JPH06134208A - Oil-water separation method and its device therefor - Google Patents

Abstract

PURPOSE:To provide a drain treatment method which can treat the drain by means of a device of small volume and also provide an oil-water separation device, the method to replace methods and devices heretofore available requiring a large volume such as the method in which an emulsified oil treating material of large volume composed of a non-woven cloth impregnated with a component destroying emulsified oil, forming rough and large oil grains and adsorbing is required, and the method in which ceramic grains of small capability for the oil-water separation of the emulsified oil are used and a ceramic layer of large volume is required as a result. CONSTITUTION:Separated oil equivalent to floating oil is adsorbed by an oil adsorption material 13 out of drain flowed from an inlet port 17, and oil emulsion is oil-water separated by a stearylamine layer 14 composed of laminated granular amine, and separated oil adheres to amine grains, and transparent water is deodorized and decolored by an active carbon layer 15, and discharged out of an outlet port 18 through an oil adsorption tank 16. As the capability of oil-water separation of oil emulsion in the stearylamine layer is large and also an intermediate cylinder 7 and an outer cylinder 5 are installed, an oil-water separation device, small as a system and of large capability, can be provided.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an oil / water separation method and apparatus thereof, and more particularly to an oil / water separation method and apparatus using amine.

[0002]

2. Description of the Related Art When water mixed with oil is put in a container, floating oil appears below the liquid open surface and dispersed oil is formed below it as an oil emulsion in the form of very small oil droplets. Such an oil-water mixture (hereinafter referred to as “drain”) occurs at the bottom of the compressed air tank of an air compressor, for example. An example of this drain treatment is an oil / water separator as shown in FIG. In the figure, the water separated in the oil / water separation tank 31 that measures the oil / water based on the difference in specific gravity is still about 500 ppm of raw water containing oil, and this raw water goes through the pipe to the oil adsorption tank 32. Oil water separation tank 3
The oil separated in 1 is recovered from the oil recovery pipe 33. The water flowing into the oil adsorption tank 32 still contains the separated oil and the oil emulsion, and is actually drain although the oil content is reduced. The oil adsorption tank 32 is filled with, for example, a nonwoven fabric strip, and when the drain passes through the nonwoven fabric strip, the separated oil in the drain adheres to the nonwoven fabric and is removed. The remaining oil emulsion proceeds to the oil decomposition tank 34 through the pipe. In the oil decomposition tank 34, a member having lipophilicity and oil adsorption,
For example, the emulsified oil treatment material disclosed in Japanese Utility Model Publication No. 58-14966 is filled, whereby an oil emulsion collects a large number of fine particles of oil to be coarse particles, is separated into oil and water, and the separated oil is The emulsified oil treatment material has a non-woven fabric as a constituent element and is adsorbed by this, and is discharged from the oil decomposition tank 34 as an oil content of, for example, 5 to 15 ppm. The oil adsorbing material in the oil adsorbing tank 32 and the emulsified oil treating material in the oil decomposing tank 34 are replaced when their processing capacity decreases as they are used.

Further, as shown in FIG. 4, there is an apparatus in which the oil adsorption tank 32 and the oil decomposition tank 34 are replaced with each other. In this case, the emulsified oil treatment material of the oil decomposition tank 34 is preferably one that does not adsorb oil after oil-water separation.

JP-A-58-1496 as an emulsified oil treatment material
According to the method disclosed in Japanese Patent No. 6, a nonwoven fabric is impregnated with the specified amine and laminated in a hollow columnar shape. Since the nonwoven fabric is impregnated with amine in the process, a large volume is required for the flow rate of the oil emulsion when the oil / water separator is configured so as to occupy a certain space as the emulsified oil treatment material. That is, the non-woven fabric does not have the ability to break the oil emulsion and coarsen the oil particles, but adheres the coarsened oil particles. On the other hand, the amount of amine impregnated into the non-woven fabric is small, and the ability to break the oil emulsion is low. In addition, such an emulsified oil treatment material is wound in a spiral shape in order to stack strip-shaped raw materials, but since the oil emulsion flows in the axial direction, the non-woven fabric portion through which the oil emulsion passes with almost no action. Occurs, and there is a problem that the content of the emulsified oil is large and the amount of amine is small and the drain flow distribution is not uniform.

The emulsified oil-treated material is wound as a raw material with a width of, for example, about 1 m, but when it is cut into small pieces and used as chips or strips, a remarkable improvement is observed.

In the above conventional example, the specific gravity type oil-water separator 3 is used.
1, the oil adsorption tank 32, and the oil decomposition tank 34 are independent devices. Therefore, a large space is indispensable for the device. On the other hand, from the environmental point of view, it goes without saying that it is preferable to treat and discharge the drainage even when the drainage of the small amount is drained by a small device. However, when the above-mentioned conventional example is used, the setting space is large, and in the above-described form, there is an inconvenience that it is extremely large as compared with a device that discharges drain.

In order to achieve miniaturization with such a device, useless space is removed, and the volume of either the oil adsorbent or the emulsified oil treatment material is preferably reduced. That is, it is necessary to increase the oil adsorption capacity or the oil-water separation capacity per unit volume.

Therefore, the present invention aims to provide a method for increasing the oil-water separation capacity per unit volume of the installation space of the oil-water separation apparatus and a device therefor, thereby providing a small-sized oil-water separation apparatus having a large processing capacity. There is.

[0009]

The present inventor tried an experiment as shown in FIG. As shown in FIG. 1 (a), a mixture of kerosene and water is used as 250 cc of raw water in a 300 cc beaker 41, and a liquid having an oil content of 350 ppm is agitated. 43 appears. Into this beaker 41, as shown in FIG. 1 (b), a stearylamine 10 mesh sieve (particle size of about 0.01-2.
If you add 0.1 g of (5 mm) particles, floating oil 42
Also, the oil in the oil emulsion 43 becomes a granular separated oil 44 and floats up, and the oil emulsion 43 becomes transparent water 45.
Next, as shown in FIG. 1C, the contents in the beaker 41 are transferred to the beaker 47 through the filter paper 46. Then, the separated oil 44 remains on the filter paper 46, and the transparent water 45 becomes beaker 47.
Housed in. Then, as shown in FIG. 1D, when the transparent water 45 in the beaker 47 is measured by an oil content measuring device, the oil content is 15 pp.
It was m.

Considering the above points, it can be seen that stearylamine not only destroys the oil emulsion 43 to turn water into oil, but also adsorbs oil separated from the oil emulsion 43. The present invention has been made by paying attention to the above points, and the above problems can be solved by the following means.

A first aspect of the present invention is a drain treatment method in which a member for treating oil is housed in a closed tank, and a drain is passed through the member for treating oil to remove oil in the drain. The member to be treated is a method for separating oil and water characterized in that granular amine is layered.

The second invention of the present invention is the oil-water separation method according to the first invention, wherein the granular amine is stearylamine having a particle size of about 0.01 to 2.5 mm.

According to a third aspect of the present invention, an intermediate cylinder having a cross section smaller than that of the sealed case is housed in a cylindrical sealed case with a space between the sealed case and one end of the sealed case. The inside of the middle cylinder communicates with the outside of the middle cylinder on the other end plate side of the closed case while the other end of the middle cylinder is fixed to the plate, and the inside of the middle cylinder and the outside of the closed case on the one end plate side of the closed case. A port that communicates with the inside of the sealed case and a port that communicates with the outside of the sealed case outside the middle cylinder are provided, and one of the ports is used as a drain inlet and the other is used as an outlet, and the middle cylinder is provided between the drain inlet and the drain outlet. A space between the inner and outer cylinders and the closed case is filled with an oil adsorbent and an emulsified oil treatment material as a member for treating drain, and the emulsified oil treatment material is a layer of granular amine, which is an oil-water separation. It is a device.

[0014]

Embodiments of the present invention will be described below with reference to the drawings.

[Example 1] In the same experiment as described above as a means for solving the problem, six materials of NO1 to NO6 were prepared and 250 cc of water was mixed with kerosene to prepare raw water.
The kerosene concentration was measured with a Shimadzu-manufactured POC-100 infrared type oil concentration meter (range 100). The experiment was as shown in Table 1. The second line following the sample NO in the heading column shows the kerosene concentration of the raw water, the third line shows the amount of stearylamine input, and the fourth line shows the oil concentration of the oil emulsion as a result of stirring stearylamine.

The amine used here is stearylamine C.
It has a total amine value of 203 to 213, a primary amine of 98% or more, and a freezing point of 47 to 53 ° C. and a hue of 120 APHA or less with ₁₈ H ₂₇ NH ₂ . The stearylamine used was a white wax-like solid at room temperature, which was crushed and sieved with a 10-mesh sieve to have a uniform particle size under the sieve.

Observation of the above experiment shows that the oil in the oil emulsion is separated and aggregated around the amine particles. Therefore, if the amine particles are layered and there is a suitable space between the amine particles, fine oil droplets in the oil emulsion are collected by the amine while adhering to the oil emulsion of the raw water, and are attached around the amine particles. If the amine particles are collected, there is a suitable space around the amine particles, so by layering the amine particles, the oil emulsion is separated into oil and water,
Wastewater with reduced oil content can be obtained. Here, the oil separation and adsorption treatment method of the oil emulsion can be embodied as a concrete device by accommodating the stearylamine particles in a layered manner in the oil decomposition tank 34 connected to the oil adsorption tank 32 as shown in FIG. In this case, the stearylamine particles are selected to have an appropriate particle size depending on the oil content of the oil emulsion, the properties of the contained oil, the flow rate and the like.

[Embodiment 2] Next, an embodiment of a small-sized and high-performance oil-water separator to which the above method is applied will be described. Figure 3
Also in the oil-water separator shown in FIG. 6, the granular amine layer can be obtained by filling the oil decomposition tank 34 with the granular amine described above. By doing so, even if the volume of the oil decomposing tank 34 is reduced, it is possible to provide the same ability as that in the case where the emulsified oil treatment material, soft ceramics, etc. in which the non-woven fabric is impregnated with amine is stored in a large tank. .

[Embodiment 3] In this embodiment, not only the granular amine is used, but also the oil adsorption tank and the oil decomposition tank are integrated so as to be downsized.

FIG. 2 is a vertical sectional view of the oil / water separator 1.
In the oil-water separator 1, a cylindrical outer cylinder 5 is fitted in circular grooves provided on the opposing surfaces of a disc-shaped upper end plate 2 and a lower end plate 3 via a sealing ring 4 such as an O ring. . Then, the through bolts and nuts 6 for inserting the end plates 2 and 3 are used to insert the end plates 2 and 3 into
The spaces are drawn together to form a sealed case. The middle cylinder 7 having a diameter smaller than that of the outer cylinder 5 is held at its upper end in contact with the upper end plate 2 or is fixed to the upper end plate 2, and its lower end is near the lower end plate 3, and the space inside the middle cylinder 7 The space between the outer cylinder 5 and the middle cylinder 7 communicates between the middle cylinder 7 and the lower end plate 3. A screen 11 such as a wire mesh or a perforated plate is fitted in the middle cylinder 7 so as to form a dispersion chamber 8 and a collecting chamber 9 inside the upper end plate 2, and is fixed to the middle cylinder 7 by welding or the like. An annular screen 12 is fitted between the cylinder 5 and the middle cylinder 7, and the end plate 2 not shown
It is fixed to the seat of the machine with screws. Below the screen 11, the middle cylinder 7 is filled with, for example, a piece of non-woven fabric of polypropylene, which is an oil adsorbent 13 in a compacted state. Middle cylinder 7
In the space below the lower end plate 3 and in the space below the space between the middle cylinder 7 and the outer cylinder 5, granular stearylamine is contained to form a stearylamine layer 14. This stearylamine has the same chemical structure as in Example 1,
It is the granular content under the sieve that has been sieved with 10 mesh. Middle cylinder 7
Granular activated carbon 15 is subsequently filled on the stearylamine layer 14 in the space between the outer cylinder 5 and the outer cylinder 5, and a fine piece of oil adsorbent 16 made of polypropylene non-woven fabric is filled thereon.
Directly above it is the screen 12. In the above, the activated carbon 15 is made of, for example, palm grains and has a particle size of 8 to 3
It is crushed to 2 mm and has methylene blue adsorption capacity (ml)
Is 120 to 150, the total area is 1100 m ² / g or more, the packing density is 0.4 to 0.46, the pH is 6.5 to 10, and the ash content is 2% or less. The upper chamber 2 has a dispersion chamber 8
An inlet port 17 communicating with the outside and an outlet port 18 communicating with the collecting chamber 9 are provided.

FIG. 1 shows a pipe for testing the oil-water separator 1, but this pipe is effective even if it is actually applied. The raw water tank 19 stores 5 liters of raw water 20. Suction pipe 22 connected to suction port 21a of pump 21
Is submerged in the raw water tank 19. Discharge port 21 of pump 21
The discharge pipe 23 connected to b is connected to the inlet port 17 via the flow control valve 24. A return pipe 25 branches from the discharge pipe 23, and a part of the discharged raw water is returned to the raw water tank 19 via a stop valve 26. The discharge pipe 23 is provided with a pressure gauge 27. The drain pipe 28 from the outlet port 18 is designed to flow toward the beaker 29.

In the above, the flow rate of the pump 21 is 20 liters / minute, the flow rate from the branch portion 23a to the inlet port 17 is 0.5 liters / minute, and the flow rate of the return pipe 25 is 19.
5 liters / minute, throttled with stop valve 26 and pressure gauge 21 is 0.2
It is set to indicate kgf / cm ² . Pump 2
When 1 is operated, the raw water 20 is sucked up from the raw water tank 19 and discharged from the pump 21 to the discharge pipe 23. By closing the flow control valve 24, the discharged raw water 20 returns to the raw water tank 19 through the entire return pipe 25 and the open stop valve 26. By this action, the raw water 20 is stirred,
The floating oil disappears and the raw water becomes a uniform oil emulsion, but floating oil occurs when it is left standing. Here, the flow rate adjusting valve 24 is opened to direct the raw water toward the inlet port 17 by 0.5 liter / minute,
Try to split the flow. As described above, the pressure gauge 27 at this time is adjusted to indicate 0.2 kgf / cm ² . The raw water 20 that has flowed into the oil / water separator 1 from the inlet port 17 enters the dispersion chamber 8, is dispersed, passes through the screen 11, and passes through the oil adsorbent 13. The oil adsorbent 13 adsorbs the oil component corresponding to the floating oil in the raw water, the oil emulsion passes through the oil adsorbent 13, and while passing through the voids in the granular stearylamine layer 14, the stearylamine disperses the oil in the oil emulsion. The fine oil is destroyed and becomes coarse, and the grains of stearylamine are adsorbed as nuclei, and the stearylamine is slightly dissolved by the oil. While passing through the voids of the stearylamine layer 14, the oil in the oil emulsion is removed to give a low concentration of oil-containing water, and in the granular activated carbon 15 layer, the raw water-containing organic matter is removed to deodorize and decolorize the oil adsorbent 1
Enter in 6. The oil adsorbent 16 blocks the activated carbon of the activated carbon layer 15 and the fine particles of stearylamine of the stearylamine layer 14 from flowing out. Then, the treated water collected from the screen 12 into the collecting chamber 9 passes through the outlet port 18 and the water distribution pipe 28 and enters the beaker 29.

"Experimental Examples" Tables 2 and 3 show experimental examples.

In the above apparatus, the raw water tank 19 was filled with about 5 liters of raw water 20. As the raw water 20, as shown in Table 3, sample Nos. 1 to 5 were prepared by mixing water, waste oil, and kerosene.
The waste oil of this sample is engine oil of a gasoline internal combustion engine. Then, as shown in Table 2 for each sample, 3
The upper column of the number of times column, which indicates the number of times of measurement, shows the oil concentration obtained by the beaker 29, and the lower column shows the flow rate flowing into the oil-water separator 1. The flow rate of the pump 21 is 20 liters / minute as already mentioned. Table 3 Sample No. Concentration Water Waste oil Kerosene 1 100 PPM 4.995 liter 2.5 cc 2.5 cc 2 500 PPM 4.975 liter 12.5 cc 12.5 cc 3 1000 PPM 4.950 liter 25.0 cc 25.0 cc 4 1500 PPM 4.925 liter 37.5 cc 37.5 cc 5 2000 PPM 4.900 liter 50.0 cc 50.0 cc

[0025]

According to the present invention, since the oil emulsion is allowed to pass through the granular amine layer, the total area of contact of the amine with the oil emulsion is large relative to the total volume of the amine layer.
In addition, the volume between amine particles is also large, and the oil emulsion is destroyed to coarsen minute oil droplets, and the action of taking in oil with the amine particles as the core cleans the oil emulsion regardless of the small volume of the granular amine layer, and the oil concentration The ability to lower
As a result, it was possible to provide a method for separating and adsorbing oil and water, which has a low cost, a small capacity, and a large capacity, as compared with the case where an amine is fused and solidified on a nonwoven fabric to form a porous nonwoven fabric.

The present invention has a particularly remarkable effect when the amine particle size is 0.01 to 2.5.

According to the present invention, a middle cylinder having a cross section smaller than that of the middle case is housed in a cylindrical case with a space from the case, and one end of the middle cylinder is fixed to one end plate of the case. The other end of the middle cylinder communicates with the inside of the middle cylinder and the outside of the middle cylinder at the other end plate side of the closed case, and the one end plate side of the closed case has a port that communicates with the inside of the middle cylinder and the outside of the closed case. A port that connects the inside of the closed case to the outside of the closed case is provided outside the middle cylinder, and one of the ports is used as the drain inlet and the other is used as the outlet, and the inside and outside of the middle cylinder are between the drain inlet and the drain outlet. The space between the closed case and the sealed case is filled with an oil adsorbent and an emulsified oil treatment material as a member for treating drain,
Since the emulsified oil treatment material is an oil-water separator characterized in that the granular amine is layered, the granular amine layer provides a large total area in which the amine contacts the oil emulsion with respect to the total volume of the amine layer, In addition, the total volume of the space between the amine particles is large, and the floating oil component is removed in advance by the oil adsorbent, and the primary treated raw water, which has almost the most oil emulsion content, passes through the granular amine layer. In addition to having a large purification capacity, the oil adsorbing means and the oil separating and adsorbing means are integrated, so the oil adsorbing tank and the oil decomposing tank are independent as in the past, and compared with the case where they were connected by piping. Installation space will be significantly reduced. In addition, the piping between the oil adsorption tank and the oil decomposition tank is eliminated, which simplifies the piping work at the installation site. Since the drain flows in the cylindrical axial direction between the middle cylinder and the outside of the middle cylinder and the closed case, the performance can be made equal to that of the conventional example.

[Brief description of drawings]

FIG. 1 is a flow sheet showing an oil / water separation method of the present invention.

FIG. 2 is a vertical cross-sectional view of the oil-water separator of the present invention.

FIG. 3 is a flow sheet of a conventional example.

FIG. 4 is a flow sheet of a conventional example.

[Explanation of symbols]

 1 Oil / Water Separation Device 2 Upper End Plate 3 Lower End Plate 5 Outer Cylinder 7 Middle Cylinder 13 Oil Adsorbent 14 Stearylamine Layer 16 Oil Adsorbent

Claims (3)

[Claims] 1. A member for processing oil is housed in a closed tank,
A drain treatment method for removing oil in drain by passing drain through a member for treating oil, wherein the member for treating drain is a layer of granular amine. 2. The method for separating oil and water according to claim 1, wherein the granular amine is stearylamine having a particle size of about 0.01 to 2.5 millimeters. 3. A middle case having a cross section smaller than that of the middle case is housed in the middle case of the cylinder at a distance from the middle case, and one end of the middle cylinder is fixed to one end plate of the middle case. The other end of the cylinder is in communication with the inside of the middle cylinder and the outside of the middle cylinder on the other end plate side of the closed case, and a port communicating with the inside of the middle cylinder and the outside of the closed case on the one end plate side of the closed case,
A port is provided outside the middle cylinder to connect the inside of the closed case to the outside of the closed case, and one of the ports is used as a drain inlet and the other is used as an outlet. An oil-water separation device, characterized in that a space between the closed cases is filled with an oil adsorbent and an emulsified oil treatment material as a drain treatment member, and the emulsified oil treatment material is a layer of granular amine.