JPH11244602A - Distillation separator - Google Patents

Abstract

PROBLEM TO BE SOLVED: To lessen the release of evaporated material into the air, to reduce the danger of its explosion when the evaporated material is flammable, and also to enable performing even in a vacuum environment. SOLUTION: A distillation device is provided with a vapor generating means I for filling the distillation device with vapor, an air discharge means III for removing air in the distillation device, and a vapor condensing means H for cooling and condensing vapor in the distillation device. A port open to the atmosphere of the distillation device is provided with a gas storage vessel IV whose volume can be increased and decreased in equilibrium with pressure outside the vessel. In this way, when a mixture of evaporated material and non-evaporated material is separated by distillation, the discharge of the evaporated material to the outside can be decreased, and when the evaporated material is flammable, by using an inert gas, the danger of its explosion can be reduced and the inert gas can be recycled.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a (pressure-reducing) distillation separation apparatus for separating a mixed substance into substances that evaporate and those that do not. This device is intended to reduce the risk of explosion, particularly when the evaporant is flammable, by reducing the emission of evaporant into the atmosphere.

[0002]

2. Description of the Related Art In the distillation separation of a substance that evaporates and a substance that does not evaporate, it is distillation that evaporates and condenses when viewed from the evaporated substance side, and is drying by distillation when viewed from the non-evaporated substance side.

When the evaporation component of the solvent evaporates, air corresponding to the evaporation vapor volume is pushed out of the apparatus. The extruded air contains vapor of the evaporating component and is lost accordingly. Organic solvent vapor is a global warming substance and often has harmful components.

[0004] In the vacuum distillation, when the air in the distillation apparatus is eliminated, the eliminated air contains vapors of evaporating components, resulting in a loss and environmental pollution.

[0005] Further, when the evaporation component is flammable, there is a danger of explosion due to mixing with air.

[0006] Distillation and drying are processes utilized in many industries. One of the major technical fields that require a drying process is CF
There was a step of using C-113 and 1,1,1-trichloroethane (hereinafter referred to as chlorofluorocarbon) as a detergent. CFCs have been used in large quantities because they are relatively inexpensive, have low latent heat of evaporation and low specific heat, are nontoxic, have no corrosiveness, and are easy to dry.

However, since fluorocarbons and the like are found to be ozone depleting substances, they have been completely abolished, and water-based detergents and hydrocarbons having a high flash point (high boiling point) have attracted attention. The water-based cleaning agent is a liquid that adheres to the dried product, and has a large specific heat and latent heat of evaporation. A high flash point hydrocarbon solvent has a boiling point of 1%.
Above 70 ° C., both detergents were difficult to dry.

For this reason, a technique of rinsing and washing with hydrofluoroether (hereinafter referred to as HFE) which is a solvent having a small latent heat of evaporation, a specific heat and a surface tension has been developed. This solvent has zero ODP (Ozone Depleting Potential Ozone Depletion Coefficient) and has a considerably lower GWP (Global Warming Potential). However, this solvent has a high fluorine content and is more expensive than Freon or the like. And the drying method using this solvent follows the conventional drying method of CFCs or the like. That is,
After the dried product is rinsed, it is heated in a solvent vapor layer and evaporated and dried with its own heat at the upper part of the vapor layer. This vapor is recovered by cooling the surrounding cooling pipes and condensing it. When the apparatus was open and the cooling temperature was set to 0 ° C. or less, ice adhered to the cooling pipe, making it difficult. The liquid adhering to the dried product could not completely evaporate and was sometimes evaporated and dried outside.

Further, since a large amount of waste liquid of a high flash point hydrocarbon solvent which is promising as a cleaning agent is likely to be generated in the future, there is an increasing need to reuse it in vacuum distillation. Explosion hazard is always present due to the organic solvent. Further, even in the distillation of ordinary organic solvents, there is no countermeasure against solvent loss from the air opening, and many small distillers exhaust the solvent vapor to the outside air and discard it.

The present invention has been made in view of the above-mentioned conventional problems, and is a (pressure-reducing) distillation separation apparatus for separating a mixed substance into substances that evaporate and those that do not. It is an object of the present invention to provide a device capable of reducing the emission to the atmosphere and reducing the risk of explosion when an evaporating substance is flammable.

[0011]

Means for Solving the Problems The distillation separation apparatus provided by the present invention is as described in the following (1) to (4).

(1) Steam generating means for filling the inside of the distillation apparatus with steam, air discharging means for removing air from the distillation apparatus,
Distillation separation characterized in that a gas storage container capable of increasing or decreasing the volume in equilibrium with the external pressure of the container is provided at the open-to-atmosphere opening of the distillation device having a vapor condensing means for cooling and condensing the vapor in the distillation device. Apparatus (hereinafter, referred to as a first distillation separation apparatus).

(2) steam generating means for filling the inside of the distillation apparatus with steam, air discharging means for removing air from the distillation apparatus,
After the air is discharged, the inside of the distillation apparatus is shut off from the outside to make the interior of the distillation apparatus air-free, and the vapor in the distillation apparatus without air is cooled and condensed to reduce the pressure inside the distillation apparatus. ,
A distillation apparatus having a vapor condensing means for creating a pressure difference between the vapor pressure of the mixture of substances in the apparatus and a condensing gas condensing means, and a gas capable of increasing or decreasing the volume in equilibrium with the external pressure of the vessel A distillation separation device provided with a storage container (hereinafter, referred to as a second distillation separation device).

(3) A steam generating means for filling the inside of the distillation apparatus with steam, an air discharging means for replacing air in the distillation apparatus with steam, and a distillation apparatus which shuts off the inside of the apparatus after discharging air from the outside. A pressure between the air shut-off means to make the environment air-free and the vapor in the air-free distillation device is cooled and condensed, the pressure in the device is reduced, and the vapor pressure of the mixture of substances in the device is reduced. A distillation apparatus provided with a vapor condensing means for making a difference, a condensing gas condensing means, and a gas storage vessel capable of increasing and decreasing the volume in parallel with the external pressure of the vessel; Hereinafter, it is referred to as a third distillation separation device.)

(4) The distillation apparatus according to claim 1, 2, or 3, further comprising means for introducing an inert gas (hereinafter referred to as a fourth distillation separation apparatus).

[0016]

(1) According to the first distillation separation device, air containing an evaporating component is collected in a gas storage container whose volume can be increased or decreased in equilibrium with the external pressure of the container at the atmospheric opening of the device. Therefore, loss of solvent vapor can be eliminated.

(2) According to the second distillation separation apparatus, it is possible to separate the substance which does not evaporate under reduced pressure and the substance which does not evaporate and collect the discharged air in a gas storage container to eliminate the loss of the evaporating substance. At the same time, when removing the separated substance from the decompression device, the loss of the evaporating substance can be reduced by utilizing the gas in the gas storage container for decompression.

(3) According to the third distillation separation apparatus, since the loss of the evaporating substance can be eliminated and the air in the apparatus is replaced by steam to create a reduced pressure environment, the mixed substance is heated, Heat can be applied to the mixed substance itself, and a pressure-reducing pump driven by electricity can be omitted, and danger of ignition by electricity can be prevented. Further, since a reduced pressure environment is created by heat, waste heat can be used.

(4) According to the fourth distillation separation apparatus, in addition to the effects of the above (1), (2) or (3), when the evaporation component is flammable, the air in the apparatus is previously converted into an inert gas. By replacing with, the risk of explosion can be reduced.

[0020]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, embodiments of the present invention will be described.
The embodiment will be described with reference to FIGS.

(Embodiment 1) FIG. 1 is a configuration diagram of a distillation separation apparatus of Embodiment 1. The main component of the mixed substance to be separated by distillation in this apparatus is a liquid. I is a steam generating means composed of the container α and the heating device A. A mixed substance β of an evaporating substance and a non-evaporating substance is placed in a container α, and heated by a heating device A to generate steam. II is a steam condensing means for cooling and condensing the generated steam. III is an air discharging means, and the air containing steam flows out from the outside opening. IV is a container for collecting exhaust gas, that is, a gas storage container whose volume can be increased or decreased in equilibrium with the external pressure of the container. B1 and B2 are check valves, and when the volume of the gas storage container IV is minimized, the check valve B
Gas enters from 1 and when it reaches a maximum, gas exits from check valve B2. If the gas storage container IV is enlarged, the check valve B
1 and B2 do not normally operate. C is a condensate storage container, γ
Is the distilled liquid (condensate) stored therein. D is a valve. F is a mixed substance storage tank.

The gas in the apparatus is sealed with a liquid and is not in contact with the outside air. The introduction of the mixed substance β and the discharge of the separated substance can be performed at the atmospheric pressure even if the outside air does not flow in and out due to the increase and decrease in the capacity of the gas storage container IV. When the mixed substance β is a flammable substance, the danger of explosion can be reduced by replacing the air in the apparatus with an inert gas in advance. Further, since the inert gas is liquid-sealed, there is no loss.

(Embodiment 2) The distillation separation apparatus shown in FIG. 2 is equipped with a decompression device VII, and discharges gas from a steam generation means I, a vapor condensation means II and a gas discharge means III in dotted lines, and discharges gas. In the gas storage container IV, the vapor condensation means VI, and the condensate storage container C. Then, the external shutoff means V, V
_1, a closed V _2, the steam generator I, the vapor condensing means II in the vacuum environment, heat and vapor condensation means II by heating device A
Is distilled under reduced pressure by cooling and condensing. The vapor condensing means II includes a heat exchanger IIa for condensing and a condensed liquid tank IIb, and the condensed liquid accumulates in a condensed liquid layer IIb. Vacuum breaking gas for taking out the separated material, open the external interrupting means V _2, gas storage vessels IV
Use the gas in When the mixed substance is flammable, it is preferable to replace the entire apparatus in advance with an inert gas. Also,
A steam condensing means VI is also provided outside the distillation apparatus VII,
Since the gas storage container IV and the condensate storage container C always have a certain degree of condensing function, the condensing capacity may be sufficient in some cases. When the distilled liquid γ is taken out without destroying the liquid seal, the loss of the inert gas is only the amount dissolved in the liquid and discharged.

(Embodiment 3) The distillation separation apparatus shown in FIG. 3 is an apparatus for removing air by extruding air in the distillation apparatus with steam and performing distillation under reduced pressure. For example, at the time of distillation of the mixture B having a solvent having a boiling point of 110 ° C., the mixture B
After the steam generation means I and the steam condensation means II are filled with steam, the inside of the dotted line is cut off by the external cut-off means V, V ₁ and V ₂ and the heat exchanger IIa is operated to reduce the pressure. Distillation is possible. The extruded air is stored in the gas storage container IV, the vapor condensation means VI, and the condensate storage container C. Vacuum breaking when taking out the distilled material and dry material, opens the external shut-off means V _2, utilizes an extruded air. When the mixed substance is a flammable substance, distillation is performed after replacing the entire apparatus with an inert gas in advance.

Although the vapor condensing means is not shown separately in the figure, the condensate storage container C and the gas storage container IV have the capability of the vapor condensing means VI.

(Embodiment 4) FIG. 4 shows a distillation separation apparatus when the mixed substance is a high flash point organic solvent. For example, boiling point 1
The distillation of a substance having a temperature of 70 ° C. or higher can be performed by the apparatus shown in FIG. 3 if the substance is heated to 170 ° C. or higher. Therefore, a vapor of a substance having a low boiling point (for example, a vapor having a boiling point of 100 ° C.) is generated by the steam generator I1, and the container α and the vapor condensing means II are filled with the vapor. ₁ , V
₂ is closed, and the heat exchanger IIa is operated to perform vacuum distillation.
Apparatus air enters the gas storage vessel IV, after the distillation was finished, opens the external shut-off means V _2, vacuum destroying the device in gas in the gas storage vessel IV, taking out separated material.

In this example, the one in which the steam generator I1 is added is referred to as steam generating means I.

(Embodiment 5) The distillation separation apparatus shown in FIG. 5 is provided with two gas discharge ports. When the air of the steam condensing means II is replaced with steam, the external shutoff means V ₁ , V
_3, closing the V _X, to prevent heating by steam introduction of vapor condensation means II. External shut-off means V
Open ₂ and do. The air removal of the steam generating means I and the air removal of the steam condensing means II can be performed separately. Vacuum distillation closes all external blocking means other than an external interrupting means V _X is
This is performed by cooling the heat exchanger IIa.

[0029] The air discharge of the vapor condensing means II uses such as vacuum pump, close the external interrupting means V _1, V _3, V _X by the pre-same means II to vacuum, steam generator I
The discharge of the air, after replacing discharged steam, close all external blocking means other than an external interrupting means V _X, the heat exchanger IIa
May be operated to perform vacuum distillation.

(Embodiment 6) FIG. 6 shows a distillation / separation apparatus for evaporating liquid adhering to a solid. The steam generator I1 generates steam or hydrofluoroether (HFE) steam,
The mixture is applied to the mixed substance β and heated, and at the same time, vapor of the evaporating substance is generated. The generated steam can be heated by the heating device A to be dried steam to speed up drying. And
The air inside the device is replaced with steam. After the air containing steam is discharged from the gas discharging means III, the condensable gas is cooled and recovered by the steam condensing means VI. The gas that does not condense is stored in the gas storage container IV. This gas is used for vacuum destruction when removing the separated substance. In the figure, the collected condensate γ is returned to the condensate storage container C and reused. Vacuum distillation closes all external blocking means other than an external interrupting means V _X performs heat exchanger IIa and cooled.

The mixed substance β is heated by steam, and the steam in the apparatus is condensed to cool the heat exchanger IIa, and is reduced in pressure. The mixed substance β also evaporates the adhered evaporant by its own heat, and is dried by vacuum distillation. In this example, the heating device is
It is used to heat generated steam and dry it.
In the present invention, any number of heating devices may be added where necessary.

(Embodiment 7) FIG. 7 shows a distillation separation apparatus provided with a rinsing function. A rinsing solution tank VIII is provided, and the rinsing liquid is heated by the pump P with the steam generator I1, the rinsing liquid is poured into the container α, poured into the mixed substance β, and rinsed. The rinsing liquid may be heated by the heating device A to generate steam at the same time as rinsing to replace air, or after rinsing, steam may be generated by the steam generator I1. By boiling sump rinsing liquid into the container α rinsed, after replacing the device air rinsing steam, and discharge the rinse liquid, after closing all external blocking means other than an external interrupting means V _X, heat The exchanger may be operated to dry the dried product under reduced pressure. Instead of storing the rinsing liquid in the container α, the cleaning liquid may be washed out by using a shower or the like. Further, the heating may be performed by the steam generation I1, and a high-temperature and high-pressure rinsing liquid may be introduced into the container α to generate flash steam. Vacuum distillation closes all external blocking means other than an external interrupting means V _X performs heat exchanger IIa and cooled.

(Embodiment 8) FIG. 8 shows a case where a cleaning tank IX is added to the distillation separation apparatus of Embodiment 7, and after cleaning with a cleaning liquid, the cleaning liquid is discharged. Thereafter, as shown in FIG. It is intended to be. In the container α, washing, drying, and rinsing steps can be performed.

(Embodiment 9) FIG. 9 shows an example of a distillation separation apparatus for heating a mixed substance when the temperature of the mixed substance is reduced by distillation under reduced pressure and evaporation of an evaporating component becomes impossible. After vacuum distillation close all external blocking means other than an external interrupting means V _X, close the external interrupting means V _X, valve D
_1, the open external interrupting means V _2, V _3, introducing a gas in the gas storage vessel IV in containers alpha, destroying the vacuum, after many gas amount of the heat medium, external interrupting means V ₂ and V ₃ is closed, the gas is heated by the heater E and sent to the container α by the blower G,
The mixed substance β in the container α is heated. The evaporating component evaporates, is discharged from the check valve B3, is condensed by the vapor condensing means VI, and is collected in the condensed liquid storage container C. Then, when the temperature in the container α rises and the vapor pressure increases, the external shutoff means V ₂
And closing the V _3, by opening the shut-off valve V _X, distilled under reduced pressure. This step may be repeated. It is preferable that the gas to be heated and introduced into the container α is distributed throughout the container α.

As shown in FIGS. 2 to 9, the inside of the container α of the steam generating means I under reduced pressure may be heated by using an electromagnetic wave. Since the electromagnetic wave can heat the mixed substance β under reduced pressure without a heat medium, there is a heating effect when the mixed substance B is the center of a solid as shown in FIGS.

When the amount of steam discharged from the air discharging means III in FIGS. 2 to 9 is small, the function of condensing the gas storage container IV is sufficient, and the steam condenser IV may not be needed. In the vacuum distillation drying by steam replacement in FIGS. 3 to 8, the steam condensing means II is not operated at the time of excluding air, but is shut off outside and then operated to perform vacuum distillation. When the mixture in FIGS. 1 to 9 is flammable, the air inside the chamber can be replaced with an inert gas in advance to reduce the risk of explosion.

[0037]

As described above, according to the present invention, since the above-described configuration is adopted, the following effects are obtained.

(1) When a mixed substance of an evaporating substance and a non-evaporating substance is separated by distillation, discharge of the evaporating substance to the outside can be reduced.

(2) When the evaporating substance is a flammable substance,
The use of inert gas can reduce the danger of the explosion. Further, the loss of the inert gas can be reduced by reusing it.

[Brief description of the drawings]

FIG. 1 is a configuration diagram of a distillation separation apparatus according to a first embodiment.

FIG. 2 is a configuration diagram of a distillation separation apparatus according to a second embodiment.

FIG. 3 is a configuration diagram of a distillation separation apparatus according to a third embodiment.

FIG. 4 is a configuration diagram of a distillation separation apparatus according to a fourth embodiment.

FIG. 5 is a configuration diagram of a distillation separation apparatus according to a fifth embodiment.

FIG. 6 is a configuration diagram of a distillation separation apparatus according to a sixth embodiment.

FIG. 7 is a configuration diagram of a distillation separation apparatus according to a seventh embodiment.

FIG. 8 is a configuration diagram of a distillation separation apparatus according to an eighth embodiment.

FIG. 9 is a configuration diagram of a distillation separation apparatus according to a ninth embodiment.

[Explanation of symbols]

I steam generator I1 steam generator II vapor condensation means IIa heat exchanger IIb condensate tank III air exhaust means IV container external pressure and a gas storage vessel V that may increase or decrease in volume in _{equilibrium, V 1, V 2, V} 3, V _X External shut-off means VI Vapor condensing means VII Decompression device VIII Rinse solution tank IX Cleaning agent tank A Heating device B1, B2, B3 Check valve C Condensate storage container P Pump D, D ₁ valve F Mixed substance storage tank α Container β Mixed substance γ Condensate G Blower E Heater

Claims (4)

[Claims] 1. A distillation apparatus comprising: a steam generating means for filling the inside of a distillation apparatus with steam; an air discharging means for removing air in the distillation apparatus; and a steam condensing means for cooling and condensing steam in the distillation apparatus. Wherein a gas storage container capable of increasing or decreasing the volume in equilibrium with the external pressure of the container is provided at the atmosphere opening port. 2. A steam generating means for filling the inside of the distillation apparatus with steam, an air discharging means for removing air from the distillation apparatus, and an inside of the distillation apparatus after the air is discharged to shut off the inside of the distillation apparatus. Steam that cools and condenses the vapor in the air-free distillation apparatus, creates a pressure difference between the pressure in the apparatus, and the vapor pressure of the mixture of substances in the apparatus. A distillation separation apparatus comprising: a distillation apparatus provided with a condensing means; and a condensing means for condensable gas and a gas storage container capable of increasing or decreasing the volume in equilibrium with the external pressure of the container. 3. A steam generating means for filling the inside of the distillation apparatus with steam, an air discharging means for replacing air in the distillation apparatus with steam, and an inside of the distillation apparatus after shutting off the inside of the apparatus after discharging the air. The pressure difference between the air shut-off means to make the air-free environment and the vapor in the air-free distillation device cooled and condensed, the pressure in the device is reduced, and the vapor pressure of the mixture of substances in the device is reduced. A distillation apparatus comprising: a vapor condensing means for producing a condensable gas; and a gas storage vessel capable of increasing or decreasing the volume in parallel with the external pressure of the vessel. 4. The distillation apparatus according to claim 1, further comprising means for introducing an inert gas.