JP6772470B2 - Organic solvent processing equipment - Google Patents

Description

The present invention relates to an organic solvent treatment apparatus suitable for treating an organic solvent-containing gas.

Conventionally, the following devices are known as devices for recovering an organic solvent from a gas containing an organic solvent and discharging the treated gas. An adsorption process in which an organic solvent-containing gas is supplied to an adsorption tank filled with granular activated carbon or fibrous activated carbon as an adsorbent and adsorbed by the adsorbent to discharge the treated gas, and water vapor is introduced into the adsorption tank. This is an organic solvent treatment device that alternately repeats the desorption step of desorbing the organic solvent from the adsorbent. Here, the temperature of the water vapor used for desorption of the organic solvent is generally 100 ° C. to 130 ° C. (see, for example, Patent Documents 1 and 2).

However, when the organic solvent-containing gas contains even a small amount of organic silicon, the adsorption performance of the adsorbent gradually deteriorates when the treatment is performed with a steam desorption type organic solvent treatment device using activated carbon as an adsorbent. I will go. Then, a situation occurs in which the recovery rate of the organic solvent is lowered and the organic solvent is mixed in the exhaust gas from the organic solvent treatment apparatus. This is because organic silicon has a high boiling point and exhibits resistance to desorption, so that it cannot be completely desorbed from the adsorbent with water vapor at 100 to 130 ° C. and accumulates in the adsorbent.

In order to solve the above-mentioned problems, a technique has been proposed in which the desorption steam of the organic solvent treatment device is heated by a heater and the non-detachable component is desorbed from the adsorbent using superheated steam at 150 ° C to 300 ° C. (See, for example, Patent Documents 3 and 4).

Special Publication No. 64-1-1326 Japanese Unexamined Patent Publication No. 2001-179041 Japanese Unexamined Patent Publication No. 3-193113 Japanese Unexamined Patent Publication No. 2011-125800

However, when the organic silicon contained in the organic solvent-containing gas is cyclic organic silicon (for example, hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, etc.), it is polymerized on the adsorbent by superheated steam and is more difficult to desorb. It changes into a component (substance). Therefore, it is not a good idea to constantly perform desorption with superheated steam. Further, raising the temperature of water vapor for desorption leads to an increase in the running cost of the processing apparatus.
Therefore, the present invention has been made in view of such a problem. That is, an object of the present invention is to enable an organic solvent treatment apparatus provided with an adsorbent tank filled with an adsorbent to more efficiently desorb and desorb adsorbent substances and to perform operation with excellent running cost.

As a result of diligent studies, the present inventor has determined the timing of introducing superheated steam when treating an organic solvent-containing gas containing cyclic organic silicon with a steam desorption type organic solvent treatment apparatus using an adsorbent. The present invention was completed by finding that the cyclic organic silicon can be efficiently attached and detached.
That is, the present invention can solve the above problems by the configuration shown below.
1. 1. A suction tank filled with an adsorbent is provided, an organic solvent-containing gas is introduced into the adsorption tank, the organic solvent is adsorbed on the adsorbent, the treated gas is discharged, and a desorption gas is introduced into the adsorption tank. Then, in the organic solvent treatment apparatus for desorbing the organic solvent from the adsorbent, when the concentration of the organic solvent in the discharged treated gas is equal to or less than the set value, the organic solvent-containing gas to the adsorption tank is charged. When the introduction and the introduction of the desorption gas are alternately repeated and the concentration of the organic solvent in the discharged treated gas exceeds the set value, the temperature of the adsorption tank is higher than that of the desorption gas. An organic solvent treatment device characterized by introducing a recycling gas.
The number of adsorption tanks provided in the organic solvent treatment apparatus may be one or more. If there are a plurality of gases to be processed, a larger amount of gas can be processed.
2. The organic solvent treatment apparatus according to 1 above, wherein the regeneration gas is superheated steam at 180 to 250 ° C., and the desorption gas is steam at a temperature equal to or lower than the temperature of the regeneration gas.
3. 3. The organic solvent treatment apparatus according to 1 or 2, wherein the organic solvent-containing gas contains organic silicon.
4. The organic solvent treatment apparatus according to 3, wherein the organic silicon is cyclic organic silicon.
5. When the concentration of the organic solvent in the discharged treated gas is equal to or less than the set value, the organic solvent-containing gas is introduced after a period during which the gas is not introduced after the introduction of the detachable gas. The organic solvent treatment apparatus according to any one of 1 to 4 above.
6. When a plurality of the adsorption tanks are provided and the concentration of the organic solvent in the discharged treated gas exceeds the set value, the regeneration gas is introduced into some of the adsorption tanks. In addition, the introduction of the organic solvent-containing gas and the introduction of the desorption gas are alternately repeated for the remaining adsorption tanks of the part of the adsorption tanks into which the regeneration gas is introduced. The organic solvent treatment apparatus according to any one of 1 to 5, wherein the operation is performed until all of the plurality of adsorption tanks are selected while sequentially selecting the gas.
7. The organic solvent treatment apparatus according to any one of 1 to 6 above, wherein the adsorbent is a fibrous activated carbon.
8. A control device for controlling the supply of the gas to be treated, the desorption gas, and the regeneration gas to the adsorption tank provided with the organic solvent treatment device according to any one of 1 to 7.
9. An organic solvent-containing gas is introduced into an adsorbent tank filled with an adsorbent, the organic solvent is adsorbed on the adsorbent to discharge the treated gas, and a desorption gas is introduced into the adsorbent to be removed from the adsorbent. In the method of supplying gas to the organic solvent treatment apparatus for desorbing the organic solvent, when the concentration of the organic solvent in the discharged treated gas is equal to or less than the set value, the organic solvent-containing gas is supplied to the adsorption tank. And the desorption gas are alternately supplied, and when the concentration of the organic solvent in the discharged treated gas exceeds the set value, the adsorption tank is supplied with the regenerative gas having a temperature higher than that of the desorption gas. A supply method characterized by

According to the above configuration of the present invention, the organic solvent treatment apparatus provided with the adsorbent can more efficiently desorb and desorb the adsorbed substance, and can operate with excellent running cost. Therefore, the life of the adsorbent can be greatly improved. Moreover, the running cost can be reduced as compared with the case where the adsorbent is always attached and detached by superheated steam. In particular, in the organic solvent-containing gas treatment containing cyclic organic silicon, the adsorbent can be regenerated while suppressing the polymerization of cyclic organic silicon.

It is the schematic which shows the structure of the organic solvent processing apparatus of Embodiment 1 of this invention. It is the schematic which shows the structure of the organic solvent processing apparatus of Embodiment 2 of this invention. It is a figure which shows the operation flow in the organic solvent processing apparatus of Embodiment 2 of this invention.

[Embodiment 1]
An embodiment of the present invention will be described with reference to FIG. The organic solvent treatment device 1 of the present embodiment is a device that treats a gas to be treated (gas containing an organic solvent) and discharges a clean gas (treated gas), and as shown in FIG. 1, each of the adsorbents 14 It includes a filled adsorption tank A13a and an adsorption tank B13b. When it is not necessary to distinguish between the adsorption tank A13a and the adsorption tank B13b, the adsorption tank 13 is used as a general term. In the present embodiment, two adsorption tanks 13 are provided, but the number of the adsorption tanks 13 is not limited, and may be one or three or more.

As the adsorbent 14, granular, powdery, fibrous, honeycomb-shaped activated carbon, zeolite, silica gel, activated alumina, or the like can be used. In particular, it is preferable to use activated carbon fiber. This is because the activated carbon fiber has micropores on its surface and has a fibrous structure, so that the adsorption speed and the desorption rate of the substance to be adsorbed are high, so that the gas to be treated can be treated efficiently. In the present embodiment, the adsorption tank 13a and the adsorption tank 13b are filled with the adsorbent 14 made of the same material, but the adsorbents made of different materials may be filled.

The organic solvent treatment apparatus 1 carries out an adsorption treatment in which the gas to be treated is introduced into the adsorption tank 13 and the organic solvent is adsorbed on the adsorbent 14 to discharge the clean gas. Further, a desorption treatment is carried out in which a desorption gas is introduced into the adsorption tank 13 to desorb the organic solvent from the adsorbent 14. In this embodiment, water vapor is used as the desorption gas. Note that FIG. 1 shows a state in which the adsorption tank 13a is performing the adsorption treatment and the adsorption tank 13b is performing the desorption treatment.

An upper damper 16 and a lower damper 15 are attached to the adsorption tank 13, and the gas flow path can be switched by opening and closing these dampers.

In the present embodiment, the gas to be treated is an organic solvent-containing gas containing organic silicon, which is sent from the gas supply duct 11 to be treated to the raw gas blower 12, and the lower damper 15 and the upper damper 16 are opened so that the gas to be treated can be adsorbed. It is introduced into the adsorption tank 13 which has become. By the adsorption treatment in the adsorption tank 13, the organic silicon and the organic solvent are adsorbed by the adsorbent 14 in the adsorption tank 13 to become clean gas, which is discharged from the clean gas discharge duct 17.

In the present embodiment, the organic silicon contained in the organic solvent-containing gas is cyclic organic silicon. Cyclic organic silicon refers to a cyclic organic compound having a cyclic molecular structure skeleton due to a siloxane bond, for example, hexamethylcyclotrisiloxane (D3), octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5). However, it is not limited to these.

In the present embodiment, the treatment target (treatment gas) of the organic solvent treatment device 1 is an organic solvent-containing gas containing cyclic organic silicon, but the organic solvent treatment device 1 changes to a component that is difficult to desorb due to superheated steam. It can also be applied to organic solvent-containing gas containing components. Superheated steam will be described later.

On the other hand, water vapor is introduced as a desorption gas from the water vapor supply port 18 provided in the adsorption tank 13 into the adsorption tank 13 in which the lower damper 15 and the upper damper 16 are closed and ready for desorption treatment. This steam is supplied from the steam supply line 21 to the steam supply port 18b via the steam line switching valve 22. By introducing water vapor into the adsorption tank 13, the organic solvent adsorbed on the adsorbent 14 is desorbed.

The steam containing the desorbed organic solvent is supplied to the condenser 32 from the desorption steam discharge port 19 connected to the adsorption tank 13 via the desorption steam line 31, and is liquefied and condensed into the organic solvent and water by the condenser 32. Will be done. After that, it is collected in the recovery liquid tank 33.

The clean gas discharged from the clean gas discharge duct 17 after the adsorption treatment in the adsorption tank 13 is monitored by a VOC densitometer (organic solvent densitometer) 25 provided in the clean gas discharge duct 17. Then, the organic solvent treatment apparatus 1 is an adsorption tank when the value measured by the VOC concentration meter 25 is less than or equal to the set value, that is, when the concentration of the organic solvent in the clean gas discharged from the adsorption tank 13 is less than or equal to the set value. The introduction of the gas to be treated and the introduction of the desorption gas into 13 are alternately repeated. As a result, the adsorption process and the desorption process in the adsorption tank 13 are alternately repeated. Here, in the two adsorption tanks 13, that is, the adsorption tank A13a and the adsorption tank B13b, the desorption gas is introduced into the other while the gas to be treated is introduced into one. That is, the desorption treatment is carried out in the adsorption tank B13b during the adsorption treatment in the adsorption tank A13a, and the desorption treatment is carried out in the adsorption tank A13a during the adsorption treatment in the adsorption tank B13b, and this is repeated. By such an operation operation, the organic solvent treatment apparatus 1 can efficiently treat a large amount of the gas to be treated. The adsorption tank 13 after the desorption treatment may be put in a standby state in which no gas is introduced until the next adsorption treatment is carried out. In the present embodiment, the above operation of the organic solvent treatment apparatus 1 when the value measured by the VOC concentration meter 25 is equal to or less than the set value is referred to as normal operation.

Further, in the organic solvent treatment apparatus 1, when the value measured by the VOC concentration meter 25 exceeds the set value, that is, when the concentration of the organic solvent in the clean gas discharged from the adsorption tank 13 exceeds the set value. , Performs the following processing. The raw gas blower 12 is stopped, the supply of the gas to be processed is stopped, the steam line switching valve 23 is switched in the steam supply line 21, and the superheated steam (regeneration gas) in which the steam is heated to a predetermined temperature by the heater 25 is used. It is introduced into the adsorption tank 13. The superheated steam is steam heated by the heater 25 to a temperature higher than the steam used for the desorption treatment.

By introducing superheated steam into the adsorption tank 13, a regeneration process, which is a desorption treatment of the adsorbent 14 in the adsorption tank 13 with superheated steam, is carried out. Here, in the present embodiment, the desorption treatment with steam is simply referred to as a desorption treatment, and the desorption treatment with heated steam is referred to as a regeneration treatment to distinguish it from the desorption treatment with steam. These are only used for distinction, and (a part of) the adsorbent 14 is regenerated even in the desorption treatment with water vapor. Since it is a wording for distinction, for example, the desorption treatment by superheated steam may be referred to as the additional desorption treatment.

In the regeneration treatment, since the cyclic organic silicon is contained in the gas to be treated in the present embodiment, the cyclic organic silicon is desorbed, but the organic solvent remains in the adsorbent 14 (in the desorption treatment using water vapor). If it remains), it is also detached. The desorbed cyclic organic silicon and the superheated steam containing the organic solvent are supplied to the condenser 32 from the desorption steam discharge port 19 connected to the adsorption tank 13 via the desorption steam line 31 and condensed in the condenser 32. .. After that, it is collected in the recovery liquid tank 33.

In the present embodiment, since the organic solvent treatment device 1 includes two adsorption tanks, the steam line switching valve 22 is switched, superheated steam is introduced into each of the adsorption tank A13a and the adsorption tank B13b, and the regeneration treatment is carried out respectively. .. It does not matter which one is regenerated first.

In the present embodiment, the operation of the organic solvent treatment apparatus 1 when the value measured by the VOC concentration meter 25 exceeds the set value is referred to as a regeneration operation.

In the organic solvent treatment apparatus 1, the temperature of the superheated steam used in the regeneration treatment is preferably 180 to 250 ° C. If the temperature of the superheated steam is 180 ° C. or lower, the cyclic organic silicon cannot be removed more efficiently than the adsorbent 14, and the regeneration efficiency is lowered. Further, when the temperature of the superheated steam is 250 ° C. or higher, the polymerization of the cyclic organic silicon is promoted, and the running cost is increased without significantly improving the regeneration efficiency of the adsorbent 14.

The time (regeneration time) for introducing superheated steam into the adsorption tank 13 is not particularly limited, but is preferably 1 hour or more. This is because if the reproduction time is less than one hour, sufficient reproduction cannot be performed.

When the regeneration treatment in all the adsorption tanks 13 is completed (when the regeneration operation is completed), the organic solvent treatment apparatus 1 operates the exhaust gas blower 12 again, introduces the gas to be treated into the adsorption tank 13, and performs the adsorption treatment. carry out. Then, when the measured value of the clean gas discharged from the clean gas discharge duct 17 by the VOC concentration meter 25 is equal to or less than the set concentration value, the normal operation is started, and when the concentration value is still exceeded, the reproduction is performed again. Regeneration processing is performed on each of the adsorption tanks 13 (regeneration operation is performed).

(Example)
Hereinafter, the present invention will be specifically described with reference to examples using the organic solvent treatment apparatus 1 of the present embodiment, but the present invention is not limited to the following contents.

(Example 1-1)
A mixed gas (processed gas) at 45 ° C. containing 2000 ppm of toluene and 1 ppm of octamethylcyclotetrasiloxane was introduced into the adsorption tank 13 by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and was adsorbed by the adsorption tank 13. Adsorption treatment was performed on the material 14 for 10 minutes. At this time, the numerical value (VOC concentration of clean gas) of the VOC concentration meter 25 installed in the clean gas discharge duct 17 was 1 ppm or less. Further, the adsorbent 14 adsorbed with the organic solvent was desorbed for 8 minutes using water vapor. The desorbed gas containing the organic solvent was supplied from the desorbed steam discharge port 19 to the condenser 32 via the desorbed steam line 31, liquefied and condensed in the organic solvent and water, and then recovered in the recovery liquid tank 33. .. The adsorption tank 13 after the desorption treatment was put into a standby state for 2 minutes until it was subjected to the next adsorption treatment.

A mixed gas containing toluene and octamethylcyclotetrasiloxane was continuously treated for 170 hours by repeating each of the above states (adsorption treatment, desorption treatment, standby state) while switching the adsorption tank 13 in order (normal operation is performed). , The value of the VOC densitometer 25 exceeded 100 ppm. Therefore, the supply of the mixed gas was stopped, and superheated steam at 200 ° C. was introduced into each adsorption tank 13 for 1 hour to regenerate the adsorbent 14. After the regeneration treatment with superheated steam of each adsorption tank 13, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. It was confirmed that the value of the VOC concentration meter 25 at this time was 1 ppm or less, and the adsorbent 14 was sampled to measure the residual amount of octamethylcyclotetrasiloxane and its polymer.

(Example 1-2)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1.5 ppm of decamethylcyclopentasiloxane was introduced into the adsorption tank 13 by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. Was done. At this time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, the adsorbent 14 adsorbed with the organic solvent was desorbed for 8 minutes using water vapor. The desorption gas containing the organic solvent was supplied from the desorption steam discharge port 19 to the condenser 32 via the desorption steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank 13 after the desorption treatment was put into a standby state for 2 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 90 hours by repeating each of the above operating states while switching the adsorption tank 13 in order, the value of the VOC concentration meter 25 exceeded 100 ppm. Therefore, the supply of the mixed gas was stopped, and superheated steam at 200 ° C. was introduced into each adsorption tank 13 for 1 hour to regenerate the adsorbent 14. After the regeneration treatment with superheated steam of each adsorption tank 13, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. After confirming that the value of the VOC densitometer at this time was 1 ppm or less, the adsorbent 14 was sampled to measure the residual amount of decamethylcyclopentasiloxane and its polymer.

(Comparative Example 1-1)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1 ppm of octamethylcyclotetrasiloxane was introduced into the adsorption tank 13 by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. It was. At this time, the value of the VOC concentration meter 25 installed at the clean gas discharge port was 1 ppm or less. Further, the adsorbent 14 adsorbed with the organic solvent was desorbed for 8 minutes using water vapor. The desorption gas containing the organic solvent was supplied from the desorption steam discharge port 19 to the condenser 32 via the desorption steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank 13 after the desorption treatment was put into a standby state for 2 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 170 hours by repeating each of the above operating states while switching the adsorption tank in order, the value of the VOC concentration meter 25 exceeded 100 ppm. Therefore, the supply of the mixed gas was stopped, and superheated steam at 200 ° C. was introduced into each adsorption tank 13 for 1 hour to regenerate the adsorbent 14. After the regeneration treatment with superheated steam of each adsorption tank 13, the supply of the mixed gas was started again and the adsorption treatment with the adsorbent 14 was performed. At this time, the value of the VOC concentration meter 25 was 25 ppm, and the adsorbent 14 was sampled to measure the residual amount of octamethylcyclotetrasiloxane and its polymer.

(Comparative Example 1-2)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1.5 ppm of decamethylcyclopentasiloxane was introduced into the adsorption tank 13 by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. Was done. At this time, the value of the VOC concentration meter 25 installed at the clean gas discharge port was 1 ppm or less. Further, the adsorbent 14 adsorbed with the organic solvent was desorbed for 8 minutes using water vapor. The desorption gas containing the organic solvent was supplied from the desorption steam discharge port 19 to the condenser 32 via the desorption steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank 13 after the desorption treatment was put into a standby state for 2 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 90 hours by repeating each of the above operating states while switching the adsorption tank in order, the value of the VOC concentration meter 25 exceeded 100 ppm. Therefore, the supply of the mixed gas was stopped, and superheated steam at 200 ° C. was introduced into each adsorption tank 13 for 1 hour to regenerate the adsorbent 14. After the regeneration treatment with superheated steam of each adsorption tank 13, the supply of the mixed gas was started again and the adsorption treatment with the adsorbent 14 was performed. At this time, the value of the VOC concentration meter 25 was 35 ppm, and the adsorbent 14 was sampled to measure the residual amount of decamethylcyclopentasiloxane and its polymer.

(Comparative Example 1-3)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1 ppm of octamethylcyclotetrasiloxane was introduced into the adsorption tank 13 by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. It was. At this time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, the adsorbent 14 adsorbed with the organic solvent was desorbed for 8 minutes using water vapor. The desorption gas containing the organic solvent was supplied from the desorption steam discharge port 19 to the condenser 32 via the desorption steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank 13 after the desorption treatment was put into a standby state for 2 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 170 hours by repeating each of the above operating states while switching the adsorption tank in order, the value of the VOC concentration meter 25 exceeded 100 ppm. Therefore, the supply of the mixed gas was stopped, and superheated steam at 300 ° C. was introduced into each adsorption tank 13 for 1 hour to regenerate the adsorbent 14. After the regeneration treatment with superheated steam of each adsorption tank 13, the supply of the mixed gas was started again and the adsorption treatment with the adsorbent 14 was performed. At this time, the value of the VOC concentration meter 25 was 1 ppm or less, and the adsorbent 14 was sampled to measure the residual amount of octamethylcyclotetrasiloxane and its polymer.

(Comparative Example 1-4)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1.5 ppm of decamethylcyclopentasiloxane was introduced into the adsorption tank 13 by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. Was done. At this time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, the adsorbent 14 adsorbed with the organic solvent was desorbed for 8 minutes using water vapor. The desorption gas containing the organic solvent was supplied from the desorption steam discharge port 19 to the condenser 32 via the desorption steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank 13 after the desorption treatment was put into a standby state for 2 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 90 hours by repeating each of the above operating states while switching the adsorption tank in order, the value of the VOC concentration meter 25 exceeded 100 ppm. Therefore, the supply of the mixed gas was stopped, and superheated steam at 300 ° C. was introduced into each adsorption tank 13 for 1 hour to regenerate the adsorbent 14. After the regeneration treatment with superheated steam of each adsorption tank 13, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. The value of the VOC densitometer at this time was 1 ppm or less, and the adsorbent 14 was sampled to measure the residual amount of decamethylcyclopentasiloxane and its polymer.

The results of Examples 1-1 to 1-2 and Comparative Examples 1-1 to 1-4 are shown in Table 1.

As shown in Table 1, the VOC concentration of the clean gas of Examples 1-1 and 1-2 is 1 ppm or less, and the residual amount of cyclic organic silicon and its polymer is 1 mg / g-KF. It can be seen that in Examples 1-1 and 1-2, the cyclic organic silicon can be desorbed and desorbed with extremely high efficiency as compared with Comparative Examples 1-1 and 1-2, and the adsorbent can be regenerated. Further, in Comparative Examples 1-3 and 1-4, the clean air VOC concentration and the residual amount of the cyclic organic silicon and its polymer are almost the same as those of Examples 1 and 2, but the superheated steam is heated to a high temperature (300 ° C.). ), The amount of electricity used becomes high, and energy efficiency is poor. From this, it can be seen that the running costs can be reduced in Examples 1-1 and 1-2.

[Embodiment 2]
Another embodiment of the present invention will be described in detail with reference to FIGS.
As shown in FIG. 2, the organic solvent treatment device 1A of the present embodiment has a configuration including three adsorption tanks 13, and is in addition to the configuration of the organic solvent treatment device 1 described with reference to FIG. 1 in the first embodiment. , The structure is provided with an adsorption tank C13c filled with the adsorbent 14. In the present embodiment, the adsorption tank A13a, the adsorption tank B13b, and the adsorption tank C13c are filled with the adsorbent 14 of the same material, but the adsorbents of different materials may be filled. Further, although the present embodiment includes two adsorption tanks 13, the number of the adsorption tanks 13 is not limited, and may be four or more.

Similar to the adsorption tank A13a and the adsorption tank B13b, the adsorption tank C13c is provided with an upper damper 16 and a lower damper 15, and is provided with a steam supply port 18 and a desorption steam discharge port 19. Further, the steam line switching valve 22 is provided so that the flow path can be switched from the steam supply line 22 to each adsorption tank 13 (adsorption tank A13a, adsorption tank B13b, adsorption tank C13c). Since the configurations other than these are the same as those of the organic solvent treatment apparatus 1, the same components are designated by the same reference numerals, and the description thereof will be omitted.

The flow during normal operation in the organic solvent treatment apparatus 1A is shown in FIG. 3A, and the flow during regeneration operation is shown in FIG. 3B. As shown in FIG. 3A, the organic solvent treatment apparatus 1A repeats the adsorption treatment, the desorption treatment, and the standby in each adsorption tank 13 in the normal operation during the normal operation.
Further, while the gas to be treated is introduced into one of the three, the desorption gas is introduced into the other one, and the other one is in the standby state. Specifically, during the adsorption process in the adsorption tank A13a, the desorption treatment is performed in the adsorption tank B13b, and the adsorption tank C13c is put into a standby state. Similarly, during the adsorption treatment in the adsorption tank B13b, the desorption treatment is carried out in the adsorption tank C13b, and the adsorption tank A13a is put into a standby state. Similarly, during the adsorption treatment in the adsorption tank C13c, the desorption treatment is carried out in the adsorption tank A13a, and the adsorption tank B13b is put into a standby state. This is repeated.

As shown in FIG. 3B, in the organic solvent treatment apparatus 1A, the gas to be treated is used in the other two adsorption tanks A13a and the adsorption tank B13b while one adsorption tank C13c is performing the regeneration treatment. By alternately carrying out the adsorption / desorption treatments, the gas to be treated containing the organic solvent can be continuously cleaned. In this case, the organic solvent treatment apparatus 1A has two steam lines 22, one of which is used to introduce superheated steam for the regeneration treatment of the adsorption tank C13c, and the other one is the adsorption tank A13a and adsorption. It is used to introduce water vapor for desorption treatment in tank B13b.

Note that FIG. 3B shows, as an example, a state in which the adsorption tank C13c is subjected to the regeneration treatment, and the adsorption tank A13a and the adsorption tank B13b are repeatedly subjected to the adsorption / desorption treatment. Similarly, the adsorption tank B13b and the adsorption tank C13c repeat the adsorption / desorption treatment while the adsorption tank A13a is performing the regeneration treatment, and the adsorption tank C13c and the adsorption tank C13c and the adsorption tank C13c are performing the adsorption treatment while the adsorption tank B13b is performing the regeneration treatment. The tank A13a repeats the adsorption / desorption process.

When the regeneration process in one adsorption tank C13c is completed, the regeneration process is started in order from the adsorption tank 13 in the desorption treatment among the other two adsorption tanks A13a and the adsorption tank B13b. In this way, the regeneration process in all the adsorption tanks 13 (adsorption tank A13a, adsorption tank B13b, and adsorption tank C13c) is continued.

When the regeneration treatment in all three adsorption tanks 13 is completed (when the regeneration operation is completed), the organic solvent treatment apparatus 1A operates the exhaust gas blower 12 again to introduce the gas to be treated into the adsorption tank 13 and adsorb it. Carry out the process. Then, when the measured value of the clean gas discharged from the clean gas discharge duct 17 by the VOC concentration meter 25 is less than or equal to the set concentration value, the normal operation is started, and when the concentration value is still exceeded, three again. Regeneration processing is performed on all the adsorption tanks 13 (regeneration operation is performed).

(Example)
Hereinafter, the present invention will be specifically described with reference to examples using the organic solvent treatment apparatus 1A of the present embodiment, but the present invention is not limited to the following contents.

(Example 2-1)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1 ppm of octamethylcyclotetrasiloxane was introduced into the adsorption tank A13a by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and the adsorbent 14 of the adsorption tank A13a was used for 10 minutes. Adsorption treatment was performed. At this time, the numerical value of the VOC concentration meter 25 (VOC concentration of the clean gas) was 1 ppm or less. Further, water vapor was introduced into the adsorption tank B13b that adsorbed the organic solvent, and the desorption treatment was performed for 10 minutes. The desorbed gas containing the organic solvent was supplied from the desorbed steam discharge port 19 to the condenser 32 via the desorbed steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank C13c that had been desorbed was placed in a standby state for 10 minutes until it was subjected to the next adsorption treatment.

By repeating the above three states (adsorption treatment, desorption treatment, standby state) in order while switching the adsorption tank 13, the mixed gas containing toluene and octamethylcyclotetrasiloxane was continuously treated for 170 hours.

When the mixed gas was continuously treated for 170 hours, the value of the VOC concentration meter 25 exceeded 100 ppm. Therefore, superheated steam at 180 ° C. was introduced into the adsorbent tank 13 in the standby state for 1 hour to regenerate the adsorbent 14. After the regeneration treatment with superheated steam was performed in all three adsorption tanks 13, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. It was confirmed that the value of the VOC concentration meter 25 at this time was 1 ppm or less, and the adsorbent 14 was sampled to measure the residual amount of octamethylcyclotetrasiloxane and its polymer.

(Example 2-2)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1 ppm of octamethylcyclotetrasiloxane was introduced into the adsorption tank A13a by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. It was. At this time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, water vapor was introduced into the absorption / adsorption tank B13b that adsorbed the organic solvent, and the desorption treatment was performed for 10 minutes. The desorbed gas containing the organic solvent was supplied from the desorbed steam discharge port 19 to the condenser 32 via the desorbed steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank C13c that had been desorbed was placed in a standby state for 10 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 170 hours by repeating the above three states while switching the adsorption tank 13 in order, the value of the VOC concentration meter 25 exceeded 100 ppm. Therefore, superheated steam at 200 ° C. was introduced into the adsorbent tank 13 in the standby state for 1 hour to regenerate the adsorbent 14. After the regeneration treatment with superheated steam was performed in all three adsorption tanks 13, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. After confirming that the value of the VOC concentration meter 25 at this time was 1 ppm or less, the adsorbent 14 was sampled and the residual amount of octamethylcyclotetrasiloxane and its polymer was measured.

(Example 2-3)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1 ppm of octamethylcyclotetrasiloxane was introduced into the adsorption tank A13a by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. It was. At this time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, water vapor was introduced into the adsorption tank B13b that adsorbed the organic solvent, and the desorption treatment was performed for 10 minutes. The desorbed gas containing the organic solvent was supplied from the desorbed steam discharge port 19 to the condenser 32 via the desorbed steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank C13c that had been desorbed was placed in a standby state for 10 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 170 hours by repeating the above three states while switching the adsorption tank 13 in order, the value of the VOC concentration meter 25 exceeded 100 ppm. Therefore, superheated steam at 250 ° C. was introduced into the adsorbent tank 13 in the standby state for 1 hour to regenerate the adsorbent 14. After the regeneration treatment with superheated steam was performed in all three adsorption tanks 13, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. After confirming that the value of the VOC concentration meter 25 at this time was 1 ppm or less, the adsorbent 14 was sampled and the residual amount of octamethylcyclotetrasiloxane and its polymer was measured.

(Example 2-4)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1.5 ppm of decamethylcyclopentasiloxane was introduced into the adsorption tank A13a by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. Was done. At this time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, water vapor was introduced into the adsorption tank B13b that adsorbed the organic solvent, and the desorption treatment was performed for 10 minutes. The desorbed gas containing the organic solvent was supplied from the desorbed steam discharge port 19 to the condenser 32 via the desorbed steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank C13c that had been desorbed was placed in a standby state for 10 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 90 hours by repeating the above three states in order while switching the adsorption tank, the value of the VOC concentration meter 25 exceeded 100 ppm for the clean gas discharged from the clean gas discharge duct 17. Therefore, superheated steam at 180 ° C. was introduced into the adsorption tank C13c in the standby state for 1 hour to regenerate the adsorbent 14. After the regeneration treatment with superheated steam was performed in all three adsorption tanks 13, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. It was confirmed that the value of the VOC concentration meter 25 at this time was 1 ppm or less, and the adsorbent 14 was sampled to measure the residual amount of octamethylcyclotetrasiloxane and its polymer.

(Example 2-5)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1.5 ppm of decamethylcyclopentasiloxane was introduced into the adsorption tank A13a by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. Was done. At this time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, water vapor was introduced into the adsorption tank B13b that adsorbed the organic solvent, and the desorption treatment was performed for 10 minutes. The desorption gas containing the organic solvent was supplied from the desorption steam discharge port 19 to the condenser 32 via the desorption steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank C13c that had been desorbed was placed in a standby state for 10 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 90 hours by repeating the above three states in order while switching the adsorption tank, the value of the VOC concentration meter 25 exceeded 100 ppm. Therefore, superheated steam at 200 ° C. was introduced into the adsorbent tank 13 in the standby state for 1 hour to regenerate the adsorbent 14. After the regeneration treatment with superheated steam was performed in all three adsorption tanks 13, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. It was confirmed that the value of the VOC concentration meter 25 at this time was 1 ppm or less, and the adsorbent 14 was sampled to measure the residual amount of octamethylcyclotetrasiloxane and its polymer.

(Example 2-6)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1.5 ppm of decamethylcyclopentasiloxane was introduced into the adsorption tank A13a by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. Was done. At this time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, water vapor was introduced into the adsorption tank B13b that adsorbed the organic solvent, and the desorption treatment was performed for 10 minutes. The desorbed gas containing the organic solvent was supplied from the desorbed steam discharge port 19 to the condenser 32 via the desorbed steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank C13c that had been desorbed was placed in a standby state for 10 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 90 hours by repeating the above three states in order while switching the adsorption tank, the value of the VOC concentration meter 25 exceeded 100 ppm. Therefore, superheated steam at 250 ° C. was introduced into the adsorbent tank 13 in the standby state for 1 hour to regenerate the adsorbent 14. After the regeneration treatment with superheated steam was performed in all three adsorption tanks 13, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. It was confirmed that the value of the VOC concentration meter 25 at this time was 1 ppm or less, and the adsorbent 14 was sampled to measure the residual amount of octamethylcyclotetrasiloxane and its polymer.

(Comparative Example 2-1)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1 ppm of octamethylcyclotetrasiloxane was introduced into the adsorption tank A13a by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. It was. At that time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, the adsorbent 14 of the adsorption tank B13b adsorbing the organic solvent was desorbed for 10 minutes using water vapor. The desorbed gas containing the organic solvent was supplied from the desorbed steam discharge port 19 to the condenser 32 via the desorbed steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank C13c that had been desorbed was placed in a standby state for 10 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 170 hours by repeating the above three states in order while switching the adsorption tank, the value of the VOC concentration meter 25 exceeded 100 ppm for the clean gas discharged from the clean gas discharge duct 17. Therefore, superheated steam at 150 ° C. was introduced into the adsorbent tank 13 in the standby state for 1 hour to regenerate the adsorbent 14. After regenerating all three adsorption tanks 13 with superheated steam, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. At this time, the value of the VOC concentration meter 25 was 62 ppm, and the adsorbent 14 was sampled to measure the residual amount of octamethylcyclotetrasiloxane and its polymer.

(Comparative Example 2-2)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1 ppm of octamethylcyclotetrasiloxane was introduced into the adsorption tank A13a by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. It was. At this time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, the adsorbent 14 of the adsorption tank B13b adsorbing the organic solvent was desorbed for 10 minutes using water vapor. The desorbed gas containing the organic solvent was supplied from the desorbed steam discharge port 19 to the condenser 32 via the desorbed steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank C13c that had been desorbed was placed in a standby state for 10 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 170 hours by repeating the above three states in order while switching the adsorption tank, the value of the VOC concentration meter 25 exceeded 100 ppm for the clean gas discharged from the clean gas discharge duct 17. Therefore, superheated steam at 170 ° C. was introduced into the adsorbent tank 13 in the standby state for 1 hour to regenerate the adsorbent 14. After regenerating all three adsorption tanks 13 with superheated steam, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. At this time, the value of the VOC concentration meter 25 was 31 ppm, and the adsorbent 14 was sampled to measure the residual amount of octamethylcyclotetrasiloxane and its polymer.

(Comparative Example 2-3)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1 ppm of octamethylcyclotetrasiloxane was introduced into the adsorption tank A13a by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. It was. At this time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, the adsorbent 14 of the adsorption tank B13b adsorbing the organic solvent was desorbed for 10 minutes using water vapor. The desorbed gas containing the organic solvent was supplied from the desorbed steam discharge port 19 to the condenser 32 via the desorbed steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank C13c that had been desorbed was placed in a standby state for 10 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 170 hours by repeating the above three states in order while switching the adsorption tank, the value of the VOC concentration meter 25 exceeded 100 ppm. Therefore, superheated steam at 260 ° C. was introduced into the adsorption tank 13 in the standby state for 1 hour to regenerate the adsorbent 14. After regenerating all three adsorption tanks 13 with superheated steam, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. At this time, the value of the VOC concentration meter 25 was 1 ppm or less, and the adsorbent 14 was sampled to measure the residual amount of octamethylcyclotetrasiloxane and its polymer.

(Comparative Example 2-4)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1 ppm of octamethylcyclotetrasiloxane was introduced into the adsorption tank A13a by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. It was. At that time, the value of the VOC concentration meter 25 installed at the clean gas discharge port was 1 ppm or less. Further, the adsorbent 14 of the adsorption tank B13b adsorbing the organic solvent is desorbed for 10 minutes using steam, and the desorbed gas containing the organic solvent is desorbed from the desorbed steam discharge port 19 via the desorbed steam line 31 to the condenser. It was supplied to 32, liquefied and condensed in an organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank C13c that had been desorbed was placed in a standby state for 10 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 170 hours by repeating the above three states in order while switching the adsorption tank, the value of the VOC concentration meter 25 exceeded 100 ppm. Therefore, superheated steam at 300 ° C. was introduced into the adsorbent tank 13 in the standby state for 1 hour to regenerate the adsorbent 14. After performing the regeneration treatment with superheated steam in all three adsorption tanks 13, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. At this time, the value of the VOC concentration meter 25 was 1 ppm or less, and the adsorbent 14 was sampled to measure the residual amount of octamethylcyclotetrasiloxane and its polymer.

(Comparative Example 2-5)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1.5 ppm of decamethylcyclopentasiloxane was introduced into the adsorption tank A13a by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. Was done. At that time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, the adsorbent 14 of the adsorption tank B13b adsorbing the organic solvent was desorbed for 10 minutes using water vapor. The desorbed gas containing the organic solvent was supplied from the desorbed steam discharge port 19 to the condenser 32 via the desorbed steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank C13c that had been desorbed was placed in a standby state for 10 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 90 hours by repeating the above three states in order while switching the adsorption tank, the value of the VOC concentration meter 25 exceeded 100 ppm for the clean gas discharged from the clean gas discharge duct 17. Therefore, superheated steam at 150 ° C. was introduced into the adsorbent tank 13 in the standby state for 1 hour to regenerate the adsorbent 14. After regenerating all three adsorption tanks 13 with superheated steam, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. The numerical value of the VOC concentration meter 25 at this time was 80 ppm, and the adsorbent 14 was sampled to measure the residual amount of decamethylcyclopentasiloxane and its polymer.

(Comparative Example 2-6)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1.5 ppm of decamethylcyclopentasiloxane was introduced into the adsorption tank A13a by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. Was done. At that time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, the adsorbent 14 of the adsorption tank B13b adsorbing the organic solvent was desorbed for 10 minutes using water vapor. The desorbed gas containing the organic solvent was supplied from the desorbed steam discharge port 19 to the condenser 32 via the desorbed steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank C13c that had been desorbed was placed in a standby state for 10 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 90 hours by repeating the above three states in order while switching the adsorption tank, the value of the VOC concentration meter 25 exceeded 100 ppm for the clean gas discharged from the clean gas discharge duct 17. Therefore, superheated steam at 170 ° C. was introduced into the adsorbent tank 13 in the standby state for 1 hour to regenerate the adsorbent 14. After regenerating all three adsorption tanks 13 with superheated steam, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. At this time, the value of the VOC concentration meter 25 was 43 ppm, and the adsorbent 14 was sampled to measure the residual amount of decamethylcyclopentasiloxane and its polymer.

(Comparative Example 2-7)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1.5 ppm of decamethylcyclopentasiloxane was introduced into the adsorption tank A13a by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. Was done. At that time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, the adsorbent 14 of the adsorption tank B13b adsorbing the organic solvent was desorbed for 10 minutes using water vapor. The desorbed gas containing the organic solvent was supplied from the desorbed steam discharge port 19 to the condenser 32 via the desorbed steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank C13c that had been desorbed was placed in a standby state for 10 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 90 hours by repeating the above three states in order while switching the adsorption tank, the value of the VOC concentration meter 25 exceeded 100 ppm. Therefore, superheated steam at 260 ° C. was introduced into the adsorption tank 13 in the standby state for 1 hour to regenerate the adsorbent 14. After regenerating all three adsorption tanks 13 with superheated steam, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. At this time, the value of the VOC concentration meter 25 was 1 ppm or less, and the adsorbent 14 was sampled to measure the residual amount of decamethylcyclopentasiloxane and its polymer.

(Comparative Example 2-8)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1.5 ppm of decamethylcyclopentasiloxane was introduced into the adsorption tank A13a by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. went. At that time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, the adsorbent 14 of the adsorption tank B13b adsorbing the organic solvent was desorbed for 10 minutes using water vapor. The desorbed gas containing the organic solvent was supplied from the desorbed steam discharge port 19 to the condenser 32 via the desorbed steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank C13c that had been desorbed was placed in a standby state for 10 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 90 hours by repeating the above three states in order while switching the adsorption tank, the value of the VOC concentration meter 25 exceeded 100 ppm for the clean gas discharged from the clean gas discharge duct 17. Therefore, superheated steam at 300 ° C. was introduced into the adsorbent tank 13 in the standby state for 1 hour to regenerate the adsorbent 14. After regenerating all three adsorption tanks 13 with superheated steam, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. At this time, the value of the VOC concentration meter 25 was 1 ppm or less, and the adsorbent 14 was sampled to measure the residual amount of decamethylcyclopentasiloxane and its polymer.

Comparative Examples 2-9 and 2-10 will explain an example in which the organic solvent treatment apparatus 1 (FIG. 1) is used and the regeneration treatment is constantly performed with superheated steam.

(Comparative Example 2-9)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1 ppm of octamethylcyclotetrasiloxane was introduced into the adsorption tank 13 by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. It was. At this time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, the adsorbent 14 adsorbed with the organic solvent was desorbed for 8 minutes using superheated steam at 250 ° C. The desorption gas containing the organic solvent was supplied from the desorption steam discharge port 19 to the condenser 32 via the desorption steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank 13 after the desorption treatment was put into a standby state for 2 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 170 hours by repeating the above state while switching the adsorption tank 13 in order, the value of the VOC concentration meter 25 exceeded 100 ppm. Therefore, superheated steam at 200 ° C. was introduced into each adsorption tank 13 for 1 hour to regenerate the adsorbent 14. After the regeneration treatment with superheated steam was performed in all the adsorption tanks 13, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. At this time, the value of the VOC concentration meter 25 was 1 ppm or less, and the adsorbent 14 was sampled to measure the residual amount of octamethylcyclotetrasiloxane and its polymer.

(Comparative Example 2-10)
A mixed gas at 45 ° C. containing 2000 ppm of toluene and 1.5 ppm of decamethylcyclopentasiloxane was introduced into the adsorption tank 13 by the raw gas blower 12 at an air volume of 4.0 Nm ³ / min, and adsorbed by the adsorbent 14 for 10 minutes. Was done. At this time, the value of the VOC concentration meter 25 was 1 ppm or less. Further, the adsorbent 14 adsorbed with the organic solvent was desorbed for 8 minutes using superheated steam at 250 ° C. The desorption gas containing the organic solvent was supplied from the desorption steam discharge port 19 to the condenser 32 via the desorption steam line 31, liquefied and condensed in the organic solvent and water, and then supplied to the recovery liquid tank 33. The adsorption tank 13 after the desorption treatment was put into a standby state for 2 minutes until it was subjected to the next adsorption treatment.

When the mixed gas was continuously treated for 90 hours by repeating the above state while switching the adsorption tank 13 in order, the value of the VOC concentration meter 25 exceeded 100 ppm. Therefore, superheated steam at 300 ° C. was introduced into each adsorption tank 13 for 1 hour to regenerate the adsorbent 14. After the regeneration treatment with superheated steam was performed in all the adsorption tanks 13, the supply of the mixed gas was started again, and the adsorption treatment with the adsorbent 14 was performed. At this time, the value of the VOC concentration meter 25 was 1 ppm or less, and the adsorbent 14 was sampled to measure the residual amount of decamethylcyclopentasiloxane and its polymer.

The results of Examples 2-1 to 2-6 are shown in Table 2, and the results of Comparative Examples 1 to 10 are shown in Table 3.

As shown in Table 2, in Examples 2-1 to 2-6, the clean air VOC concentration was 1 ppm or less, and it can be seen that the adsorbent cyclic organic silicon could be removed very efficiently.

As shown in Table 3, in Comparative Examples 2-1 and 2-2 and 2-5 and 2-6, the superheated steam temperature was 170 ° C. or lower, so that the cyclic organic silicon could not be efficiently removed from the adsorbent. , The clean air VOC concentration is a high value. Further, as shown in Table 3, in Comparative Examples 2-3, 2-4, 2-7, and 2-8, the superheated steam temperature was 260 ° C. or higher, and the VOC concentration of the clean gas was 1 ppm or lower. There is almost no difference from the results of Examples 2-1 to 2-6 shown in 2, and the amount of electricity used is high because the superheated steam is heated to a high temperature. Therefore, it can be seen that the energy efficiency is poor in Comparative Examples 2-3, 2-4 and 2-7, 2-8.

As shown in Table 3, Comparative Examples 2-9 and 2-10 constantly regenerate the adsorbent with superheated steam at 200 ° C. Therefore, although the cyclic organic silicon can be removed from the adsorbent, the energy efficiency becomes extremely poor. From this, it can be seen that the running costs are high in Comparative Examples 2-9 and 2-10.

It should be noted that each of the above-disclosed embodiments and examples is merely an example and is not limiting. In addition, the scope of the present invention also includes embodiments and examples in which the contents disclosed in each embodiment and each embodiment are combined. The technical scope of the present invention is valid depending on the scope of claims, and includes the description of the claims and the meaning equivalent to the description and all changes, modifications, replacements, etc. within the scope.

According to the present invention, the desorbable substance can be desorbed more efficiently, and the operation can be performed with excellent running cost, which can greatly contribute to the industrial world.

11 Gas supply duct to be treated 12 Raw gas blower 13 Adsorption tank 13a Adsorption tank A
13b Adsorption tank B
13c adsorption tank C
14 Adsorbent 15 Lower damper 16 Upper damper 17 Clean gas discharge duct 18 Steam supply port 19 Desorption steam discharge port 21 Steam supply line 22 Steam line switching valve 23 Superheated steam switching valve 24 Heater 25 VOC densitometer 31 Desorption steam discharge line 32 Condensation Vessel 33 Recovery liquid tank

Claims (7)

A suction tank filled with an adsorbent is provided, an organic solvent-containing gas is introduced into the adsorption tank, the organic solvent contained in the organic solvent-containing gas is adsorbed on the adsorbent, and the treated gas is discharged. In an organic solvent treatment apparatus that introduces a desorption gas into an adsorption tank to desorb the organic solvent from the adsorbent.
When the concentration of the organic solvent in the discharged treated gas is equal to or less than the set value, the introduction of the organic solvent-containing gas into the adsorption tank and the introduction of the desorption gas are alternately repeated.
When the concentration of the organic solvent in the discharged treated gas exceeds the set value, a regeneration gas having a temperature higher than that of the detachable gas is introduced into the adsorption tank.
A plurality of the adsorption tanks are provided.
When the concentration of the organic solvent in the discharged treated gas exceeds the set value,
The regeneration gas is introduced into a part of the adsorption tanks, and the organic solvent-containing gas and the desorption gas are alternately introduced into the remaining adsorption tanks. The organic solvent treatment apparatus is characterized in that the process of repeatedly selecting the above-mentioned part of the adsorption tanks into which the regenerating gas is introduced is sequentially selected until all of the plurality of adsorption tanks are selected. The organic solvent treatment apparatus according to claim 1, wherein the regenerating gas is superheated steam at 180 to 250 ° C., and the desorption gas is steam having a temperature equal to or lower than the temperature of the regenerating gas. The organic solvent processing apparatus according to claim 1 or 2, wherein the organic solvent-containing gas contains organic silicon. The organic solvent treatment apparatus according to claim 3, wherein the organic silicon is cyclic organic silicon. When the organic solvent concentration in the discharged treated gas is less than or equal to the set value,
The organic solvent treatment apparatus according to any one of claims 1 to 4, wherein the organic solvent-containing gas is introduced after a period during which the gas is not introduced after the introduction of the desorption gas. The organic solvent treatment apparatus according to any one of claims 1 to 5, wherein the adsorbent is a fibrous activated carbon. A plurality of adsorption tanks filled with an adsorbent are provided, an organic solvent-containing gas is introduced into the adsorption tank, the organic solvent contained in the organic solvent-containing gas is adsorbed on the adsorbent, and the treated gas is discharged. A method of supplying gas to an organic solvent treatment apparatus that introduces a desorption gas into the adsorption tank to desorb the organic solvent from the adsorbent.
When the concentration of the organic solvent in the discharged treated gas is equal to or less than the set value, the organic solvent-containing gas and the desorption gas are alternately supplied to the adsorption tank.
When the concentration of the organic solvent in the discharged treated gas exceeds the set value, a regeneration gas having a temperature higher than that of the detachable gas is supplied to the adsorption tank.
When the concentration of the organic solvent in the discharged treated gas exceeds the set value,
The regeneration gas is supplied to a part of the adsorption tanks, and the organic solvent-containing gas and the desorption gas are alternately supplied to the remaining adsorption tanks. The supply method is characterized in that the process of repeatedly selecting the above-mentioned partial adsorption tanks for supplying the regeneration gas is sequentially selected until all of the plurality of adsorption tanks are selected.