JPS6235625B2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to continuous measurement of oil concentration in oil-containing water such as factory wastewater. The present invention relates to a device that continuously measures the oil concentration in treated water and other various types of water.

Currently, as a means to accurately measure trace amounts of oil, the oil in the sample water is extracted with an extractant such as carbon tetrachloride (CCl ₄ ), and the extracted liquid containing the oil is analyzed using an infrared analyzer. There is a so-called solvent extraction-infrared absorption method that measures the oil concentration.

Conventionally, as an apparatus using this solvent extraction-infrared absorption method, there is an apparatus shown in FIG. 1, for example. To explain what is shown in FIG. 1, as sample water a, wastewater A in the drainage channel is constantly quantitatively fed through a sample water sampling pipe 1 and a metering pump 2 via a solenoid valve 3. Then, water is collected into the stirring extractor 4. At the same time, the metering pump 2 quantitatively adds the extract b, for example, carbon tetrachloride (CCl ₄ ) from the regenerator 5 to the stirring extractor 4 . Then, in this stirring extractor 4, the sample water a and the extract b are stirred and mixed by a stirring plate 6 which is interlocked with an electric motor 10, whereby the oil content in the sample water a is extracted. Extracted into liquid b. Extract containing this oil
The mixed liquid (a'+b') of b' and water a' is supplied to a first separator 7 equipped with a hydrophobic filter, for example, a Teflon filter. ′+b′) is the extract b′ containing oil and water.
It is separated into a′ and a′. This separated water a′ is further
Then, it is introduced into the second separator 8, where the extract b' containing a very small amount of oil mixed in the water a' is completely separated. This separated extract b' containing oil is introduced into the regenerator 5. On the other hand, the oil-containing extract b' dehydrated in the first separator 7 is continuously flowed into a measuring cell 9a of an oil concentration measuring device, for example, an infrared analyzer 9, and analyzed by this analyzer 9. The measured results are displayed and recorded on the recorder 11. The extracted liquid b' containing oil after this measurement is introduced into the regenerator 5. The oil-containing extract b' introduced into the regenerator 5 from the measurement cell 9a and the second separator 8 is extracted using an adsorbent such as activated carbon filled in the regenerator 5. Extract liquid b is regenerated by adsorbing only the oil from liquid b'. This regenerated extract b is sucked into the metering pump 2 via the comparison cell 9b of the analyzer 9, and is again introduced into the stirring extractor 4 for reuse.

In the conventional device configured in this way, if the hydrophobic filter of the first separator 7 allows water a' to pass through for some reason, for example, a surfactant may be present in the mixed liquid (a'+b'). If water is mixed in, the action of this surfactant causes water a″ to mix into the oil-containing extract b′ that passes through the hydrophobic filter and is introduced into the measurement cell 9a, and this water The disadvantage was that the contamination of a'' caused measurement errors, making it impossible to perform accurate measurements.

In view of the shortcomings of the conventional devices, the present invention provides a method for measuring, without reducing the response speed of measurement,
It is an object of the present invention to provide an apparatus that can reliably separate an oil-containing extract from water, and can continuously measure oil concentration quickly and with high measurement accuracy.

Embodiments of the present invention will be described in detail below based on the drawings.

FIG. 2 shows the overall configuration of the continuous oil concentration measuring device according to the present invention, and A in the figure shows
For example, this is waste water flowing through a drainage channel in a factory, and a water sampling pipe 1 having a water sampling port disposed in this waste water A is connected to one pump 2a of a metering pump 2 via a solenoid valve 3. This one pump 2a is connected to one inlet of the stirring extractor 4, and is configured to suction a fixed amount of the wastewater A as sample water a using this one pump 2a, and introduce it into the stirring extractor 4. . The inlet side of the other pump 2b of this metering pump 2 is connected to the regenerator 5, and the outlet side thereof is connected to the other inlet of the stirring extraction device 4, and the extract b from the regenerator 5 is extracted with, for example, tetrachloride. It is configured to suck a fixed amount of carbon (CCl ₄ ) and introduce it into the stirring extractor 4. The stirring extractor 4 is equipped with a stirring plate 6 that is interlocked with a drive device 10, for example, an electric motor, and the sample water a and the extract liquid are continuously supplied by the rotation of the stirring plate 6 from the metering pump 1. The oil content in the sample water a is extracted with the extraction liquid b by stirring and mixing with the extract liquid b. The outlet side of this stirring extractor 4 is connected to the first separator 7, which separates the oil-containing extract b' and water.
The mixed liquid (a'+b') with a' is introduced into a first separator 7, and this first separator 7 is equipped with a hydrophobic filter, such as a Teflon filter, and the mixed liquid is passed through this filter. The extractor (a'+b') is separated into an oil-containing extract b' and a water a', and these are continuously taken out. The extract b' outlet of the first separator 7 is connected to a water separator 12, and the water separator 12 extracts the oil-containing extract.
The lower outlet side of this moisture separator 12 is configured to extract a small amount of moisture a'' mixed in the water b', and the oil concentration analyzer 9, for example, an infrared analyzer measurement cell
The measuring cell 9a is connected to the cell 9a, and is configured to analyze and measure only the oil-containing extract b'. The measurement result by this measurement cell 9a is configured to be displayed and recorded on a recorder 11 connected to this cell 9a.

Since the first separator 7 is a so-called high-speed separator that quickly separates the mixed liquid (a'+b'), the extracted water a' contains an extract b'' containing a small amount of oil. Since it also contains water a′, a mixed solution of extract b″ containing mixed oil (a′+b″)
is introduced into the second separator 8 which has excellent separation performance,
In this separator 8, the extract containing water a' and oil is extracted.
It is configured to be separated into ``b'' and ``b''.

The analyzer 9 is configured such that the extract b' is continuously introduced into the measurement cell 9a, and the extract b regenerated by the regenerator 5 (described later) is free from measurement errors due to a decrease in the regeneration capacity of the regenerator 5. In order to prevent this from occurring, it is configured to be continuously introduced into the comparison cell 9b. The outlet side of the measuring cell 9a is connected to the regenerator 5. This regenerator 5 is used as an adsorbent.
For example, an extract containing activated carbon and introduced from the measurement cell 9a or the second separator 8.
b′, b″ are extracts containing oil in the adsorbent.
Only the oil in b' and b'' is adsorbed, and the extract b is thereby regenerated. This regenerated extract b is passed through the comparison cell 9b of the analyzer 9. It is configured to be sucked in by the metering pump 2 and continuously returned to the extractor 4 again.

Incidentally, a piping connection is made from the regenerator 5 to the solenoid valve 3 for the purpose of zero checking or cleaning the piping.

Next, the detailed structure of the moisture separator 12 and the measurement cell 9a of the moisture separator 12 and the analyzer 9 will be explained.
The vertical positional relationship will be explained. As shown in FIG. 3, the moisture separator 12 includes a cyclone 20, which is connected to the first separator 7 through an inlet pipe 21 continuous in the circumferential tangential direction at the upper part of the cyclone 20. and is connected to the lower part of the measurement cell 9a of the analyzer 9 via an outlet pipe 22 connected to the lower part thereof. A first connecting pipe 23 extending upward is connected to the central upper end position S1 of the cyclone 20.
A discharge position S2 is formed in the middle of the connecting pipe 23, and a discharge pipe 24 is connected downward from the discharge position S2, and the upper end of the first connecting pipe 23 is open to the atmosphere. At the top of the measurement cell 9a,
A second connecting pipe 25 extending upward is connected in communication,
A lead-out position S3 is formed in the middle of the second connecting pipe 25, and a lead-out pipe 26 connected to the regenerator 5 is led downward from the lead-out position S3.
The upper end of this second connecting pipe 25 is open to the atmosphere. With these first connecting pipe 23 and second connecting pipe 25,
A so-called communication pipe is configured via the cyclone 20 and the measurement cell 9a of the analyzer 9.
In addition, in FIG. 3, position S4 indicates the presence of water in the oil-containing extract b' separated in the first separator 7.
Extract containing oil when not mixed with a″
b', which is at approximately the same height as the outlet position S3 of the outlet pipe 26 (a position higher by the resistance within the communication pipe).

The following positions are located between the upper end position S1 of these cyclones 20, the discharge position S2 of the discharge pipe 24, the discharge position S3 of the discharge pipe 26, and the normal liquid level position S4 of the extract b' containing oil. It is set to satisfy the inequality condition.

△H(S1・S3)×p＞△H(S1・S2) ＞ΔH(S1・S4) [Here, △H(S1・S3) is the position S1 and S3
The vertical distance between positions S1 and S2, △H (S1・S2) is the vertical distance between positions S1 and S2, △H
(S1·S4) is the vertical distance between position S1 and position S4, p is the specific gravity of the extract b', and the specific gravity of water is assumed to be 1. ] The significance of setting this way is that △H
If (S1・S3)×p>△H(S1・S2) is not satisfied, the water a″ is not discharged from the discharge pipe 24,
If the oil passes through the cyclone 20 and is introduced into the measurement cell 9a, there is a risk that an error will occur in the measurement of the oil concentration, and if △H (S1, S2) > △H (S1, S4) is not satisfied. The extract containing the oil is
b' is discharged through the discharge tube 24, which significantly reduces the response speed of the measurement.

Next, the operation of the continuous oil concentration measuring device having the above configuration will be explained.

Drainage A in the drainage channel is constantly quantitatively sampled as sample water a by a metering pump 2 via a water sampling pipe 1 and a solenoid valve 3, and is supplied to a stirring extractor 4. At the same time, an extract b, such as carbon tetrachloride (CCl ₄ ), is supplied from the regenerator 5 to the stirring extractor 4 using the metering pump 2 . Inside this stirring extractor 4, an electric motor 10
The sample water a and the extract b are stirred and mixed by a stirring plate 6 connected to the agitator plate 6, whereby the oil in the sample water a is extracted into the extract b, and the extract containing these oils is mixed.
The mixed liquid (a'+b') of b' and water a' is supplied to the first separator 7, and the oil-containing extract b' and water a are passed through a hydrophobic filter in the first separator 7. ′ and are separated. The separated water a' is introduced into the second separator 8, where the extract b'' containing a very small amount of oil mixed in the water a' is completely separated. The extract b'' containing oil is introduced into the regenerator 5. On the other hand, the separated oil-containing extract b' is introduced into a water separator 12, where the water separator 12 removes a small amount of water mixed in the oil-containing extract b'. a″ is removed and only the oil-containing extract b′ is collected in the measuring cell 9 of the infrared analyzer 9.
a, and the results of analysis and measurement by the analyzer 9 are displayed and recorded on the recorder 11. The oil-containing extract b′ used for this measurement was recycled.
It is introduced into the container 5. The oil-containing extracts b' and b'' introduced into the regenerator 5 have only the oil adsorbed by the adsorbent filled in the regenerator 5, and are regenerated as the extract b. The extract b is sucked into the metering pump 2 via the comparison cell 9b of the analyzer 9, and is again introduced into the stirring extractor 4 to be reused.

Next, the operation of the moisture separator 12 will be explained in detail.

The oil-containing extract b' separated in the first separator 7 is passed through the inlet pipe 21 to the cyclone 20.
The air flows into the cyclone 20 from the tangential direction of the circumference, creating a swirling flow within the cyclone 20. As a result, the oil-containing extract b' is subjected to centrifugal force and is transferred to the cyclone 2.
0 and introduced into the measuring cell 9a via the outlet pipe 22. At this time, if no water a'' is mixed in the oil-containing extract b', the liquid level of the oil-containing extract b' in the first connecting pipe 23 is On the other hand, since the separation of the water a' and the oil-containing extract b' in the first separator 7 is incomplete, the oil-containing extract b' is introduced into the cyclone 20. If water a″ is mixed in extract b′, this water a″ has a lower specific gravity than extract b′, which contains oil, so the extract contains oil, which has a higher specific gravity.
b′ falls as mentioned above, but water with low specific gravity
The water a″ gathers in the center, gradually aggregates into large water droplets, and is accumulated in the first connecting pipe 23.Then, the water a″ in the first connecting pipe 23 reaches the discharge position S2. Then, this water a'' is discharged to the outside through the discharge pipe 24. With this, the measurement cell 9a
Since no moisture a″ is introduced into the
Smooth and accurate measurements can be performed without causing measurement errors due to a″.Moreover, the cyclone 20 is used to generate a swirling flow to separate the water a″ from the oil-containing extract b′. As a result, water a″ and oil-containing extract b′ can be quickly separated, resulting in an extremely high separation rate.Furthermore,
Moisture a'' that interferes with the measurement is discharged from the discharge pipe 24, and the extract b' containing oil necessary for the measurement is sufficiently introduced into the measurement cell 9a.
There is no reduction in measurement response speed.

FIG. 4 shows another embodiment of the invention. In this other embodiment, a temperature adjustment tank 31 surrounding the cyclone 20 is configured, and the temperature inside the cyclone 20 is adjusted to a temperature slightly higher than room temperature, for example, 35°C. ~50℃, preferably 40℃ depending on the type of oil extraction solvent
It is intended to be adjusted and maintained. According to this configuration, the extract containing oil in the cyclone 20
The rate of separation between b' and water a'' can be increased, and the separation action can be performed more quickly. However, if the temperature in the cyclone 20 is made higher than room temperature in this way, the oil-containing extract Since air bubbles v... may occur in b', in order to prevent these air bubbles v... from being introduced into the measurement cell 9a, a midway point of the output pipe 22 is connected to the second connecting pipe 25. A bubble branch pipe 32 may be configured in which the bubbles generated in the cyclone 20 are...
is from the middle of the output pipe 22 to the bubble branch pipe 32.
Then, the bubble v... is introduced into the measurement cell 9
a, and is introduced into the second connecting pipe 25, but is not introduced into the measurement cell 9a. With this,
Smooth measurement can be performed without measurement errors caused by air bubbles v in the analyzer 9.

In the above embodiment, the input pipe 2 is arranged in the same direction from the circumferential tangential direction to the cyclone 20.
In step 1, the extract b' containing oil was introduced to generate a high-speed swirling flow, but the input pipe 2
1 is connected to the upper part of the cyclone 20 to cause the oil-containing extract b' to fall from the upper part of the cyclone 20, and a guide plate disposed inside the cyclone 20 allows the oil-containing extract b' to fall down from the upper part of the cyclone 20.
It may be configured to guide b' to produce a swirling flow.

Further, in the embodiment described above, the extract b' containing oil is introduced into the cyclone 20 from the first separator 7 in a free fall manner using gravity, but the first separator 7 A pump may be disposed between 7 and the cyclone 20, and the pump may be configured to forcibly introduce the oil-containing extract b' into the cyclone 20.

As described above, in the oil concentration measuring device of the present invention, the extract containing oil and water can be quickly separated in the first separator, and the separated extract containing oil contains After completely separating the slight amount of water mixed in with the water separator, only the extract containing oil can be introduced into the analyzer for measurement.
〓〓〓〓
Accurate measurements without measurement errors can be performed continuously without reducing the measurement response speed.

[Brief explanation of the drawing]

FIG. 1 is a flow sheet showing the overall configuration of a conventional device, FIGS. 2 to 4 show embodiments of the present invention, FIG. This figure shows the vertical positional relationship between the moisture separator and the measuring cell, and FIG. 4 is a diagram showing the vertical positional relationship between the moisture separator and the measuring cell in another embodiment. 4... Stirring extractor, 7... First separator, 9...
Analyzer, 12...Moisture separator, 20...Cyclone, 24...Discharge pipe, 31...Temperature adjustment tank, 32
...bubble branch pipe. 〓〓〓〓

Claims (1)

[Claims] 1. A feeding means that continuously supplies a fixed amount of sample water and extract liquid, a stirring extractor that mixes and stirs the sample water and extract liquid to extract the oil content in the sample water with the extract liquid, and this extraction a first separator equipped with a hydrophobic filter that continuously separates a mixed liquid of an oil-containing extract and water derived from the vessel into an oil-containing extract and water; and the first separator. A continuous oil concentration measuring device comprising an analyzer that continuously measures the oil concentration by introducing an oil-containing extract from a container, and a cyclone structure is provided between the first separator and the analyzer. A water separator is provided, the water separator is configured to separate a trace amount of water mixed into the oil-containing extract derived from the first separator, and the separated water is discharged. The value obtained by multiplying the vertical distance between the upper end position of the cyclone structure and the extraction position by the specific gravity of the extraction liquid is the value obtained by multiplying the position and the extraction position of the oil-containing extract derived from the analyzer by the specific gravity of the extraction liquid. The vertical distance between the upper end position of the cyclone structure and the discharge position is set to be greater than the value obtained by multiplying the specific gravity of water, and the distance between the upper end position of the cyclone structure and the discharge position is A continuous measuring device for oil concentration, characterized in that a vertical distance is set to be larger than a vertical distance between an upper end position of the cyclone structure and the lead-out position.