JPS58216704A - Method and apparatus for at least partially separating one kind of liquid component of solution - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed description of the invention]

The present invention maintains the solution and distillate separated from each other by a porous separating wall that is permeable only to the vaporous distillate and maintains the solution and distillate in agitated contact. The conversion of the solution to the vapor phase is carried out on the solution side of the pores of the gold porous separator and by converting the solution to the vapor phase in a manner that causes the vaporous distillate to diffuse through the pores to the distillate side. The present invention relates to a method and apparatus for at least partially separating at least one liquid component. From U.S. Pat. No. 3,361,645, a beverage is prepared from saline water in which water vapor from the liquid is diffused into the interior of a tube through a water vapor permeable silicone rubber f and conveyed from the kernels together with a carrier gas, e.g. air, to a condenser. Devices for harvesting water are known. In this case, steam transport with the aid of a carrier gas is carried out either by means of a fan or by means of a vacuum pump. Therefore, in this case, water vapor condenses! IFi does not already take place inside the tube. At this time, the saline water is heated to a temperature between ambient temperature and boiling temperature. From DE 25 34 780 A1 a process is known for the separation of phenol from an aqueous mixture using an organic heavy membrane diaphragm which is selectively permeable to phenol. It consists in contacting the incoming stream in the liquid or vapor phase with a diaphragm, the permeate in this case being in the form of a phenol vapor, a solution of phenol or as a phenol complex solution. With this method, the absolute pressures in the charge zone and in the permeate zone can be varied considerably. In other words, the number ■H
A vacuum or overpressure from about 30 to 70 kf/- or more can be used. Above 1. According to the technical idea of the first-line publication, if the permeate band is lower than the liquid phase condition,
Pressure is generally not an important factor. However, when using vapor charge mixtures or diaphragm evaporation conditions, the high pressure in the charge zone can constitute a high chemical potential, which is preferred. If in this known process the permeate is present in the vapor phase,
Generally, the charge side of the diaphragm is adjusted to overpressure relative to atmospheric pressure, and the permeate side is adjusted to underpressure. From DE 16 19 749 A1, a method is known for separating liquid solutions and mixtures using porous shaped bodies, such as liquidphobic porous films, in contact with the liquid. It can also be operated under reduced pressure. This is because significantly less heat is required to achieve the same effect as when operating under normal or superpressure. The permeate flow rates achieved with these known methods were previously considered to be the greatest achievement. Surprisingly, however, in a method of the type described at the outset, a significantly higher permeate flow rate (i.e. per unit time and unit area of the effective porous separator from the solution side through the pores of the porous separator) than has been previously achieved. It has been found that it is possible to achieve an amount of distillate that diffuses through the distillate side. The object of the invention is therefore to provide a method of the type mentioned at the outset.
The object was to improve the chapter area of the porous separating wall and the amount of distillate or condensate obtained per unit time to be significantly increased over that hitherto achieved with the above-mentioned process. This problem is achieved according to the invention in a method of the type mentioned at the outset by means of pressure and/or temperature control during the continuation of the separation process, at least in at least a partial region of the immediate surroundings of the porous separating wall on the solution side. P can be solved by operating so that the boiling point range of F- is achieved. The driving force in the diaphragm distillation method of the present invention is the vapor pressure difference between the solution side and the distillate side. Such a vapor pressure difference is caused by the fact that the distillate is continuously transported out of the porous separation wall in a vapor state, or that the distillate side of the porous separation wall is constantly loaded with a liquid having a lower temperature than the solution. This is achieved by recovering the distillate condensed on the distillate side of the pores of the porous separating wall, ie by virtue of the temperature difference between the solution and the condensate. Advantageously, this cooling or carrier liquid consists of the condensed and cooled distillate itself. Mixing of distillate with other liquids is thereby avoided. This is particularly advantageous in those operations where the distillate itself is the original target substance and is not to be disposed of like waste. By the way, if the vapor pressure gradient between the solution side and the distillate side is the same and the distillate flow through the permeable diaphragm tt-, for example, the solution 1lIIIl can be raised by a factor of four just by reducing the pressure compared to the ambient pressure. Furthermore, it is sufficient that, according to the invention, at least the nodal area of that capital of the solution is achieved by reducing the pressure as described above in at least a partial region immediately around the porous separating wall in the solution. That it should be considered absolutely amazing. In this case, the boiling point l in the above term is pressure,
It is to be understood that the boiling point of a solution is dependent on the temperature and the concentration of the solution. This boiling point generally changes constantly. The position at which the respective boiling point or range thereof is achieved can also vary. Advantageously, the pressure and temperature curves on the solution side should be controlled such that at least the respective boiling point range of the solution is achieved over the entire solution side, but at least along the entire porous separator. In the present invention, the boiling point range in each case means whether the absolute temperature of the solution expressed in Kelvin is at most 3 degrees lower than the boiling temperature corresponding to the total prevailing pressure at the local position f in question;
Or in other words, the temperature T of the solution is at least 0.97
Ta (here -1i, Ts is the boiling temperature of the solution at the measurement point). The method of the invention uses a vacuum evaporation or Fi
It cannot be compared to distillation. In other words, in the method of the present invention, the amount of distillate penetrating and diffusing into the distillate side through the pores of the porous separation wall can be increased by, for example, connecting the vapor chamber above the solution to a vacuum equipment station, thereby increasing the amount of distillate penetrating and diffusing only on the solution side. This is also done when reducing the pressure, particularly when adjusting the pressure to 4m. Another crucial difference between the method of the present invention and the above method using a classification stopper that operates in a vacuum is that in the method of the present invention, the liquid component to be separated of the solution is transferred from the liquid phase to the vapor phase. The problem is that the liquid surface penetrates into the pores of the porous separating wall and is thus subjected to capillary forces. Also, in terms of effects, the method of the present invention is significantly different from the above-mentioned classification stopper method. This is because the distillate obtained according to the invention is a condensate which cannot be achieved by a single evaporation step, i.e. for example a subsequent rectification or other evaporation step without distillation. This is because it has purity. As classified, the boiling point of a liquid is reached only when the vapor pressure of the liquid is equal to the ambient pressure. Therefore, at a given environmental pressure, the boiling point is achieved by increasing the temperature of the liquid;
This is achieved by reducing the environmental pressure at a given temperature. In a stationary nine-liquid column, the resting pressure in the lower region of the column is higher than at the surface, so the boiling point is only reached at a higher temperature in the lower region of the column than at the surface. When a liquid column is connected to a reduced pressure source, and assuming that the temperature distribution within the liquid is uniform, the boiling point will be reached when a predetermined reduced pressure is achieved at the surface of the liquid column. In the region below the boiling point is not achieved. This means that it is not possible to achieve a boiling state in the entire column simply by reducing the pressure above the liquid column while the temperature distribution is uniform. For example, in a water column with a height of lQm, the pressure at the deepest point is 0.981 nodal higher than at the highest point. Therefore. When a water column with a height of lOt is under atmospheric pressure, the boiling point temperature at the deepest position of the water column increases to about 120°C. Therefore, if such a water column is arranged upright, the height t
om contact with a hydrophobic porous separating wall and boiling the water by increasing the temperature or reducing the environmental pressure, the necessary precondition for the highest possible vapor flow permeation through the porous separating wall is the increase in the water column. It is only satisfied in the upper region. The above-mentioned disadvantages do not occur in the process of the invention, since in the process of the invention, by controlling the temperature and/or pressure of the solution on the solution side and/or on the distillate side, as much as possible of the porous separating wall is This is because the boiling point is achieved at least approximately on the solution side, at least in the vicinity. This can be achieved, for example, in the case of an upright porous separating wall of height lQ+n, for example, as follows. That is, the solution is guided along the porous separating wall from bottom to top, with the solution already reaching the boiling temperature t-W corresponding to the pressure when it approaches the porous separating wall, and in the process from bottom to top always having a local temperature. It is cooled to such an extent that it reaches a boiling temperature corresponding to the target pressure. On this occasion. Cooling takes place in any case by evaporation via the porous separating wall. If this cooling is too strong, so that the temperature in the solution falls below the boiling temperature corresponding to the respective (level-dependent) pressure, then heat can be supplied from the appropriate locations or the throughflow of the solution can be increased. can be compensated. On the other hand, if the amount of evaporation is too small compared to the flow rate of the solution, the solution boils violently (also called boiling) with the formation of strong steam bubbles up to a certain height.
Start. This can be avoided, for example, by reducing the flow rate conducted along the porous separating wall on the solution side. In the same way as for varying the flow tt, the pressure state can optionally also be distributed to a predetermined temperature state by incorporating additional flow resistors. The same applies if the solution is conducted essentially horizontally along a porous separating wall which is also arranged horizontally in this case. This means that in this case, in effect, the possibly small pressure loss (flow loss) causes a pressure difference in the solution along the porous separating wall, which in turn leads to very small (slightly different boiling temperatures). bring. If the pressure difference that can occur along a horizontally arranged porous separating wall due to flow losses alone is too small compared to the temperature drop of the solution that occurs due to the evaporation and possible heat losses that occur through the porous separating wall. The boiling point may be achieved or maintained within the solution that is not along the entire porous barrier. In this case too, the temperature drop in the solution and the pressure change state in the solution can be mutually matched and at least partially It can be ensured that the respective boiling point of the solution, at least the range thereof, is achieved within the range. If the porous separating wall consists of, for example, one or more tubes, the flow resistance in the tube can be increased, for example, by correspondingly reducing the internal diameter of the tube or by filling the tube with a filler. be able to. Furthermore, this means can be used, for example (1
) reducing the residence time of the liquid flowing through the pipe; (2)
) Causes at least semi-turbulent flow in the pipe at a small flow rate, (3)
It offers other advantages such as easy destruction of the available boundary layer within the tube wall. For the same purpose, it is also possible to fill the chamber surrounding the tube with a filling, which acts as a porous partition. In the question of which type of control is more suitable, it should be taken into account that the higher the temperature on the solution side, the greater the amount of evaporation will generally be. However, if it is not possible, or is only possible to a limited extent, to simultaneously convert at least one liquid component of the solution into the vapor phase and to supply heat, the above-mentioned On the solution side, the boiling point can also be achieved and maintained in the solution by simultaneously supplying heat with (sub)pressure control. On the solution side, pressure and temperature are controlled as much as possible along the entire porous separating wall. The method of maintaining the solution according to the invention at least as close as possible to the boiling point by In this case, it is advantageous to control the temperature, pressure and flow rate on the distillate side with corresponding devices.In certain situations, detailed below, Vi, the total boiling point in solution To achieve this, it is possible to forego the above-mentioned mutually matched fCIE power/temperature control and nevertheless obtain a distillate stream t which is in any case very slightly less than that, i.e. surprisingly, Under certain preconditions, starting from the previously known methods, the pressure required to bring about the boiling point (
It has been found that a significant increase in distillate storage capacity can be achieved simply by generating vacuum (reduced pressure) only within the pores of the porous separating wall. This operation can be effected, for example, simply by connecting only the porous separating wall directly to a device for generating pressure (reduced pressure). This operation therefore ensures that even if the bath liquid and the distillate (condensate) are, for example, at atmospheric pressure and both then have a temperature below the normal boiling temperature, the porous isolation By appropriately defining and adjusting the earth pressure (vacuum) in the pores of the wall, temperatures at least close to the boiling point can be achieved in the solution directly around the porous separating wall. This embodiment of the process according to the invention is so effective that it is often possible to dispense with additionally establishing a corresponding boiling pressure (reduced pressure) on the solution side. This mode of operation is therefore a particularly advantageous embodiment of the process according to the invention. Depending on the size and type of the porous separating wall, it may be advantageous to connect the porous separating wall with devices for generating (reduced) pressure at several points. Generating a vapor pressure corresponding to the temperature of the solution in the pores of the porous separator in the above-mentioned manner results in the porous separator being constructed in the form of a network, i.e. the pores are formed by gas- or vapor-permeable openings, passages, If the filament is constructed of filaments interconnected by holes etc., it is possible to perform 0T. This embodiment of the method of the invention provides that the porous separator consists of a thermally 0T plastic heavy material selected from the group of olefin-based diaphragms, condensation-direct diaphragms and oxidation-site diaphragms or mixtures thereof. is present in the form of a microporous cellular molded body, the molded body has an isotropic structure with a large number of spherical cells evenly distributed within the entire structure, and the adjacent cells are smaller than said cells. This can be carried out particularly effectively when they are communicated by holes having a diameter. Advantageously, the spherical cells of the microporous molded body as described above have an average diameter of 00.5 to
100 μm, the shape function 8 is 1 to 30, and the ratio 0/P of the average bubble size to the average diameter P of the pores connecting one bubble is 2:1 to 200:l, and! , of O
/ P is 0.2-2.4 and Lot 8 / O
is -1,4 to 1. In this case, the shape function %f3tt
(9 functions) are defined by analysis of mercury penetration curves. In order to carry out the method of the invention, at least a planar separating wall,
Microporous cellular moldings, which can be present in the form of planar diaphragms, tubes, hoses or hollow fibers, and a process for their production are known from DE 27 37 745 A1. This publication also describes on page 53 how to obtain eight functions. It is suitable as a porous separator for carrying out the process of the invention and is explained earlier in the process of the invention on the basis of its special pore structure.

[7] A molded body suitable for the embodiment described above, that is, an embodiment in which only the inside of the pores of the porous partition wall is adjusted to a pressure substantially corresponding to the vapor pressure of the solution, and a method for producing the same, are disclosed in the West German Patent Application Publication No. No. 2833493, No. 28336
No. 23 and No. 3,049,557. For example, a porous separator made of biaxially expanded polytetrafluoroethylene (PTB). It is only conditionally suitable for carrying out the process according to the invention, i.e. with this separating wall the embodiments of the process according to the invention described immediately above are not practicable or are at best impractical. It is only possible to implement it effectively. This is due to the different shape and arrangement of the pores and the different structure of the porous material. In the method of the present invention, 1! It must be carried out so that a pressure equal to, greater than, or less than atmospheric pressure is generated on the condensate side, and generally different pressures are generated locally.d! can. This can be done for example by adjusting the solution side to atmospheric pressure and a pressure higher than the "vapor pressure" of the solution, so that the entire pores of the porous separating wall, under the above-mentioned conditions, substantially correspond to the vapor pressure of the solution, and This means adjusting the pressure to a pressure that may be higher than the atmospheric pressure, and adjusting the pressure to a higher pressure than the pressure on the distillate [t-solution side. In this case, in order to maintain the necessary vapor pressure gradient, the distillate The (local) temperature of the condensate should be lower than the (local) temperature of the solution. In this embodiment of the method of the invention, too, the solution is at atmospheric pressure and Similar to the embodiment described above in which the vacuum pressure is adjusted to substantially correspond to the vapor pressure of the solution, at least an approximate range of boiling points is achieved in the solution directly around the porous separating wall. High permeation. An important prerequisite for achieving flow agility is that the process according to the invention does not utilize a carrier gas on the distillate side, since it is possible to avoid the high distillate production characteristic of the process according to the invention. This is because it has been found that the device cannot be achieved in the presence of a carrier gas or a foreign gas.The increase in efficiency that can be achieved with the method of the invention compared to previously known methods, i.e., unit area and unit of diaphragm area under otherwise identical conditions. The increase in the amount of distillate diffusing through the porous separator is often more than 7 times. This can be carried out subsequently directly on the surface of the porous separating wall, so that the condensate formed in this case is in contact with the porous separating wall.However, it is possible to carry out the distillate first in vapor form from the porous separating wall. However, it can also be condensed at another location, in which case the liquid distillate (condensate) does not come into contact with the porous separating wall.This can be carried out in a conventional condenser of the #! In this case, a pressure gradient constituted by a reduced pressure source, e.g. a vacuum pump, is generally required in order to assist in the removal of the vaporous distillate to such a condenser.Instead of the usual condensation Mechanical vapor compression methods known per se, for example using rotary piston compressors or radial fans, can also be applied to increase the vapor pressure W11, thereby also increasing the energy efficiency of the process. If the distillate is to be removed in vapor form from the porous separating wall, this operation should be carried out without a carrier gas, or the distillate should be condensed M on a condensing surface opposite the porous separating wall. If this is to be done, the intervening intermediate chamber filled with distillate vapor should not contain any gas that does not condense at the given temperature and pressure. The method of the invention is suitable not only for treating so-called pure solutions such as salt water, acids, etc., but also for treating liquid admixtures. It is also suitable for liquids and extracts, emulsions, etc. containing organic or inorganic particles in insoluble form and microorganisms in the submicron range. Accordingly, all liquids from which at least 1 m of the liquid component of the liquid can be at least partially separated in the method according to the invention are described as solutions in the present invention. The desired product is always #! This means that it need not be a filtrated distillate, but may be a concentrated solution or both. The boiling point of a solution is often different from the boiling point of the pure solvent or of the various mixture components in pure form. For this reason, the concentration-dependent boiling point of the solution often changes in the course of carrying out the process of the invention, which must be taken into account in the pressure and temperature control. Porous separators are permeable to vapor, but solution and lil!
Silk can be constructed from porous or microporous materials that are impermeable. Porous separators which have proven suitable for carrying out the process of the invention and which can also be present as diaphragms include nylon, acetic acid/Cl-acetate, polypropylene, polytetrafluoroethylene, polyethylene,
Polyvinylidene fluoride, polyvinyl chloride, cellulose, asbestos, silicates, minerals, or mixtures thereof. These materials should advantageously be non-wettable by either of the two liquids. This property of the porous separating wall generally suffices if it is present under the conditions under which the process of the invention is carried out, and may therefore, if appropriate, only be achieved by a corresponding pretreatment of the porous separating wall. Moreover, part of the method of the present invention surprisingly uses a solution that wets the porous separating wall in the solution state, but does not wet the condensate at atmospheric pressure, in which case only the solution side is wetted by the solution. This can be carried out by adjusting the pressure to a level corresponding to the vapor pressure of . The porous separating wall may be planar or non-planar, for example curved. They can be present in corrugated or closed form, for example as planar diaphragms (flat film-filled hose diaphragms), 'f' or hollow fibers. For carrying out the process of the invention, synthetic porous or microporous diaphragms are generally preferred as porous separating walls. In a further advantageous embodiment of the invention, the amount of solution and/or condensate present or only a portion thereof can be transferred by natural convection or by forced means, for example using natural pressure gradients or conveying devices known per se, such as pumps. The solution and/or condensate is caused to flow along the porous separator by moving the porous separator one or more times along the porous separator. in this case,
The solution and condensate can flow with respect to each other in countercurrent, countercurrent, crosscurrent or any arbitrary mixed flow. Any necessary heating or cooling of the solution and/or condensate can be carried out in the vicinity of the porous separating wall or in a step separate therefrom. Recovery of at least a portion of the amount of heat transferred by condensation of the distillate vapor and heat transfer from the solution through the porous separating wall to the condensate can be achieved by a method other than the aforementioned method and apparatus, such as by using a heat pump. is also possible and sometimes advantageous. The process according to the invention can be carried out in one step or in a multistep manner, ie the solution is conducted in succession along various optionally different porous separating walls and in this case concentrated stepwise and/or beforehand. The condensed distillate of step 1--can be used as a solution in the subsequent step if this format yields a purer distillate than in the stepwise procedure. Furthermore, the process according to the invention can also be used as a previous, intermediate or last step in a multi-step process, which is always connected for some reason before or after another distillation, evaporation or similar process. If the temperature on the solution side is high or the temperature difference between the solution and the condensate is large, the amount of distillate that permeates through the porous separating wall due to the high vapor pressure difference that occurs in this case will be reduced even if the boiling point is not reached in the solution. Even if the temperature is low or the temperature difference is small, the amount will be higher than when the temperature is low or the temperature difference is small. For this reason, the pressure drop on the solution side of the porous separating wall or in the pores until the boiling point is reached in any case causes a more or less high increase in the distillate vessel. In contrast, in an aqueous solution, if the condensate is water and the temperature in the solution is only, for example, 25° C. and the temperature in the condensate is, for example, 14° C., the amount of distillate in the process according to the invention is large. For example, 23 cm of Na01 at atmospheric pressure
This is 7.5 times or more compared to the method using a solution. In order to achieve a boiling point in the solution at least adjacent to the porous separating wall, on the distillate side, where the distillate is in liquid form,
That is, if condensate is present, it is generally not absolutely necessary to create a reduced pressure. however. If desired for other reasons, condensate 1! It has been found to be advantageous to adjust the IJ to a higher hydrostatic pressure than on the solution side; this measure prevents sudden leakage of the porous separating wall when the condensate is to be obtained in pure form. The solution is also prevented from reaching the condensate. By this means, the leakage flow from the condensate to the solution side that occurs in such leaks does reduce the distillate yield, however, the method is generally not harmful up to certain limits. This is because the condensate does not constitute any foreign substance to the solution. On the other hand, the difference between the hydrostatic pressure on the solution side and the hydrostatic pressure on the condensate side is due to mechanical deformation of the porous separating wall, and Such a situation can occur when the porous separating wall is present in the form of one or more very thin diaphragms.The porosity induced by such hydrostatic pressure differences In order to prevent undesired deformation of the separating wall, customary elements and means for supporting or reinforcing the porous separating wall can be applied, which however at least reduce the specific evaporation efficiency of the porous separating wall. No appreciable drop should occur. However, in most cases the hydrostatic pressure (vacuum) on both sides of the porous separator is at approximately the same level, i.e. the hydrostatic pressure acting on the porous separator is substantially It has been proven to be extremely advantageous to adjust the value to zero or nearly zero.In this case, in the present invention, if the difference between the two is in the range of 00 to 10% of the lower of the two,
The hydrostatic pressure is assumed to be approximately the same. Based on the high purity of the distillate obtained with the process according to the invention, the good thermal efficiency and the fact that the process according to the invention can be carried out even at low temperatures in the boiling range, the process according to the invention can be used for example for drinking water or even boiler water ( It is extremely suitable for obtaining completely desalinated water) from salt water. Therefore, it can also be used on ships. Another field in which the method of the invention can be effectively used is the post-treatment of electrolyzed wastewater as a preliminary step for metal recovery, caustic soda solutions, fruit juices, sugar-containing juices or aliquots such as milk in obtaining sand a Tsumugi, preparation of whey, production of sterile water and j in the laboratory! ! ! Pretreatment or production of pharmaceutical products, obtaining drinking water from urine in space travel, e.g. evaporative concentration of dye baths in the rayon dye industry, and other similar methods. An apparatus according to the invention suitable for carrying out the method according to the invention consists of at least one container. the vessel is divided by at least one porous separating wall into at least two chambers, one of which is configured to receive the solution and the other chamber to receive the distillate; In those types, the chamber receiving the container and/or the chamber receiving the distillate and/or the porous separating wall connects each of the components with a device for generating a reduced pressure (vacuum) or an overpressure. It is characterized by having a member that can do the following. According to the invention, at least the parts of the device according to the invention which operate under reduced pressure or overpressure are constructed in a manner that is sealed from the outside. In order to generate the reduced pressure proposed in the invention to achieve a static point at low temperatures, two chambers may be arranged and connected barometrically. This means that if the vessel is placed at a level corresponding to the desired boiling pressure and the supply and discharge conduits are configured as lifting conduits, the 4f/ri vessel is also placed at a low level and the liquid (solution or condensate) I
This means that the J-rack is fully connected. In this case, the chamber should be configured in a sealed manner to the outside and may be connected to a common or specific reduced pressure or vacuum device only for evacuation, for example with a porous separating wall. . Furthermore, the device according to the invention has, if desired, the necessary and per se known measuring, control and monitoring devices. However, these will not be described in detail since these devices are well known to those skilled in the art and are self-evident given the requirements set. In another embodiment, the device of the invention comprises a solution and/or
or a conveying device for supplying and discharging the distillate or condensate to and from the chamber and, if appropriate, a corresponding control mechanism which makes it possible to circulate the entire solution and/or condensate several times, or only in parts. and a return conduit. Furthermore, the apparatus according to the invention can have a device for heating and/or cooling the solution and/or the silk material, which device can, as necessary or desired, separate the solution and distillate or condensate chambers. Furthermore, the device according to the invention may consist of multiple chambers for solutions and/or multiple chambers for distillate or condensate, in which case The solution chamber and the distillate or condensate chamber may be connected in flow technology in parallel or in series.If the solution chamber and the condensate chamber are connected in series, KVi, solution and condensate Advantageously, they can be conducted in countercurrent to each other, so that, if desired, the solution and It is also possible to produce an equal or slightly different temperature difference between the condensate and the condensate.If the method of the invention is to be carried out discontinuously, that is, in the Nototsuchi manner, pump circulation etc. may be omitted. However, in this case as well, it is also possible to provide a stirring device or a mixing device to bring the solution and condensate into ring motion.It is advantageous to provide a heating device and a cooling device. If a boiling temperature so high as to require an overpressure for this purpose is desired, the chamber can be connected to a riser pipe of a corresponding height and a liquid column of a corresponding height can be used to achieve the desired overpressure. This can likewise be achieved without the use of risers by means of air cushions or by means of correspondingly dimensioned circulation pumps and throttling mechanisms.In vessels of closed construction, The vapor pressure, which corresponds to the temperature of the liquid and corresponds to the boiling pressure in the absence of gas, is automatically adjusted. Advantageously, the device according to the invention has a porous separating wall configured in a network, i.e. according to the present invention. As already detailed in the general description of the inventive process, it is open on the solution side and on the distillate side and is open through so that the vaporous distillate can diffuse from the solution side to the distillate side. The resulting pores are crossed and connected by gas- or vapor-permeable openings, passageways, capillaries, pores, etc. If a gas is dissolved in the solution, the solution is It may be advantageous to degas in a manner known per se. This operation is advantageous when the boiling point in the solution is reached only in the region of the porous separating wall and not before. For this purpose, a corresponding degassing device should be provided in front of the storage chamber for the solution, since the device according to the invention generates a pressure in the borehole that substantially corresponds to the respective vapor pressure of the solution. Appropriate for In the case of a porous separating wall constructed in the form of a mesh, it is advantageous if at least the pattern 1c should be connected to a pressure reduction device or an overpressure device. Next, the present invention and its effects will be explained in detail with reference to embodiments of the present invention apparatus and the present invention method shown in schematic drawings and graphs. In the embodiments of the apparatus of the present invention shown in FIGS. 1 to 10, all position numbers with the symbol a indicate the part on the effluent side, and all position numbers with the symbol a indicate the part on the distillate side or #. Part of the plaited side is shown. Identical parts are numbered the same in all drawings. FIG. 1 shows the following parts of a device according to the invention: two chambers 1" separated by a porous separating wall 2.
Container l divided into elb (la is solution chamber, 1b is condensate chamber), annular conduit 3a, 3b% solution supply conduit 4m
, discharge conduits 5a, 5b, heat exchangers 6a, 6b, pump 7
m, 7b, valve 8 a. Common or separate, but not shown - reduced pressure (vacuum)
or connections 9a, 9b to a device for generating overpressure as well as throttling mechanisms 13a, 13b, the mode of implementation of the method according to the invention using this device is clear from the above description of the method; The direction of flow is indicated by arrows in the drawing. The bonsiff a, 7b can be circulated via the annular conduits 3a, 3bi, possibly in a larger amount than the solution t% supplied via the supply conduit 4a or the amount of condensate discharged via the discharge conduit sbt-g. The solution can be regulated to the desired degree using the TA valve 8a, which is freshly supplied to the device. The temperature of the solution or condensate can be adjusted to the desired level using a heat exchanger 68 or 6bi-. Chambers 1a and lb
The pressure level within can be adjusted to the same or different values via the connecting conduit 9a or 9b by means of a device (not shown) for generating a reduced or overpressure. Discharge conduit 5
The concentrated solution via a is discharged via the discharge conduit 5b to form a distillate (condensate).The heat exchanger 6m or 6b
can also be placed in chamber 1a or lb. Instead of the conventional heat exchanger, it is also possible to use other, for example electrically operated heating or cooling devices (Peltier elements). These devices are particularly advantageous because they allow the supply or removal of heat in the immediate vicinity of the porous separating wall. It is also possible to utilize the wall of the container 1 itself as a heat transfer surface. The pressure reduction in the separating wall 2 can be achieved by appropriately adjusting the throttling mechanism 13m and 7b on the suction side even if the pressure reducing device (not shown) and the connecting conduits 9a and 9b leading to the device are omitted. , by creating a sufficiently large vacuum that is also effective in chambers 1a, lb. In the embodiment of the apparatus according to the invention shown in FIG. Flows along the porous separating wall 2 in a countercurrent to the flow.By arranging throttling mechanisms 13m, 13b behind the chambers 1a and 1b, the flow in the chambers 1a,
It is also possible to generate an overpressure at b. FIG. 2 shows a pair of chambers 1a, 1b connected in series. The solution flows into four chambers 1 atl in order from left to right on the drawing, and the distillate (condensate) flows into four chambers 1 btl.
flows from right to left. The inlet temperature t3 of the solution is lower than its outlet temperature t4, and the inlet temperature t1 of the condensate is lower than its outlet temperature t2. Furthermore, % t3 is greater than t2 and t
4 is smaller than tl. To adjust the liquid flow, use Habot3
It is possible to select so that t2:t4-11, that is, approximately the same temperature difference occurs between the solution and the distillate (condensate) at any of the four steps. It is also possible to take off a condensate sub-stream from the same place or from several places, said sub-stream being equal to the amount of condensate produced in each step. Similarly, it is also possible to optionally blend fresh solution into the solution stream between each step (chamber pair).If desired, heat may be added to heat or cool the liquid stream between each step. It is also possible to arrange an exchanger.This figure is for schematically illustrating the possibility of connecting several separating walls in series, so that it is possible to connect other devices, e.g. Connections, pumps, measuring and control devices and mechanisms, etc. for this purpose are not shown. In FIG. container 12
m, 12b and 14a are constructed as immersion vessels in which a riser pipe 10m for the solution and downcomers 11b and tta for condensate and concentrated solution open below the water surface of the vessel, and the vessel is connected to conduits 4a, 4b and 15a'ft can be filled or emptied continuously or discontinuously. The vacuum prevailing in the chambers 1a, 1b is determined by the height of the riser pipe 10a and the downcomer pipe 11a, 11b. pump 7
a, 7b Serves as a circulation pump for Fi solution or condensate. The new solution supplied to the chamber 1a is in the dipping container 12a.
and 14 m and can be throttled using valve 13a. Both chambers 1a, 1b may additionally be connected to a vacuum system w1, but their sole purpose may be for exhaust. In addition, the heat exchanger is a water riser pipe 10a,
It can also be provided in the circulation conduits 3a, 3b and/or the downcomers 11a, llb. Furthermore, the upper side of the chamber 1a for the solution can be designed, for example, as a solar collector and the lower side of the condensate chamber 1b can be provided with radiation fins. Finally, a conveying pump or a metering pump can also be arranged in the riser pipe 10a and/or the downcomer pipes 11a, 11b. By arranging the vessels 12a, 12L+ and 14b above, rather than below, the vessel 1 (elevated tank), the chambers 1a and 1b can be operated at overpressure. , the height of the overpressure is the (elevated) vessel 12a. It is defined by the level difference between inside 12b and 14a and inside porous separating wall 2. In this arrangement, the downcomers 10a, 11m, and Ilb in FIG. 3 become riser pipes. - (elevated), d vessels 12a, 12b and 14aI/'i serve as storage vessels in correspondingly large volumes or exclusively as leveling vessels in small volumes; The same applies to the arrangement of the three containers described above as dipping containers shown in FIG. The embodiment of the device according to the invention shown in FIG. 4 also exists in the embodiment shown in FIG. 1, so parts having the same functions are designated by the same numbers. It has the following components. That is, the solution supply ponzo 16a, the solution filter 17511 and the permeable diaphragm distillation (heat of vaporization) and distillate (condensate) from the solution.
It has a heat exchanger 18 which makes it possible to recover a part, or even a major part, of the thermal energy transferred by the VC. The heat t required to achieve the desired temperature at the inlet of the solution is supplied to the solution by a heat exchanger 6a just before the entrance to chamber 1a. In this embodiment of the device d according to the invention, the solution and condensate are also circulated by circulation pumps 7a and 7a. The amount of distillate leaving the circulation via the withdrawal conduit 5b corresponds to the amount permeating through the porous separating wall 2. The amount of solution leaving the circuit via the withdrawal conduit 5at- corresponds to the amount of solution supplied to the circuit via the supply conduit 4a minus the condensate ii exiting via the withdrawal conduit 5b. As is clear from FIG. 4, in this embodiment, the concentrated solution is taken from the location where the concentration of the solution is maximum and the temperature of the solution is lowest. Condensate removal takes place at the point where the condensate has its lowest temperature. FIG. 5 shows a particularly advantageous embodiment of a container 1 for carrying out the method according to the invention. In this embodiment, the porous separating wall 2 consists of a number of tubes. The tubes constituting the porous separating wall 2 are embedded at their ends in a tube base 21, which can for example consist of a customary casting for this purpose and which is connected between the individual chambers. Acts as an isolation wall. Furthermore, the container l has an inlet 24a for the solution (or distillate or condensate).
(24b) and an outlet 25a (25b)s; an inlet 22b (22a) and an outlet 23b (23a) for distillate or condensate (or solution); In this case, the solution can therefore be led through the tube, with the distillate (condensate) flowing around the tube. However, the opposite may be true. In FIG. 5, this is indicated in parentheses for both chambers 1a and 1b, with the possibility of selecting the opposite mode of operation. The tubes constituting the porous separator 2, and thus the container 1, may be of any length and may be arranged horizontally or vertically, as shown in FIG. In case of upright arrangement,
Corresponding to the length of the tube, there will be a difference in hydrostatic pressure and therefore boiling temperature between the highest and lowest positions, whereas in the case of a horizontal arrangement the pressure difference between the inlet and outlet sides will be substantially Only caused by unavoidable flows and losses. For the sake of completeness, it may also be advantageous to have the container shown in FIG. 5 and also in other figures in a tilted or intermediate position between a horizontal and an upright position. If an embodiment is chosen in which the container 1 is arranged so as to be pivotable from a horizontal to an upright arrangement or vice versa, the pressure state can be easily changed, possibly even during operation of the device. This type can be very advantageous, for example, for experimental or laboratory equipment, especially in such equipment where hoses are often used instead of rigid conduits. An important feature of the container l shown in FIGS. 5 and 5a is the (de)pressure chamber 19, which can be connected via a connection port 9c to a device for generating a reduced or overpressure. This outfit [111
9,9c, it is particularly advantageous to maintain the pressure in the pores of the porous isolation tube substantially at the vapor pressure of the solution, even if a pressure higher than the vapor pressure prevails in the chambers 1a and 1b. Can be adjusted to match pressure. The prerequisites for this are, as explained in detail above, that the walls of the tube constituting the porous separating wall are suitable for this mode of operation, i.e. made of a material structured, for example, in the form of a mesh. That's true. In this case, the network structure is to be understood within the scope of the invention as described in detail above. In some cases, it may be advantageous to arrange a large number of such short containers in series instead of a long container l with a (de)pressure chamber 19. However, it is also possible to provide such chambers 19 on both sides of the container l, ie two chambers 19 in one container l. Finally, more than two such chambers 19 can be arranged in one container. In this case, for the chambers 19 which are not located at the ends of the tubes, pipe/e channels 35 should be provided for the liquid flowing around the tubes, as shown in FIG. 5a. . In order to control the pressure (reduced pressure) prevailing within the pores of the porous separating wall 2, it is preferable to provide a pressure gauge 20 connected to one of the tubes. The connection between this type of porous tube and the pressure needle is not shown in detail in FIG. In the embodiment of vessel 1 shown in FIG. 5, the solution and the distillate (condensate) can be conducted in countercurrent flow as shown, provided that only one flow of both liquids It is also possible to direct the flow forward by reversing the direction (crossing). In view of the position numbers, there is no need to discuss Figure 5a in detail. Furthermore, position number 36
The filling body is shown in . In the case of wetting liquids, it is advantageous for the liquid to flow around the tubes, since otherwise such liquids would run the risk of being sucked into the chamber 19 through the tube walls. 6 and 7 show an embodiment of the device according to the invention in two different nine-sided views, in which the porous separating wall 2 is constructed as a plane plate or a diaphragm and the porous separating wall 2 It is made of a material that can generate vapor pressure only within the pores of No. 2. In this case, the (de)pressure chamber 19 is constructed in the form of an annular channel, into which the porous separating wall 2 opens on its four sides. The annular passage-shaped chamber 19 is hermetically sealed against the chambers 1a and lb. The rest of this embodiment is clear from the position numbers and does not seem to need to be explained again. In this case, the generation of a (reduced) pressure corresponding to the vapor pressure of the solution only within the pores of the porous wall 2 means that between the solution side 1a and the condensate side ]b, the porous wall 2 may It has the additional advantage that at least no problematic pressure differences arise, which could be dangerous. FIG. 8 shows that various pressures (reduced pressures) can be generated in the pores of the tubular porous separating wall 2 having a suitable pore structure, and the deworming pressure (reduced pressure) can be applied to the pressure source connection position. A measuring device is shown that can measure at different distances from 26. In the connecting position 26 , the tubular porous separating wall 2 is surrounded by a ring 27 with an annular channel 28 , which is sealed hermetically against the surroundings by a sealing ring 29 . The annular passage 28 can be connected via a conduit 30 to a device (not shown) for generating (low) pressure. Measurement position 31
The same part 27.28.29.30 as connection position 26
is located. However, in this case, the conduit 30 is connected to a pressure gauge 30. The measuring position 31 is slidably arranged on the tubular porous separating wall 2, so that at any distance from the connecting position 26 any magnitude of vacuum or overpressure can be created in the annular passage of the connecting position 26. It is possible to measure the (decreased) pressure prevailing throughout the pores of the porous wall 2, which occurs when the pores of the porous wall 2 are generated. For the measurement, the porous separator 2 is prepared without wetting the porous separator 2.
That is, it is immersed in a liquid that does not penetrate into its pores, such as water (which may be present in the container 32). In this case, the liquid also penetrates inside the tube, but the VC inside the pores does not penetrate due to the liquid-repelling property (non-wetting) of the porous separating wall. The apparatus for measuring the pressure within the pores of the porous partition #II wall 2 illustrated in FIG. 8 can also be used in the embodiment of the apparatus of the invention illustrated in FIG. For example, the planar distance i1 as shown in FIGS. 6 and 7! For walls, a measuring device 2 may be used, for example as shown in FIGS. 7a and 7b.
7.28.29 should be suitably modified and adapted to the planar shape of the porous separating wall. For these drawings,
There seems no need for further explanation. The pressure in the pores of the porous separating wall 2, shown in FIG. 8 and measured with a ratio measuring device, is the average value of the prevailing, for example slightly different, pressures in the individual pores. However, it has been found that the determination of this average value, when used in the method and apparatus of the invention, generally satisfies the specified requirements and allows good control and monitoring of the process. However, it is also possible to detect the pressure prevailing inside the pores in a locally significantly limited manner by means of pressure measuring probes whose dimensions are only a few fractions of the thickness of the porous separating wall 2. For this purpose, recesses (holes) corresponding to the dimensions of the probe can be provided at the desired locations and to the depth in the porous separating wall whose pressure is to be detected. The sonde 37 is then inserted into this recess (hole) and the recess (hole) together with the sonde therein is sealed from the outside. FIG. 5b shows such a measuring device - In the embodiment of the device according to the invention shown in FIG.
The distillate or condensate (or solution) can be conducted through the tubes. In this case, distillate or condensate chamber lb (or solution chamber 1a in the reverse mode of operation)
is constituted by the inside of the tube of the porous separating wall 2. Solution chamber 1 m (or distillate or condensate chamber 1 b in the reverse mode of operation) is constituted by container 10 chamber. Stirring 41134 to move the liquid in the container l
is provided. A driving device for this agitator 34 is not shown. Furthermore, the container l is designed in its lower region with a double wall, so that the intermediate chamber 33 formed thereby
can be filled with cooling or heating liquid as required. This embodiment of the device according to the invention is particularly suitable for discontinuous operation methods, ie so-called batch operation, in which case a solution (which solution should preferably be filled into a container l) is used. It is possible to concentrate very mildly. However, if desired, it is possible to fill the vessel l continuously with solution (or distillate or condensate in the reverse mode of operation); for this purpose it is customary to fill and empty the vessel l. Inlet and outlet 24m (24b) and 25a working for
(25b) i can be used. If, in this type of apparatus according to the invention, the distillate or condensate is conducted via a tube, the boiling point directly around the porous separating wall 2 on the solution side 1a can be easily determined, for example on the distillate or condensate side. 1b, ie by creating as low a pressure as possible in the conduit, for example a pressure equal to the vapor pressure of the condensate. If the distillate is to be removed in vapor form, lower pressures can be generated in the conduit. Furthermore, this embodiment is eminently suitable as a laboratory device in suitably miniaturized form, in this case a container (tank).
If it is necessary to raise the temperature of the solution present in 1 to the boiling point with a Bunsennomer or an electric heating plate and to collect the distillate without separating it, the tube forming the porous separating wall 2 may be Can be connected to water conduit. The embodiment of the device according to the invention shown in FIG. 10 is likewise suitable for discontinuous operation. In this case, the container l has a porous separating wall 2 which is planar, curved or of any other shape.
It is divided into two chambers 1a and lb for solution and condensate. Disposed within these two chambers 1a, lb are stirrers 34g and 34b, which keep the solution and condensate in motion. Further, a heating device 6a, for example a heat exchanger, is arranged in the chamber la, and a cooling device 6b is arranged in the chamber lb. In order to operate the device, it may be advantageous to fill chamber lb at least partially with condensate or a condensate-like liquid at the start of operation. An overflow port (not shown) can be provided at the highest point of the chamber 1b, so that the chamber 1b is always filled with condensate, thus keeping the porous separating wall completely covered M. sex is provided. Instead of the heat transfer devices 6a and 6b shown in FIG. 10, the chambers 1m and 1b'6 are surrounded by heating or cooling jackets, as shown in FIG. 9 (indicated at 33 in that drawing). You can also. Conversely, other heating or cooling devices may also be used in the apparatus shown in FIG. Chambers 1a and lb and porous septum 1111v
2 can also be connected to a device that generates a vacuum or a lotus field. In this case as well, as shown in FIGS. 5 to 8 and described in detail with respect to the Sowara drawings,
A measuring device may be provided to monitor the force (in the hole of) F. In FIGS. 1 to 7, 9 and 10, the chambers 1a and 1b are fully sealed 11. However, in the case of a bending chamber that operates at overpressure or underpressure, it may also be designed as an open container. Furthermore, these drawings VC do not show, for the sake of clarity, any necessary measuring, controlling or monitoring equipment for pressure, temperature, liquid flow caps, #changes, etc. When the apparatus of the present invention is first put into operation, the general V (condensate is not present, so unless the distillate is released in vapor form), the condensate Md (lllllIlb) is the same as or similar to the condensate. In this case, it has often been found to be advantageous to first fill the distillate side with a cold liquid. For the case where the same vacuum prevails, the condensate that cannot be obtained by lowering the pressure on the solution side and the condensate side below atmospheric pressure is the condensate that can be obtained at atmospheric pressure. From the drawing, it can be seen that the total permeation through the porous separator wall is diffused and the resulting distillate water, which corresponds to the condensate, is approximately It increases by a factor of 5 and at a pressure of approximately 100 mbar it increases by a factor of approximately 7. This relationship has been found for different porous separators and different solutions. The experiment was carried out using an apparatus in which the porous barrier was placed at a higher level than the solution storage container and the condensate or concentrated solution. However, the container IIi was constructed with a closed structure and had a short vertical lift V.The solution storage chamber and the condensation storage chamber Fi were each connected to an independent pressure reducing device.Porous partition wall teeth,
It consists of six tubes of porous polypropylene arranged in a network as described in detail above. c, t'1
The tube was 420 cm long and had an outer diameter of 6.1 m and an inner diameter of 4.2 m. In this case, the solution flowed around the tube and the condensate flowed inside the tube. A circulation pump circulated the solution and condensate 25'Ot/b in the circuit and guided it along the porous saliva wall. At atmospheric pressure, the amount of condensate permeated through the porous separating wall was 3 mt/h of I O and 720 td/h at an absolute pressure of 100 mm IJ par. The temperature of the solution was approximately 77°C, and the temperature on the condensate side averaged 15°C. The boiling temperature of the solution at 100 mm 17 Parr was about 77°C. Figure 12 shows a comparison between a condensate container obtained by the method of the present invention and a condensate container obtained by a method other than the present invention.
, lh. The lower curves were obtained by carrying out the permeable diaphragm distillation process at atmospheric pressure and at various temperatures. On the other hand, it is clear that as the temperature of the solution increases, the condensate passing through the porous separating wall increases only slightly at first. In this case, the method of operation of the invention, i.e. if temperatures in the solution are achieved which are at most only slightly below the nine boiling temperatures defined above, a particularly proportional increase in the strength of the condensate results. That is clear. That is, in the lower curve 4I, only the line segment on the outer right side represents the operating method of the present invention. The upper curve always sets the pressure on the solution side to the vapor pressure vci!, which belongs to the respective temperature of the solution, so that according to the invention the boiling point is achieved on the solution side at all temperatures. I! It was obtained by adjusting the The two curves do not meet at about 100° C. (not shown), since at this temperature the boiling point is reached with both operating methods. Furthermore, from the comparison of both curves, it is found that the lower temperature range, e.g.
℃, twice the amount of condensate is achieved with the method of the invention (upper curve), but as the temperature increases, the difference in the amount of condensate becomes absolutely larger, although the proportion decreases. is clear. In this case, the condensate temperature was set constant at approximately 20°C. FIG. 13 shows the condensate cap obtained when varying the vacuum on the solution side at a constant solution temperature of 55c. This diagram also shows that the amount of condensate passing through the porous separating wall increases significantly and strongly at the point when the boiling point is reached in the solution, i.e. when the operation is carried out within the scope of the invention. Show that. In this diagram, for example '-600<'
) Pearl I indicates that the regulated pressure on the solution side is 600 mbar below atmospheric pressure. FIG. 14 graphically shows the results obtained using the apparatus of the invention shown in FIG. The lower curve represents the amount of condensate obtained at atmospheric pressure and various solution temperatures. In this case, the process according to the invention uses temperatures above 90° C., which is due to the ultra-proportional increase in condensate capacity obtained according to the invention at least on the solution side by achieving at least the amoboiling range defined above. it is obvious. The upper curve corresponds to the pressure in the pores of the porous separating wall to the respective temperature, so that according to the invention at least an approximate range of boiling points is achieved at least in the immediate area of the porous separating wall. vapor pressure. That is, the % condensate obtained for various solution temperatures when adjusted to reduced pressure compared to atmospheric pressure is shown. In this case, it is clear from a comparison of the two curves that the process according to the invention (upper curve) results in a greater increase in the condensate yield at lower temperatures than at lower temperatures. For example, at 50°C, 4 times as much condensate as in the method not according to the present invention, 161.70°C.
At t7. The absolute increase in the amount of condensate in Ih was also significantly greater at lower temperatures. Therefore, the increase achieved by the method of the invention (upper curve) compared to the non-inventive procedure is 30 t/L at 90°C.
rr? h, but at 50°C it is only about 9 t/y/h. Therefore, if lower solution temperatures are desired. The method of the invention therefore offers very significant technical and economic advantages. It should be noted that the double condensate cap achieved at high temperatures in the method of operation of the present invention is also a significant effect. The results are shown graphically in Figures 12-14. This was obtained with a 0.1% Na01 aqueous solution. In this case, the porous separating wall consisted of a tube of length 420 Ia with an outer diameter of 6.2 tm and an inner diameter of 4.1 m, thus having a wall thickness of 1.05 mm. 9. The tube wall consists of porous polypropylene structured in a network as described in detail above. In this case, the porosity is 80% and the maximum pore diameter is 0.
．． It was 85 μm. One unit was constructed from a total of 18 pipes connected in parallel as described above (configuration, see Figure 5). In this case, the solution flowed through the tube, and the condensate flowed through it, surrounding the outer circumference of the tube. The amount of solution and condensate supplied to this distillation unit was 250 t7h, and in this case, the amount of solution flowing out from the distillation unit was the distillate that passed through the porous separation wall and migrated into the condensate due to permeable diaphragm distillation. and the amount of condensate flowing out increased by this amount. The results shown graphically in FIG. 15 were obtained under the same conditions as shown in FIG. 14, except that a different porous separator e was used. That is, the tube used in this case has an outer diameter of 8.6 wm and an inner diameter of 5.5 wm *Therefore, the wall thickness is 1
-55m+, porosity 75% and maximum pore diameter (1,55μm
f. All other nosolameters remained unchanged. Significantly less condensate was obtained under these conditions. This is due to the large wall thickness of the tube, the small porosity, and the small pores (pore diameter). The consequences of stiffness are self-evident. FIG. 16 shows a comparison of the condensate amounts obtained under different operating conditions, in which an average value was calculated from the corresponding values obtained from a number of measurement series when preparing the graph. The solution inlet temperature was 50°C, and the condensate inlet temperature was 16°C. The other Nose 2 meters were the same as when calculating the results shown in graphs in FIGS. 12 to 14. Under the above conditions, by adjusting the total atmospheric pressure on the solution side, on the condensate side, and in the pores of the porous separating wall, a condensate t'1'' was obtained in an operating method not according to the present invention. Condensate - Dispersion "2" was obtained when a vacuum equal to the vapor pressure of the solution was generated on the solution side, i.e. when the boiling point was achieved on the solution side and the boiling point was maintained. This was obtained when only the pressure in the pores of the septum l1g1 buds was adjusted to a pressure (reduced pressure) equal to the vapor pressure of the solution at 50°C and to atmospheric pressure in the solution and condensate side tubes. The amount of condensate '4# is the pressure (reduced pressure) equal to the vapor pressure of the solution at the pressure t50°C on the solution side and in the pores of the porous separating wall.
This was obtained by adjusting. These results clearly show that a significant increase in condensate capacity is possible with the method of the invention. Moreover, simply by generating a pressure in the pores of the porous separating wall that corresponds to the temperature of the solution, a corresponding adjustment of the (de)pressure on the solution side can lead to a noticeable, even small, increase in the condensate capacity. An increase in the yield of condensate can be achieved to the extent that it may even be discarded. This means that, if the respective boiling point of the solution, at least in the range thereof, is achieved in accordance with the invention at least on the solution side and in the immediate surroundings of the porous isolation, the maximum possible condensate amount can be achieved in practice at least It means that it can be obtained approximately. FIG. 17 shows the connection to a device that generates reduced pressure. and shows the pressure gradient in the bore of a core tube made of the same material as the tube described with respect to FIGS. 12-14 and also having the same diameter, but of different lengths. One tube has a total length of 0.5m and the other has a total length of 2mff. Both pressure drop curves were measured at room temperature and in water using the nine measuring apparatus shown in FIG. 8 and described above, and consisted of nine values. In this case, the atmospheric pressure at one end of the tube is also 930 mm IJ/
The measurement position (position number 31) is
．． The vacuum produced in the holes at different distances l111 from the end of the tube was measured by the t-travel (see FIG. 8). This measurement shows that the length of the tube significantly affects the pressure drop within the bore of the tube. This is of course a flat plate. This also applies to rods or other shaped bodies having a correspondingly networked pore structure. This means that if the tube is short or the area of the plate is small, the reduced pressure that occurs at one location, for example at the end of the tube, can be applied at any distance r from that location.
As for c. This means that it also acts strongly on long pipes or large-area plates. Based on the respective temperature distribution occurring in the porous isolation and the resulting vapor pressure distribution when carrying out the process of the invention,
The pressure distribution, as represented by the lower curve, produces on the solvent side the respective boiling point of the solution, at least in the range contemplated by the present invention, around the entire polygon. On the other hand, the ri between the inlet and outlet sides on the solution side
If the A degree difference, and therefore the vapor pressure difference, is too small, the porous separator 1, e.g. It may also be advantageous to connect the sexual separator at short intervals with a device that generates a reduced pressure. The measured values shown in the graph of FIG.
112 solution and the lower curve is the value obtained with 33 Li0L solution. The measurement is performed at a pressure higher than atmospheric pressure, in particular, the upper curve (1065 for 0a (1t2 solution)
Runs were carried out in millinol and for the lower curve (Li0t solution) at 1040 millinol. In this case the boiling point temperature was higher than 120°C. The measurement results also show that sufficiently high condensate amounts can be achieved only with one operating method according to the invention, ie in the direct range of the boiling points defined above. Therefore, for the first time in the process of the present invention, the permeable diaphragm distillation method can be applied economically. The porous separating wall used in both measurements was
It was the same as that used in detecting the measurements shown graphically in the figure and detailed above. Another Example A series of measurements were carried out for various flow rates on the solution side and on the condensate side using an apparatus according to the invention whose main components were identical to the apparatus shown in FIG. The nine temperatures t, flow rate Q1 and pressure Pf used or obtained in each case were measured at the positions A-D circled in FIG. 4. The results are summarized in Table 1. In this case, the porous separating wall consisted of six tubes with a length of 9.2 m made of porous polypropylene with a porous structure arranged in the form of a network. The outer diameter of the tube was 9 m and the inner diameter was 611aI. Measurement position B is on the inlet side of the solution to the distillation apparatus, measurement position B is on the outlet side of the solution from the distillation apparatus, measurement position 0 is on the inlet side of the condensate to the distillation apparatus, and measurement position is on the inlet side of the condensate from the distillation apparatus. It was on the exit side of the product. At the ninth measurement of the flow rate Q, only the solution flowing into the distillation apparatus and the condensate were measured each time. Overflow pipe (4th
The nine condensates flowing out from position number 5b) in the figure were collected and weighed. From the values thus obtained, 1 hour and porous separator 1 n? The amount of distillate Dt obtained in this process was calculated and summarized in the last column of the 19th lie. In this case, the S solution flowed through the interior (cavity) 1 of the tube, while the condensate flowed through the outside of the tube. The condensate side was connected via an overflow conduit 5b to the surroundings, ie to the ambient pressure, while the solution side was connected to a pressure reduction device. The measurement value code in Table 1 indicates at which measurement position the value was measured.1For example, tB indicates the temperature measured at measurement position B, that is, the temperature of the solution flowing out from the distillation apparatus2. The series of measurements summarized in the table clearly show that the flow rates on the solution and condensate sides influence the amount of distillate obtained. Furthermore, these series of measurements show that the method of the invention also gives good results when the pressure on the solution side is adjusted to a pressure partially higher than atmospheric pressure, provided that at least the boiling point range of the solution is achieved in each region. Showing money. Table 2 shows, for comparison, tap water and the distillate obtained from tap water by the permeable diaphragm distillation method of the present invention, as well as the distillate obtained from the Na06 solution at o, 1ts. distillate and fully demineralized water (vE
) In order to be able to summarize the analysis results of the present invention, it is here mentioned that the comparison between the non-inventive operating method and the inventive operating method is always based on the distillate olII (condensate side). Equivalent temperature characteristics dominate. In particular, it should be noted that the detailed description has been made under the assumption that the inlet and outlet temperatures of the distillate or condensate are at least substantially the same as in the procedure described for comparison. 1llt- increase,
Due to the large average temperature difference between the solution side and the distillate side that can thereby be achieved on this side, the distillate flow rate passing through the porous separating wall is increased even in the non-inventive operating method. is generally known, extensive and self-evident. Therefore, unless one takes this fact into account, it is impossible to objectively compare the method of the present invention with the operating method other than the present invention. If the boiling point is achieved according to the invention, e.g. by creating a vacuum equal to the vapor pressure on the solution side or by increasing the temperature on the solution side, and thus a high permeability diaphragm distillate flow rate is achieved, If the flow rate is not changed on the distillate side (condensate), the condensate outlet temperature will increase, since now the increased distillate volume will be absorbed and condensed by the same condensate volume and will be correspondingly higher. This is because the heat energy of condensation is transferred to the condensate. This method of operation therefore reduces the average temperature difference between the solution side and the condensate side. As a result, a comparison of the two methods of writing will lead to nine incorrect conclusions. In contrast, in the method of operation of the invention described above, the flow rate on the condensate side is kept unchanged, the temperature at the condensate mouth remains unchanged, and thus the average temperature difference between the solution side and the condensate side also changes. To a height that won't happen! Once the illumination is set up, comparisons can be made.

[Brief explanation of drawings]

1 to 1θ show partially sectional schematic diagrams or sectional views of various embodiments of the device of the invention and various measuring devices, and FIGS. 11 to 18 show measurement results in graphs. FIG. 1 shows an embodiment suitable for continuous operation of the apparatus of the invention, FIG. 2 shows a series connection of four distillation apparatuses of the invention, and FIG. FIG. 4 shows an embodiment of the device according to the invention configured to operate at a difference in height; FIG. 4 shows an embodiment suitable for continuous operation of the device with a thermal energy recovery device; Figure 5 shows porous septa! FIG. 5 shows a particularly advantageous embodiment of the distillation apparatus according to the invention, in which different pressures can be set in the wall boreholes on the solvent side and/or on the condensate; FIG.
Figure a shows one embodiment of the distillation apparatus in Figure 5, Figure 5b is a cross-sectional view of an apparatus for measuring the pressure inside the pores of a porous separating wall using a pressure measuring sonde, and Figure 6 is a diagram showing an embodiment of the distillation apparatus in Figure 5. Different pressures can be set for the whole solution side and/or the condensate side in the pores of the separating wall. 7a is a side view of an embodiment of the distillation apparatus of the invention suitable for continuous operation with non-tubular porous separating walls; FIG. 7 is a plan view of the apparatus shown in FIG. 6;
Figure and Figure 7b show the same porous gap S as the device shown in Figure 6.
A diagram showing an example of a measurement position for detecting pressure in a hole in a wall,
FIG. 8 shows a measuring device for detecting pressure and pressure distribution in the pores of a (tubular) porous separating wall. Figure 9 has a stirrer. Figure 1O shows a distillation apparatus according to the invention suitable for continuous and discontinuous operation methods
It has two stirrers. FIG. 11 shows a distillation apparatus according to the invention suitable for discontinuous operation; FIG. Figure 12 graphically shows the rate of increase in distillate flow rate of a permeable diaphragm that can be achieved under the same conditions, and Figure 12 shows, for comparison, at various temperatures and pressures and when the boiling point is not achieved on the solution side. Figure 13 shows the permeability diaphragm effluent flow 1tch graph obtained when the pressure on the solution side is lowered until the boiling point is achieved in the solution, but otherwise under the same conditions. For comparison, Figure 14 is a graph showing the increase in the amount of outgoing materials.For comparison, the solution side is under atmospheric pressure and the pressure inside the pores of the porous isolation tube is the same as that on the solution side, and the pressure inside the pores. Figure 15 shows the distillate flow timigraph of a permeable diaphragm obtained when increasing the temperature on the solution side when corresponds to the respective vapor pressure of the solution. FIG.
The figure shows, for comparison, permeable diaphragm distillate firi obtained with a non-inventive procedure and various inventive procedures.
Fig. 17 is a graph showing the pressure distribution inside the pores of (tubular) porous separating walls configured with various sizes and lengths, and Fig. 18 is a graph showing the pressure distribution in the pores of the (tubular) porous separation walls of various sizes and lengths. FIG. 2 is a graphical representation of the distillate streams t obtained in two different solutions using a non-inventive procedure and an inventive procedure. l... Container (a... solution side, b... distillate side),
2... Porous separation wall, 3... Annular conduit, 4... Supply conduit, 5... Discharge conduit, 6... Heat exchanger, 7...
・Pump, 8...Valve, 9...Connection port" (conduit), l
O... Rising pipe, 11... Downpipe, 12.14...
Immersion container, 13... throttle mechanism (valve), 17... filter, 18... heat exchanger. 19... pressure chamber, 20... pressure needle, 21...
tube bottom. 23...Exit, 24...Inlet, 25...Exit, 2
6...Pressure connection position, 27...Ring, 2i...
circular passage. 29... Seal ring, 30... Conduit, 31...
Measurement position, 32... Container, 33... Intermediate chamber, 34.
... Stirrer, 36... Packing body 32 1 Fig. 9

Claims (1)

[Claims] 1. The solution and distillate are completely separated from each other by a porous separating wall that is permeable only to the vaporous distillate and maintains the solution and distillate in stirring contact. 1- held in a state of
At least one portion of the solution is converted into a vapor phase by converting the solution to the vapor phase in such a way that the conversion to the vapor phase takes place on the solution side of the pores of the porous separator and the vaporous distillate diffuses through the pores to the distillate side. In a method for the at least partial separation of the liquid component gold of the liquid component, during the continuation of the separation process, pressure and/or temperature control is constantly applied to the immediate surroundings of the porous separating wall on the solution side, at least in a partial region of the solution in each case. A method for at least partially separating at least one liquid component of a solution, characterized in that the method operates in such a way that a boiling point range of . 2. The method as claimed in claim 1, wherein the method is operated in such a way that at least the respective boiling point range of the solution is achieved at least in the immediate surroundings of the solution side of the porous separating wall. 3. Adjusting the distillate side of the porous separator to a hydrostatic pressure higher than the vapor pressure on the distillate side and bringing the distillate to a temperature below its boiling temperature at that pressure, whereby the porous separator The vaporous distillate is condensed on the distillate side of the hole. A method according to claim 1 or 2. 4. The method according to any one of claims 1 to 3, wherein at least the solution side of the porous separating wall is adjusted to a hydrostatic pressure lower than atmospheric pressure. 5. The method according to any one of claims 1 to 4, wherein the distillate side of the porous separating wall is also adjusted to a hydrostatic pressure lower than atmospheric pressure. 6. The method according to claim 1, wherein the pressure at least in the pores of the porous separating wall is adjusted to correspond at most to the respective vapor pressure of the solution. L. The method according to any one of claims 1 to 6, wherein the distillate side of the porous separator is adjusted to a higher hydrostatic pressure than the solution side of the porous separator. 8. The method according to any one of claims 1 to 7, wherein the solution and/or distillate is made to flow along a porous separating wall. 9. The porous separating wall is a sweet acid diaphragm. A method according to any one of claims 1 to 8. 10. Process according to any one of claims 1 to 9, characterized in that thermal energy is applied to the solution before and/or simultaneously with converting at least one liquid component of the solution into the vapor phase. 11. Thermal energy is extracted from the distillate or condensate after and/or simultaneously with the conversion of at least one liquid component of the solution into the vapor phase, claims 1-g.
10. The method according to any one of paragraphs 10 to 10. 12. Part of the thermal energy supplied to the solution is extracted from the distillate or condensate, claims 1 to 11
The method described in any one of paragraphs. 13. The through holes opening on the solution side and on the distillate side are crossed and connected to each other by gas or vapor permeable openings, holes, etc. 13. A method according to any one of claims 1 to 12, characterized in that a porous separating wall constructed in the form of a rod is used. 14. keeping the solution and distillate separated from each other by a porous separating wall that is permeable only to the vaporous distillate and maintains the solution and distillate in agitated contact; At least one portion of the solution is converted into a vapor phase by converting the solution to the vapor phase in such a way that the conversion to the vapor phase takes place on the solution side of the pores of the porous separator and the vaporous distillate diffuses through the pores to the distillate side.
Apparatus for at least partially separating the liquid components of seeds, comprising at least one vessel, the vessel being divided by at least one porous partition into at least two chambers, of which - In those types in which one chamber is configured to receive the solution and the other chamber to receive the distillate, the chamber (1 m) for receiving the container and/or the chamber (1 m) for receiving the distillate ( lb) and/or the porous separating wall (2) is connected to the component (1a-1b #2
) can be connected to a device for generating reduced pressure or overpressure (9a, 9b, 9c). Apparatus for at least partially separating at least one liquid component of a solution. 15. Only a suitable porous separating wall (2) can be connected to a device generating a reduced or overpressure in order to adjust the pressure in the pores to substantially correspond to the respective vapor pressure of the solution, % F
F. The device according to item 14 of the scope of KR requirements. 16. The chamber (1a) receiving the solution can be connected to a device for generating reduced or overpressure. An apparatus according to claim 14 or 15. 17.Both chambers (1a, 1b) and porous separating wall (2)
17. A device according to any one of claims 14 to 16, wherein the containers (1) having: are arranged and connected in a height-actuated manner. 18. Device for transmitting thermal energy to the solution on the solution side (6
a) is located. Claims 14 to 1
7. The device according to any one of clauses 7. 19. Distillate or #-i on the distillate side or condensate side
A device is arranged for extracting thermal energy t'' from the condensate. The device according to any one of claims 14 to 18. 20. Behind the chamber (1b) receiving the output or condensate, there is a heat transfer device (18) capable of transferring thermal energy from the condensate to the solution in order to cool the condensate and heat or preheat the solution. Claims 14-
Apparatus according to any one of clause 19. 21. It has a porous separating wall configured in a net shape, in which the through holes opening to the solution side and the distillate side are interconnected and connected to each other by five gas- or vapor-permeable openings, holes, etc. , any one of claims 14 to 20
Equipment described in Section.