JP2002370001A - Solvent separator - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a solvent separator equipped with a storage tank for storing a mixed solvent, a separation tank having a solvent heating part provided to the lower part thereof and having a cooling part provided to the upper part thereof and a circulating means for circulating the solvent between the storage tank and the separation means and constituted so that the mixed solvent is heated in the solvent heating part to evaporate a fluorine solvent and the evaporated solvent is liquefied and regenerated in the upper cooling part to be separated from the mixed solvent to be well separated into the fluorine solvent and a hydrocarbon solvent to be reutilized. SOLUTION: The solvent separator 3 is constituted so as to separate the mixed solvent D of the fluorine solvent B and the hydrocarbon solvent A into the fluorine solvent B and the hydrocarbon solvent A and equipped with the storage tank 35 for storing the mixed solvent D, the separation tank 38 having the solvent heating part 36 and the cooling part 37 respectively provided to the lower and upper parts thereof and the circulating means 48 for circulating the solvent D between the storage tank 35 and the separation tank 38. The mixed solvent D is heated in the solvent heating part 36 to evaporate the fluorine solvent B and the evaporated solvent B' is liquefied and regenerated in the upper cooling part 37 to be separated from the mixed solvent D.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION The present invention relates to a fluorine-based solvent which is a mixture of a hydrocarbon solvent used for cleaning a work and a fluorine-based solvent used for rinsing the hydrocarbon solvent adhered to the work. The present invention relates to a solvent separation device that separates hydrocarbon solvents.

[0002]

2. Description of the Related Art Generally, a hydrocarbon solvent (see HC) and a fluorinated solvent (HFE) are used for cleaning and rinsing a work.
However, if these two are mixed with each other, the cleaning ability is greatly reduced, so that it is necessary to separate both mixed solvents.

Therefore, conventionally, the specific gravity difference between a hydrocarbon solvent and a fluorine-based solvent (for example, the specific gravity of HC is about 0.8,
Although the specific gravity of HFE is about 1.52), attempts have been made to separate these two solvents at a specific gravity. However, the fluorine-based solvent dissolved in the hydrocarbon solvent is not sufficiently separated by the specific gravity separation. Therefore, conventionally, a mixture of both solvents has been disposed of.

[0004]

SUMMARY OF THE INVENTION The present invention relates to a storage tank for storing a mixed solvent, a separation tank having a solvent heating section at the bottom and a cooling section at the top, and a storage tank and a separation tank for storing the solvent. A circulating means for circulating the solvent is provided, and while the solvent is circulated, the mixed solvent is heated in the solvent heating section to vaporize the fluorinated solvent, and the vaporized solvent is liquefied and regenerated in the upper cooling section for mixing. An object of the present invention is to provide a solvent separation device that can be separated into a fluorine solvent and a hydrocarbon solvent and can be reused by being configured to be separated from a solvent.

[0005]

A solvent separator according to the present invention is a solvent separator for separating a mixed solvent obtained by mixing a fluorine-based solvent and a hydrocarbon solvent into a fluorine-based solvent and a hydrocarbon solvent, A storage tank for storing the mixed solvent, and a separation tank having a solvent heating unit at the bottom and a cooling unit at the top,
Circulating means for circulating the solvent between the storage tank and the separation tank; heating the mixed solvent in the solvent heating section to vaporize the fluorine-based solvent; and liquefying the vaporized solvent in the upper cooling section It is regenerated and separated from the mixed solvent.

The fluorinated solvent having the above constitution has a boiling point of about 60.
C., HFE having a specific gravity of about 1.52 (hydrofluoro
Ether). The hydrocarbon solvent having the above configuration may be set to HC (hydrocarbon) having a boiling point of 100 ° C. or higher and a specific gravity of about 0.8.

According to the above arrangement, when the mixed solvent in the storage tank is heated by the solvent heating section in the lower part of the separation tank while circulating the mixed solvent in the storage tank between the separation tank and the storage tank by the circulating means, The fluorinated solvent is vaporized, and the vaporized fluorinated solvent is liquefied and regenerated in the upper cooling section.

As a result, the entire amount of the mixed solvent can be satisfactorily separated into a fluorine-based solvent and a hydrocarbon solvent, and can be reused.

In one embodiment of the present invention, the heating temperature of the solvent heating section is set to be lower than the boiling point of the fluorine-based solvent. According to the above configuration, since the heating temperature is set to be equal to or lower than the boiling point of the fluorine-based solvent, and the fluorine-based solvent is slowly vaporized by so-called low-temperature heating, the vaporization of the hydrocarbon solvent in the mixed solvent can be prevented.

When the heating temperature is set to a high value, the hydrocarbon solvent has a higher boiling point than that of the fluorine-based solvent. Since the vapor of the hydrocarbon solvent is mixed with the vapor of the solvent to inhibit good separation, the fluorine-based solvent is slowly vaporized over a long time by the low-temperature heat treatment as described above. Note that the low-temperature heat treatment method can also be configured by means using an inclined surface using indirect heating.

In one embodiment of the present invention, a specific gravity separation tank for separating a fluorine-based solvent and a hydrocarbon solvent from each other is provided at a stage preceding the storage tank or the separation tank.

The specific gravity separation having the above structure is desirably performed under cooling conditions in view of the physical properties of the solvent. According to the above configuration, it is possible to improve the separation efficiency of both solvents as compared with a configuration in which heat separation is immediately performed without performing specific gravity separation processing.

[0013]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS One embodiment of the present invention will be described below in detail with reference to the drawings. The drawing shows a work cleaning and rinsing device provided with a solvent separation device, and in FIG.
A rinsing device 2 and a solvent separating device 3 are provided.

The above-mentioned ultrasonic separating apparatus 1 is provided with a bottomed cylindrical tank body 5 having a work entrance 4 formed by opening the upper part, and this tank body 5 is divided into storage tanks 8 by partitions 6, 7.
And a first-stage cleaning tank 9 and a second-stage cleaning tank 10.

Ultrasonic vibrators 11 and 12 are arranged in each of the cleaning tanks 9 and 10 described above. In the pre-stage washing tank 9, a circulation line 15 provided with a pump 13 and a filter 14 is connected between the outlet port and the inlet port to circulate the hydrocarbon solvent A.

Similarly, a circulation line 18 provided with a pump 16 and a filter 17 is connected between an outlet port and an inlet port of the post-stage washing tank 10 to circulate the hydrocarbon solvent A. ing.

Here, the above-mentioned hydrocarbon solvent A is H
C (hydrocarbon) is used. The properties of this HC are as follows. Physical properties of HC Specific gravity: 0.816 Flash point: 86 (PM, ° C) Boiling point: 100 ° C or higher Aniline point: 67 ° C In addition, heating means such as heaters are provided in each of the above-mentioned cleaning tanks 9 and 10 as necessary. Arrows a and b in the figure indicate overflow.

On the other hand, the above-described rinsing device 2 is configured as follows. That is, there is provided a bottomed cylindrical tank body 20 having an upper part opened to form a work entrance 19, a distillation tank 21 for forming a vapor of the fluorinated solvent 8 below the tank body 20, and a distillation tank 21 An ultrasonic bath 23 and a water separation bath 24 are formed adjacent to each other via a partition 22.

A cooling jacket 25 is provided around an intermediate portion of the tank body 20 in the vertical direction, while a cooling coil 26 is provided above the water separation tank 24.
Further, an ultrasonic vibrator 27 is provided in the ultrasonic tank 23, and a partition 28 having a lower end in non-contact with the bottom in the tank is provided in the water separating tank 24.

Then, a vapor layer C of the fluorinated solvent B is formed between the liquid levels of the distillation tank 21 and the ultrasonic tank 23 and the cooling jacket 25, while the solvent cooled by the cooling jacket 25 is formed in the water separation tank 24. The liquid obtained by cooling and regenerating the vapor of the vapor layer C by the cooling coil 26, that is, the liquid of the fluorinated solvent B is stored, and the specific gravity of water in the air and the fluorinated solvent B is separated (specific gravity of water 1.0, specific gravity of HFE) 1.52).

In the ultrasonic bath 23, a circulation line 31 provided with a pump 29 and a filter 30 is connected between the outlet port and the inlet port to circulate the fluorine-based solvent B. .

Here, the above-mentioned fluorine-based solvent B is H
FE (hydrofluoroether) is used. The physical properties of this HFE are as follows.

Physical properties of HFE Chemical formula C_FourF₉OCH_Three  Boiling point: 60 ° C Surface tension: 13.6 dynes / cm Specific heat: 0.28 cal / g / ° C Flash point: None Specific gravity: 1.52
May be provided, and arrows c and d in FIG.
This shows the data flow.

As shown by a virtual arrow e in FIG. 1, the work is immersed in the hydrocarbon solvent A in the pre-cleaning tank 9 of the ultrasonic cleaning apparatus 1 and subjected to ultrasonic cleaning. The substrate is immersed in the hydrocarbon solvent A in the cleaning tank 10 of the first stage to perform ultrasonic cleaning.

Next, the work after cleaning is rinsed by a rinsing device 2.
And immersed in the solution of the fluorinated solvent B in the ultrasonic bath 23 to remove HC attached to the work by HFE.
(Rinse), and then lift up once from the liquid to the vapor layer C, clean the work with steam, lift the work after steam cleaning to the drying area 32 and dry it, and then carry out the work for the next process. However, since HC and HFE are mixed with each other particularly in the above-described ultrasonic bath 23, this bath 2
The mixed solvent D of HC and HFE flows into the distillation tank 21 in which the liquid of No. 3 overflows as indicated by the arrow d.

The above-mentioned solvent separation device 3 uses the mixed solvent D
Is separated into a fluorinated solvent B and a hydrocarbon solvent A, the details of which are shown in FIG. This solvent separator 3 is shown in FIG.
As shown in the figure, a specific gravity separation tank 33 for separating the specific gravity of the fluorine-based solvent B and the hydrocarbon solvent A under cooling conditions, a preliminary tank 34 for storing the mixed solvent D, and a storage tank for storing the mixed solvent D A solvent pool tank 35, a heater 36 (heating means) as a solvent heating unit at the bottom, a separation tank 38 having a cooling unit 37 at the top, and a solvent regeneration unit 39. Here, the above-mentioned cooling unit 37 has a cooling coil 43 to be described later and is constituted by a cylindrical tank having an open top and a bottom, and receives a regenerating liquid of a liquefied solvent.

The bottom of the distillation tank 21 of the rinsing apparatus 2 shown in FIG. 1 is connected to the upper part of the specific gravity separation tank 33 shown in FIG. 2 by a line 40 so that the mixed solvent D flows into the specific gravity separation tank 33. ing.

The specific gravity separation tank 33 is provided with a partition portion 41 and a cooling coil 42. The cooling coil 42 and the cooling coil 43 arranged in the cooling unit 37 are connected in series, and are configured to flow cooling water or refrigerant to the two cooling coils 42, 43 via the cooling line 44.

The above-mentioned hydrocarbon solvent A and HFE as the fluorinated solvent B are dissolved in a large amount as the temperature rises and become completely mixed, while they have the property of separating when cooled, so that the mixed solvent D While being cooled by the cooling coil 42.

Since the specific gravity of HC as the hydrocarbon solvent A is about 0.8 and the specific gravity of HFE as the fluorine-based solvent B is about 1.52, HC floats above the HFE. However, even after this specific gravity separation, H
About 13 wt% of FE is mixed.

The mixed solvent D (mixed solvent having a mixing ratio of HFE of about 13 wt%) after the specific gravity separation overflows the partition 41 (see the arrow f), reaches the tank 45, and then flows into the line 46.
Is stored in the reserve tank 34 via the
Is supplied to the solvent pool tank 35 and stored.

The above-mentioned solvent pool tank 35 and separation tank 38 are connected to each other by a circulating means 48. That is, the solvent pool tank 35 and the separation tank 38 are connected by a discharge line 50 having a pump 49, and the lower part of the separation tank 38 and the lower part of the solvent pool tank 35 are connected by a reflux line 51.

When the mixed solvent D is separated, the pump 49 is driven to remove the mixed solvent D from the solvent pool tank 3.
5 and the separation tank 38, the heater 3
In step 6, the mixed solvent D in the separation tank 38 is heated to a temperature lower than the boiling point of the fluorinated solvent B, for example, 40 to 50 ° C. (this heating temperature is lower than the aniline point of HC).

When the mixed solvent D is heated to a low temperature of 40 to 50 ° C., the fluorinated solvent B having a boiling point of about 60 ° C. is vaporized. It is liquefied and regenerated in the provided cooling unit 37 to become a liquid fluorine-based solvent B and stored in the cooling unit 37.

Specifically, HFE having a concentration of 99 wt% could be recovered by subjecting 10 to 20 liters of the mixed solvent D to heat treatment and circulation treatment for 6 to 8 hours under the above conditions. .

Therefore, after such treatment, only HC remains in the lower portion of the separation tank 38 and in the solvent pool tank 35.

Therefore, the cooling unit 37 and the solvent regenerating unit 3
9 through a line 52, and the liquefied and recovered fluorine-based solvent B flows out to the solvent regenerating section 39 through the line 52, where it is subjected to, for example, specific gravity separation (specific gravity of water 1.0, specific gravity of HFE 1.52 After the separation of water in the solvent regeneration section 3
9 connecting the bottom of the rinsing device 9 with a predetermined portion of the rinsing device 2
3, the fluorinated solvent B after separation is returned to the rinsing device 2 for reuse, while the fluorinated solvent B is reused while being connected to the solvent pool tank 35 and a predetermined portion of the ultrasonic cleaning device 1 through a line 54.
The separated hydrocarbon solvent A is returned to the ultrasonic cleaning device 1 for reuse.

The above-mentioned line 54 is connected to the suction side of the pump 13 as shown in FIG. 1, and an on-off valve (not shown) such as a solenoid valve is interposed in the line 54. When the on-off valve is opened, the suction force of the pump 13 causes
The separated hydrocarbon solvent A can be returned to the ultrasonic cleaning device 1. The fluorinated solvent B separated from the line 53 can be returned to the rinsing device 2 by a water head or a pump (not shown) provided in the line 53.

As described above, the solvent separator of the above embodiment is
A solvent separator for separating a mixed solvent D in which a fluorinated solvent B (see HFE) and a hydrocarbon solvent A (see HC) are mixed into a fluorinated solvent B and a hydrocarbon solvent A, A storage tank (see solvent pool tank 35) for storing,
A separation tank (see separation tank 38) having a solvent heating section (see heater 36) at the bottom and a cooling section 37 at the top;
Circulating means 48 for circulating the mixed solvent D between the storage tank (see the solvent pool tank 35) and the separation tank (see the separation tank 38), and heating the mixed solvent D in the solvent heating section (see the heater 36). The fluorinated solvent B is vaporized, and the vaporized solvent B ′ is liquefied and regenerated in the upper cooling section 37 to be separated from the mixed solvent D.

According to this configuration, the mixed solvent D in the storage tank (see the solvent pool tank 35) is separated by the circulation means 48 into the separation tank.
(See separation tank 38) and the storage tank (solvent pool tank 3).
And the separation tank (separation tank 38).
Below the mixed solvent D in the solvent heating section (heater 3).
6), the fluorinated solvent B in the mixed solvent D is vaporized, and the vaporized fluorinated solvent B ′ is liquefied and regenerated in the upper cooling section 37.

As a result, the entire amount of the mixed solvent D can be satisfactorily separated into a fluorine-based solvent B and a hydrocarbon solvent A, which can be reused.

In addition, the solvent heating section (see heater 36)
Is set at a temperature not higher than the boiling point of the fluorinated solvent B (see the boiling point of HFE of about 60 ° C.). Since the heating temperature is set to be equal to or lower than the boiling point of the fluorinated solvent B and the fluorinated solvent B is slowly vaporized by so-called low-temperature heating, the vaporization of the hydrocarbon solvent A in the mixed solvent D can be prevented.

When the heating temperature is set high, the hydrocarbon solvent A is vaporized even though the boiling point of the hydrocarbon solvent A is higher than the boiling point of the fluorinated solvent B. Since the vapor of the hydrocarbon solvent A is mixed with the vapor of the fluorine solvent B in the vapor B ′, the good separation is hindered. It is to let.

Further, the storage tank (solvent pool tank 3)
5) or a separation tank (see the separation tank 38) is provided with a specific gravity separation tank 33 for separating the fluorine-based solvent B and the hydrocarbon solvent A from each other.

According to this configuration, both the solvents A and B are used for the configuration in which heat separation is immediately performed without performing specific gravity separation processing.
Separation efficiency can be improved.

FIG. 3 shows another embodiment of the solvent separating apparatus 3, in which an inclined surface 54 is provided in the separating tank 38, and the mixed solvent D is indirectly heated to a low temperature by the heater 36. Even with such a configuration, substantially the same operation and effect as in the previous embodiment can be obtained. Therefore, in FIG. 3, the same portions as those in FIG. 2 are denoted by the same reference numerals, and detailed description thereof will be omitted.

In correspondence between the structure of the present invention and the above-described embodiment, the fluorine-based solvent of the present invention is the same as the HFE of the embodiment.
(Hydrofluoroether), the hydrocarbon solvent corresponds to HC (hydrocarbon), the storage tank corresponds to the solvent pool tank 35, and the solvent heating unit is a heater 36 (heating means). And the separation tank corresponds to the separation tank 38, but the present invention is not limited only to the configuration of the above embodiment.

For example, instead of HFE, the fluorine-based solvent may be another fluorine-based inert solvent such as HFC, PFC, HCFC, FC, and the like. Other hydrocarbon solvents such as Ichi Kogyo Seiyaku Co., Ltd.) may be used.

[0049]

According to the present invention, a storage tank for storing a mixed solvent, a separation tank having a solvent heating section at a lower part and a cooling section at an upper part, and a solvent between the storage tank and the separation tank are provided. With a circulating means for circulating, while circulating the solvent, the mixed solvent is heated in the solvent heating unit to vaporize the fluorinated solvent,
By configuring the vaporized solvent to be liquefied and regenerated in the upper cooling section and separated from the mixed solvent, there is an effect that the solvent can be well separated into a fluorine-based solvent and a hydrocarbon solvent and reused.

[Brief description of the drawings]

FIG. 1 is an explanatory view of a work cleaning and rinsing device provided with a solvent separation device of the present invention.

FIG. 2 is a system diagram showing a solvent separation device of the present invention.

FIG. 3 is a system diagram showing another embodiment of the solvent separation device.

[Explanation of symbols]

 A: hydrocarbon solvent B: fluorine-based solvent D: mixed solvent 33: specific gravity separation tank 35: solvent pool tank (storage tank) 36: heater (solvent heating unit) 37: cooling unit 38: separation tank (separation tank) 48 ... Circulation means

 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 4D076 AA12 AA22 AA24 BA02 BA05 BC03 DA14 DA22 FA02 FA11 FA31 HA05 JA03

Claims (3)

[Claims] 1. A solvent separating apparatus for separating a mixed solvent in which a fluorinated solvent and a hydrocarbon solvent are mixed into a fluorinated solvent and a hydrocarbon solvent, comprising: a storage tank for storing the mixed solvent;
A separation tank having a solvent heating section at the bottom, a cooling section at the top, and a circulating means for circulating the solvent between the storage tank and the separation tank are provided, and the mixed solvent is heated by the solvent heating section. ,
A solvent separator that vaporizes a fluorinated solvent, liquefies and regenerates the vaporized solvent in the upper cooling section, and separates it from the mixed solvent. 2. A solvent separating apparatus according to claim 1, wherein the heating temperature of said solvent heating section is set to be lower than the boiling point of the fluorine-based solvent. 3. The solvent separating apparatus according to claim 1, wherein a specific gravity separation tank for separating a fluorine-based solvent and a hydrocarbon solvent from each other in a specific gravity is provided upstream of the storage tank or the separation tank.