preventing the resin from flowing out of the synthetic resin pellet can be further enhanced.

(4) By forming the periphery of the bag of the mesh woven net in a fold shape, the liquid passage area is increased, and the filtration surface speed at the time of passage of the liquid is reduced so that an increase in pressure loss can be suppressed.

[Brief description of the drawings]

FIG. 1 is a longitudinal sectional view of a resin outflow prevention device for an adsorption tower according to an embodiment of the present invention.

FIG. 2 is a sectional view taken along line AA in FIG.

FIG. 3 is a sectional view taken along line BB in FIG. 2;

FIG. 4 shows experimental results of a resin outflow prevention device for an adsorption tower according to an embodiment of the present invention, showing the relationship between resin pellets / ion exchange resin and pressure loss.

FIG. 5 is a graph showing the relationship between the distance between mesh lines and pressure loss in an experimental result of the apparatus for preventing resin outflow of an adsorption tower according to an embodiment of the present invention.

6A and 6B are configuration diagrams of a conventional liquid filtration device, wherein FIG. 6A shows an example of sand layer filtration, FIG. 6B shows an example of net layer filtration, and FIG. 6C shows an example of slit layer filtration.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Adsorption tower 2 Ion exchange resin 3 Net layer (multilayer filtration layer) 4 Processing liquid 5 Liquid inflow / outflow pipe 6 Processing liquid 7 Outflow / inflow hole 8 Separation pipe 9 Synthetic resin pellet 10 Mesh layer 13 Bag-shaped net

──────────────────────────────────────────────────続 き Continuing on the front page Examiner Hiroshige Meshiro (56) Reference Jikken Sho 51-41081 (JP, Y2) (58) Field surveyed (Int. Cl. ⁷ , DB name) B01J 47/00-49 / 02 B01D 15/00-15/08 B01D 29/00-29/48 B01D 35/00-35/04 B01D 35/08-35/30 C02F 1/42 C02F 1/28

Claims (4)

(57) [Claims] 1. An upper liquid inflow / outflow pipe through which liquid flows in and out from the upper part of a column; a liquid separation pipe communicating with the upper liquid inflow / outflow pipe; A bag-shaped net whose periphery is wrapped in a bag shape with a mesh woven net; an ion-exchange resin filled in a tower below the bag-shaped net; and a lower liquid inflow / outflow pipe through which liquid flows in and out of the lower part of the tower. At the time of adsorption, a liquid to be treated containing metal chloride ions is caused to flow in from the lower liquid inflow / outflow pipe, the ion components are adsorbed by the ion exchange resin, and the liquid is transferred to the outer periphery of the bag-shaped net. Flowing toward the center, and the solid matter dispersed in the liquid with the bag-shaped net and the synthetic resin pellets is filtered and discharged from the upper liquid inflow / outflow pipe through the liquid separation pipe,
At the time of desorption, the liquid flows in from the upper liquid inflow / outflow pipe, passes through the synthetic resin pellets and the bag-shaped net from the liquid separation pipe, separates the solid matter adhered to the outer periphery of the bag-shaped net, and removes the ions. A resin outflow preventing device for an adsorption tower, wherein the resin flows into an exchange resin, and the adsorption trapping component is collected and discharged from the lower liquid inflow / outflow pipe. 2. The resin outflow of an adsorption tower according to claim 1, wherein the mesh woven net is made of any one of Saran, polyethylene and polypropylene, and the line distance of the net is in a range of 50 μm to 250 μm. Prevention device. 3. The ion exchange resin has an average particle size of 45.
The resin outflow prevention device for an adsorption tower according to claim 1 or 2, wherein the synthetic resin pellet has a diameter of 1 to 10 times the average particle diameter of the ion exchange resin. 4. The apparatus for preventing resin from flowing out of an adsorption tower according to claim 1, wherein a large number of pleats are provided around the bag of the mesh woven net.