JPS60106501A - Method and apparatus for separating thermally sensible substance mixture in vacuum - 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 relates to the separation in vacuum of thermally sensitive multi-substance mixtures, in particular from thermally sensitive fatty acids of plant and animal origin, to pre-distillate, main distillate, etc. The present invention relates to a method and apparatus for separating output and residue.

Furthermore, the method of the present invention can be utilized in cases where the pre-distillate and residue separations have to be subjected to rectification, for example in the distillation of essential oils, synthetic fatty acids, tallow, fatty alcohols, etc. be.

Raw fatty acids obtained by separating vegetable oils and animal fats contain dissolved air in addition to water, and during subsequent thermal processing, they have a low boiling point that cannot be condensed under thermal pressure. Contains organic compounds. During storage, other separated products may be formed by autooxidation and by hydrolysis of fats and oils, which are markedly odorless, colorless, heat resistant and chemically resistant to the separated fatty acids. Affect properties.

Thermal processing of degassed and dewatered raw fatty acids is carried out under conditions such that thermal or autooxidative damage is avoided as much as possible under the new formation of lighter and heavier separation products. The distillation must be carried out in such a way that the High yields for fatty acids of the best distillable quality, which are generally required today, are among other things (
In addition to the processing of low-value raw materials, additional equipment and process-technical outlays are required due to the high-boiling color carriers and other organic contaminants containing the residues.

Large-scale technical distillation processing of isolated fatty acids is carried out in the processing steps of degassing and dehydration, separation of pre-distillate and separation of main distillate. For degassing and dehydration as well as separation of pre-distillates, 1. It is customary to use a flow-through thin film evaporator with a length of 0.5 m and a solid distillation column with a length of j m or a rock garden distillation column with 10 exhaust bell beds as the amplification head. At the head of the distillation column.

There is a separation unit in which water is separated from the fatty acids and the majority of the light fatty acid phase is fed as after-distillate onto the distillation column. The distillation pressure is / J 300 Pa, and the temperature inside the expulsion part is / t 00~20
It is 0°C. The proportion of post-distillate is adjusted in the range from 10 to 200 (German Published Patent Application No. 23!2139)
issue).

The main separation and the post-separation are carried out in serial stages which can be carried out continuously. In the main separation stage.

Up to 977 wt% of the distillable amount is evaporated, yielding about goWt of distillate in the final stage.

to move - to be swept away, undesirable.

In order to avoid components such as monochromatic carriers and saponifiable components, these distillation columns are equipped with separation-like devices and the effective evaporation rate is maintained within the range from J to 6 to 8. Ru. In addition, the product coming out of the degassing/dehydration stage has a slight evaporation rate/! Directed into a relaxation chamber in which a comparable air velocity of less than n/s is maintained.

The unevaporated portion is subjected to further evaporation in the main thin film evaporator located in the lower left part of the relaxation chamber, and the unevaporated portion is placed in the right part of the relaxation chamber. The remaining amount is normally fed to a falling film evaporator for evaporation. Besides maintaining a smaller evaporation rate to avoid mechanical entrainment of unevaporated fluid particle fragments or higher acidity flow of the residue via fatty acid vapors flowing upward from the retention chamber to the condensation zone. One drop separator "Euroform separator" (11turoformabsc
(German Patent Publication No. J9.?4JJ) Q Furthermore, East German Patent No. 9
A method with a device according to No. 1ZA00 is also known and is described here.

Degassing/dewatering is carried out by means of a single-stage or multi-stage falling film countercurrent device, and the main separation product and the post-separation product are discharged into a downstream device. In this equipment, 6! n
For evaporation rates up to /e, natural fatty acids are distilled with higher yields, in which case a color-stable distillate is maintained without additional separator equipment.

To the extent necessary, the propellant distillate is subsequently freed from undesired fore-distillates and low-boiling fatty acids in the main distillate by rectification.

In the known processes for the separation of the main distillate and after-distillate, an energy demand of toO% is required for one evaporation; is increased by 20 to 30 inches for one evaporation, depending on the characteristics of the raw mixture and the separation method used.

Separation of migrating color carriers and other evaporation contaminants and low evaporation rates in the evaporation column space are necessary in the equipment and structures used in G) for all these processes.

The desired high yields, especially in the case of raw material products of poor quality, are only achieved by a reduction in the quality of the final product.

The object of the present invention is to separate thermally sensitive multi-substance mixtures into pre-distillates, main distillates and residues with low energy and equipment costs.

The present invention develops a method and apparatus for the separation of a dehydrated and degassed thermally sensitive multi-substance mixture into a pre-distillate, a main distillate and a residue, whereby the residue and pre-distillate are separated into pre-distillate, main distillate and residue. It is based on the problem that by complete separation of the distillate it is possible to ensure a high yield of a one-color, benign and good-quality main distillate.

According to the invention, this task was degassed and dehydrated.

The feed mixture in which the condensate from the first condensation phase is added as a circulating distillate amount exceeds the phase balance in the first partial evaporation above the total pre-distillate as well as in the second partial evaporation at lower pressure. The first main distillate is evaporated in the third partial evaporation, the after-distillate is evaporated and the residue is separated, and then the vapors of the first and third partial evaporation are combined. This vapor also causes rectified evaporation of the pre-distillate fraction at the outer surface in the condensation phase of the
At the inner surface, by the λth partial reevaporation, this vapor causes the separation of the second main distillate from the condensate from the second condensation phase, which also takes place at the outer surface. The second condensation phase is therefore the evaporation of the first main distillate from the feed mixture.

A second partial evaporation takes place at the internal surface, in which case a partial amount of the pre-distillate flows out. The solution is to allow the light product from the second reevaporation to be added as a recycled amount to the condensate of the second condensation phase.

According to the invention, the raw material mixture, free of pre-distillate, is mixed as a circulating amount from the effluent originating from the first condensation phase described below, in one or more falling film evaporators or thin film evaporators. In the evaporator, 1% is evaporated from all the pre-distillate under low pressure from 3 tO to ≠ 20 Pa, overcoming the phase balance by the addition of further heat during the first partial evaporation into a separate distillation column. is added below. The unevaporated raw material mixture is fed to the internal surface of a subsequent heat exchanger, in which a second partial evaporation takes place in a second condensation phase, which will be further explained below. , the evaporation of the first main distillate is from 100 to 200P
Under pressure up to eL, also -0 to g.

It is carried out under an evaporation rate of up to m/8, which is condensed and removed. The remaining raw material mixture is now evaporated from the ago in a falling film or thin film evaporator heated by other or multiple other energies.
At pressures up to Pa 2, a third partial evaporation or post-distillate evaporation is reached and evaporated to a residue. The vapor of the third partial evaporation is likewise fed to the bottom of a special distillation column and the residue is discharged.

The vapors of the first and third partial evaporations enter a special distillation column and in the first condensation phase G) 30 to 10 s.

At higher flow rates in the range of .

The external heat exchanger surface is fed upwards from a special distillation column and likewise upwards to the external heat exchanger surface. The first condensation phase provides energy for the single rectification described below. The pre-distillate-free condensate which exits is added as a recycle quantity for the first partial evaporation.

In external heat exchangers, the already described second condensation phase of the vapor takes place on the outer surface, which causes a second partial evaporation to occur on the inner surface of the heat exchanger. The mixture of steam and condensate is removed below the heat exchanger and completely condensed. This condensate is now passed over the inner surface of the first partial re-evaporator at the head of a special distillation column, in which the pre-distillate is concentrated between 3θ and 50 In/θ. The unevaporated condensate, which is rectified at the evaporation rate and evaporated above the phase balance, exits at the bottom of the first reevaporator as a second main distillate without pre-distillate. The vapor from the first reevaporator is condensed and passed onto the internal surface at the top of the second partial reevaporator. In the second re-evaporator, the pre-distillate is rectified, enriched and evaporated, condensed and the light fraction in the feed mixture or freshly formed from the third partial evaporator is concentrated. A portion corresponding to the lighter portion flows out, and the other portion is fed as a recycled quantity to the condensate from the second condensation phase. The condensate falling downwards from the second re-evaporator is likewise mixed as a circulating quantity with the condensate of the second condensation phase. Rectification at the internal surface is carried out in countercurrent phase contact, in which case the pre-distillate from the first internal surface exceeds one phase balance at an effective evaporation rate from 3θ to IO”/a. The second internal surface serves for circulation guidance as the actual rectification stage. The pressure state and velocity state are “Dat =PDa4 =PDall
−400P& and vDas ”” DILs = vDas~arm/θ.

The pressure and velocity conditions in the second partial evaporator of the feed mixture are preferably "Da2-//3Pa and
na2-30 In/a.

From the residue separation from the second falling-film or thin-film evaporator, the lower-boiling fraction produced, optionally by thermal transfer, is transferred to a condensate circulation guide from an external surface located outside the distillation column. By this, the first internal surface in the distillation column is reached for separation of the pre-distillate and therefore there is no deterioration in the quality of the main condensate. The high-boiling color carriers and M-organic contaminants, such as non-saponifiable constituents, transferred by the steam from the remaining evaporator are only retained at the outer surface under slight rectifying action. .

When no pre-distillate fraction is present or should be removed, then the condensate from the first partial evaporator and the remaining evaporators is transferred to a heat exchanger outside the distillation column. It is of the essence of the invention that it is subsequently carried away as a final product and is condensed and removed from the internal surface of the heat exchanger outside the distillation column.

The saponifiable process mode also includes the raw product being preheated in an open surface heater to the boiling point by an effluent heating medium from a falling film or thin film evaporator to a boiling point of 3.99-0.
From/to R300'E'a, preferably 43 OP
It is to be degassed and dehydrated at a pressure of a.

The solution according to the invention is 20 to 30
% of energy is saved, equipment costs are reduced by 30%, and high yields are achieved, also with very good quality, even at low value charge products.

According to the invention, the task is to provide external and internal heat exchanger surfaces, preferably in a distillation column known per se,
G) with a bundle of tubes, whose internal surface is divided into two so-called reevaporators, separated from each other by a partition at the top and bottom, and whose external surface is by the surface of the distillation column G)
The external heat exchanger surface, preferably the bundle of tubes, forms a so-called first condensing phase, together with the external surface.

It has a condensation space of the so-called second condensation phase and is also connected via the product vapor conduit to the so-called first and so-called third, each consisting of one or more falling film or thin layer evaporators. In this case, the condensation space of the distillation column is solved by still having a condensate return conduit to the first partial evaporator. The evaporator of the first partial evaporator is connected on the fluid product side via a fluid product conduit.

and the inner surface of the heat exchanger, which is the second partial evaporator.

It is also connected to some degree in series with the evaporator of the third partial evaporator. After the first evaporator, the fluid product conduit is interposed with a float receiver, a supply device and a control device.

Behind the JII' control device there is a switchable short-circuit line which leads to the evaporator of the third partial evaporator. For the evaporation device of the third partial evaporator, the flow of the raw product is advantageously connected to the preheater.
It has an outflow conduit for the residue.

A line is connected to the head of the heat exchanger and thus of the second partial evaporator, which leads to the total condenser, on the fluid side of this condenser.

A discharge conduit for the first main distillate is connected. A total condenser is likewise connected below the heat exchanger chamber, but this condenser is connected on the condensate side to the chamber above the first partial reevaporator. This adjustable condensate conduit.

It is connected to the condensate outlet of the second reevaporator and to the take-off conduit for the second-mentioned pre-distillate, thus acting as a circulation conduit for the light fraction. An interposed transport device and a float receiver create a flow of media. For cases where no pre-distillate is present or no pre-distillate is to be removed, a discharge conduit with a shutoff device and a shutoff element before the transport device. is placed. The upper chamber of the first reevaporator is connected to the upper chamber of the second reevaporator, which is also followed by a total condenser. , to the condensate side of this condenser is connected the previously described adjustable discharge conduit for the pre-distillate. A discharge conduit for the second main distillate is connected to the lower chamber of the first reevaporator.

A vacuum line is connected to the float receiver, which is inserted after the first partial evaporator and lies between the distillation column and the heat exchanger. It is suitable for this purpose to be led into a steam conduit. This vacuum conduit can also be connected to the vacuum conduit of an open surface heater.

The condensate side of all condensers is connected to a vacuum conduit, which includes a float in the condensate conduit lying between the heat exchanger and the first re-evaporator. A receiver is also connected.

A heating medium circulation conduit may lie between the evaporator arrangement, the first partial evaporator and the open-surface heater.

The solution according to the invention is better than the conventional method.
7% energy savings.

It has the advantage that the equipment costs in sO% are reduced and that high yields are achieved with very good quality even in the case of low-value charges. In the case of known methods,
The required tm height exchange surface is reduced to 3 m.

The method and apparatus of the present invention will be explained below with reference to the accompanying drawings.

Example 1 (See Figure 3) Pre-distillate content of % cowt% and ygw from dehydrated and degassed fatty acids having a free fatty acid content of 94 wt%.
It is assumed that t% of the main distillate is to be separated.

The raw material mixture Fz+(WtS) is fed to an open surface heater l heated by the exhaust heat transfer medium from the thin film evaporator and further reaches the thin film evaporator, where it
Approximately g Q wt % of the feed product is evaporated at a pressure of approximately 1100P, and the resulting vapor Da1 ("t%) is deposited on an external surface 3 having a height of approximately 3 m in the distillation column structure. , with an effective evaporation rate of 4Ism/B, θθpa
Flows upward under pressure.

It is fed to a heat exchanger located above the outer surface 3 of the distillation column structure. The amount (xttwt%) not evaporated in the thin film evaporator is fed to the inner surface of the heat exchanger under a pressure of /33 Pa. By heat exchange within this device l.

At an effective evaporation rate of 36 m/, about 3 s% of the feed mixture is evaporated with respect to the inflow. This evaporation Daz
(%) is condensed in a condenser S and taken off as finished product FJ* (first main distillate).

Amount not evaporated from the inner surface of heat exchanger l”*(”%
) is fed to a second falling film evaporator group located in the lower part of the distillation column structure. The amount, which is not evaporated here and is approximately gwt% with respect to the amount of raw material mixture flowing in, is separated as residue F23 (wt%). A post-distillate having an amount of about
%) flows together with the vapor Da, (wt%) on the outer surface 3 in the distillation column structure and is fed to the outer surface in the heat exchanger hole above the distillation column structure. On the outer surface of the heat exchanger,
Vapor not yet condensed Dal (wt%) p Da
s (wt%) is aH4a? (7) Medium R: Oil
Condensed, all these condensates are passed onto the inner surface g of a first re-evaporator in which a pressure of 1 g00 Pa is maintained, which acts as a pure propulsion head. . Due to the temperature difference between the outer surface 3 and the inner surface t, approximately
Partial steam (Dajwt%) of wt% is produced. This steam D
A4 is condensed in the condenser 9 and passed to the inner surface 10 of the second reevaporator, which primarily acts as an amplification head. Here about /Q i
t % evaporates. This JRDas (wt%) is condensed in a condenser//, and 7J, (wt%) of the condensate is removed as a pre-distillate enriched at about λwt% with respect to the inflow of the feed mixture. is partially mixed into the condensate Fl, (it) as a light circulating quantity P'17 (it).

An amount of about 7 (7 wt%) not evaporated from the second inner surface 10 and partially reduced in the pre-distillate
h) is similarly condensate FJ, (it h) and 1'JT
("J) and is now passed over the first inner surface 3 of the distillation column.

The amount 'J*(Wt'l') of approximately 3 q wt % not evaporated from the first inner surface t and free of pre-distillate components.
*Falls out as a finished product (second main distillate).

By the amount of fluid passed over the internal surface area and IO,
At the outer surface, the amount of raw material mixture flowing in is approximately 3
t) Partial condensation of wt % of steam Dal (wt %) takes place. This condensate FJto (wt%) is mixed into the feed mixture as a circulating quantity and passed to the thin film evaporator for re-evaporation. In this case, the energy consumption is approximately qs% for one evaporation. low value about y
When processing a raw product with a free fatty acid content of 9 wt%, approximately F2. =
JJwt%.

Fl, = kowt%p 'As = ” ' itchi, I
J, = 3 Da wt steamed rice is obtained. The energy consumption for a single evaporation is in this case approximately to9%.

Example (see Figure 1)? It is assumed that 94 wt% main distillate is to be separated from the dehydrated and degassed fatty acids having a free fatty acid content of fwt%.

After heating the raw mixture Fit(W”%) to the boiling point in the open surface heater I, about 6 wt% of the inflow product is evaporated in the thin film evaporator at a pressure of uoop6. .This steam Daz (%) is
It flows into the distillation column space with an effective evaporation rate of 30 m/8 and, above the distillation column structure, is fed at the external surface to an externally arranged heat exchanger. The unevaporated amount XJ (wt%) from the falling film type or thin film type evaporator is:
It is supplied to the inner surface of the heat exchanger l under a pressure of approximately /33 Pa.

Due to the temperature drop at the inner and outer surfaces in the heat exchanger q, the partial steam Da, (w
t%) is generated. This vapor condenses in the condenser 5 and flows down as finished product FJ2 (wt%)1. The amount X, (w
t%) is fed to a second falling film or thin film evaporation well located below the distillation column structure. In this, about //wt% is evaporated with respect to the amount of raw material mixture flowing in.

The vapor Das (wt%) reaches the outer surface of the heat exchanger q, and the remainder is condensed in the condenser, producing the finished product F2. (wt%).

The amount of goo FL, (wt%) (residue) that is not evaporated in the thin-film evaporator likewise flows down as the final product.

The energy demand for one evaporation is approximately 73 inches.

If a product is processed that has a free amount of fatty acids of about s 9 wt %, the amount is Dal = J t wt
%.

Da, = f2. = / t wt% + Das
='Wt'I' t Df's +Das == '
J.

= 4 (Hiro wt% and Fis (residue) = << wt%) Energy demand for 01 evaporations is about ts%
It is.

Example 3 (See Figure 1) In the distillation column structure shown in Figure 1, 3 m long tubes are provided with upper and lower tube spacing, preferably with an external tube spacing of 0 cIrL. in each case welded to the bottom 1.2° 13 sealed to the surface of one distillation column, the outer surface 3 for the first condensation phase and the inner surface for the second and second reevaporation. t, forming 10. At the top of the distillation column there is provided a tube with a conventional fluid distributor, and a tube g which acts as a propulsion head.
It is separated by a septum/g from the tube lO, which acts as an amplification head. In the T-side part of the distillation column,
Similarly, division is performed by a partition wall /j.

an open surface heater l heated via conduit 16 by the discharge heating medium from the falling film/thin film evaporator;
The feed of the raw product takes place via conduit /'7 and is then fed via conduit /E to the falling film/thin film evaporator λ, where a first partial evaporation takes place. The condensate from the outer surface 3 also flows into the evaporator - as a circulating quantity via the after-distillate line 59.

The product that is not evaporated in the falling film type/thin film type evaporator reaches the float receiver O through the conduit 2S, and this receiver O is transferred to the falling type heater through the vacuum conduit 2. As well as through the vacuum conduit t of l, the steam conduit 2
Vacuum is applied from 0.

A pump 30 via conduit 25 sucks raw product from a float receiver 31 and forces it, controlled by control valve 31, to the inner surface of the heat exchanger for a second partial evaporation. A conduit 32 is provided in such a way that the supply of fluid to the inner surface 33 of the heat exchanger plate and to the falling film/film evaporator well is ensured. Below the heat exchanger q, a conduit 39 leads to a falling film or thin film evaporation well.

Via this conduit 398, the remaining raw product reaches the third partial evaporator. The residue exits via the removal conduit 10.

At the top, a steam line 36 to a condenser S is connected to the heat exchanger q, in which the first main distillate is condensed. The finished product is removed via the removal line 3g, to which the vacuum line 37 is also connected. The evaporated fraction from the third partial evaporator, via vapor conduit IIl, is combined with the vapor of the first partial evaporator from conduit /9 into a first condensation phase at the outer surface 3 of the distillation column. After that, the steam conduit θ reaches the outer surface of the heat exchanger bower for the second phase of condensation, and then passes through the conduit 7 to the condenser 7. reach. The condensate conduit 21I from the partial condenser 7 is followed by a float receiver, and a vacuum conduit 3 is also connected to this receiver. It has been led to 23. By Sharai pp, lIt, the product can be optionally removed when no pre-distillate is removed, or carried away to pump 4'& when the pre-distillate is carried away. It has become. The conduit widening provides for the supply of product onto the internal surface of the first reevaporator and thus of the propelling head. The rising product vapor is fed via conduits 4!9 to a condenser 9, which is also connected to a vacuum conduit sho. The condensate is passed via conduit 31 onto the inner surface, which acts as an amplification head, for a second reevaporator.

The amount not evaporated is transferred to conduit Sλ as the second main distillate.
is retrieved via.

The product vapor emerging from the amplification head on the inner surface 10 is an enriched pre-distillate and reaches the condenser/l by conduit 33, which also includes a vacuum conduit, tlI
and finished product conduit j& are also connected. Conduit j! There is a control valve inside r! There is a t, but above it,
A connecting line 37 for light circulation leads to product line j+. A product conduit 5g from the outlet of the amplification head lθ is also connected to this conduit 2da. Vacuuming the entire installation is provided by conduit 6o. The pressure differences required for the operation of the equipment are the conduits lIO, jJ, Q, for the high pressure area and for the low pressure area. The corresponding dimensioning of the conduit in the condenser chamber ensures that no additional adjustment devices are required. Thermal action of thin film/falling film evaporators is caused by the inflow conduit AI,! , 2 and an outflow conduit/6°A zone.

[Brief explanation of the drawing]

FIG. 1 is a schematic representation of a third embodiment of the apparatus for the separation of multi-substance mixtures according to the invention; FIG. Schematic diagram showing the flow of substances during the separation of the main distillate and residue in the second embodiment of the multi-substance mixture according to the invention, FIG. 1 is a schematic diagram showing the flow of substances during separation into distillate, distillate and residue; FIG. l...heater; c...evaporation device for first partial evaporation; 3...
External heat exchange surface of heat exchanger? , //... Total condenser; 6... Evaporator for third partial evaporation; t... Inner surface of first evaporator; lO... Inner surface of second re-evaporator; /, 2.
/, 7... Bottom for pipe distribution; /lI, it... Partition wall between the propulsion head and amplification head; lA... Heating medium inflow and outflow conduit;
/7゜1g...raw material mixture supply conduit; tq, lIt
・・Product vapor conduit of i- and third partial evaporator;
Product steam conduit; 21... Heat exchanger outer surface; 2J...
- product steam condensation conduit; c3. t, 21.: Vacuum conduit';
,yq,4t3. go, s; lI... Vacuum conduit; Koda... Condensate circulation conduit; Ko S2.7 Co... Raw material product conduit;
λ6, 4' Co... Float receiver; 29... Short-circuit conduit for raw material products; 3o, lIx... Transport pump; 3/, Dak,!
6.-Control valve; , ys, J4t, 4t4t, yr...
Shaarai; 3! f... Inner surface of heat exchanger: 36... Raw product conduit for the first main distillate; 3g... Conduit for the finished product; Dao... Residue conduit; 41g... Main distillate Export conduit; 4'? ...Product vapor conduit of the first re-evaporator; s/...Product conduit: 5 pieces...Finished product conduit for second main distillate; 5S...Finished product conduit for pre-distillate; S7
・・Connecting conduit for light circulation amount; 5g・・Connecting conduit for circulating amount; Tata・・Post-distillate conduit; tθ・・Central vacuum conduit; A/
, 42... Heating medium supply conduit; ≦3,6 Da... Heating medium outflow conduit.・Fig, 2゜

Claims (1)

Claims: 1) A process for separating thermally sensitive multi-substance mixtures in vacuo by distillation, evaporation and condensation after their degassing and dehydration, wherein the multi-substance mixture is
At a pressure of OOPa, it is separated into the main distillate containing the fore-distillate and the main distillate containing the residue, and the main distillate containing the residue is subsequently 〇 Pa
The final products are the first main distillate and the after-distillate, which are then completely evaporated to a separable residue, the resulting after-distillate being rectified at a pressure of The vapor is in countercurrent with the main distillate vapor containing the pre-distillate of the first evaporator at a velocity of 30 to 5θ and the condensate containing the pre-distillate. connected at a pressure of 300-sooPa, in which case in the simultaneous rectification the fore-distillates are evaporated out of phase balance, and the unevaporated and retained
The vapors obtained as the final product, the second main distillate, containing the pre-distillate vaporized above the phase balance, are condensed, circulated and re-evaporated at a pressure of lθθ~Co00Pa. and subsequently separated as a highly concentrated pre-distillate. In the case of minor distillate-free distillation of multisubstance mixtures, it is necessary to ensure that the vapor remaining after the production of the first main distillate and the residue is completely condensed as the second main distillate. The method according to claim 1. 3. The main distillate containing the residue is transferred to the first evaporator for 30 minutes.
The process according to claim 1 or claim 1, wherein the evaporator is immediately drawn into the residual evaporator at a pressure of 0-tooPa, in which the residual product is separated. In an apparatus in which a heat exchange device is installed in the distillation column space for the separation of a thermally sensitive multi-substance mixture containing a small amount of boiling point contaminants, the heat exchange device < t, /n is a tube = the spacing of the external tubes is ゛10 to -1 preferably 20 cm, and the tube (t, 10) has a post-distillate conduit < sq. forming a first condensation and relaxation space, which is bounded above and below by a conventional bottom (13) from the vapor space and the space for the fluid product; <t, to'') is separated by a partition (/l, #) into an evaporation space and a space for the fluid product;
This causes the first inner surface (t) to form the first re-evaporator or propulsion head, the re-evaporator having a finished product conduit (S) in the lower part and In the upper part there is a steam conduit (4I) followed by a condenser (9).
? ), and above the inner surface (to') forming the second reevaporator or amplification head, a product groove '1 (ff/) flows into the amplification head; (lΦ is the lower part where the condensation conduit (co → connecting conduit (ffJ) is connected to the condenser (li'
) is connected, and a finished product conduit (5υ) is connected to the condensing side of the condenser ('/ /), and this conduit (
The S column has a control valve (S6), and a connecting pipe (S7) to the condensing pipe (2II) is led in front of it. Evaporator', preferably thin film type or falling film type evaporator (co, &)
is arranged, the steam conduit (/?, l/) flows downward into the first condensation space (3), and above the first condensation space (3) the steam conduit (/?, l/) flows into the first condensation space (3). (20
) through an ordinary heat exchanger (
1) is similarly connected to the outer surface (21) of the heat exchanger @), which is followed by a conventional total condenser below via a conduit (21), and its The condensation conduit is led upwards onto the first re-evaporator under the interposition of a float receiver (gx), a % transport device (16) and a control device (tower), and also a heat exchanger. The inner surface of the vessel (da) (3υ
is fed to the evaporator (6) via the i-tube (S9), which is followed by a conduit (4I) for the residue. Furthermore, in its upper part, the heat exchanger (ri) is connected on the one hand via a steam line (3A) to a condenser (y);
A finished product conduit (3t) is connected to y), and on the other hand, a raw product conduit (32,
The lower part of the first partial evaporator is connected to the falling film type/thin film type evaporator (c) via the condenser (9, //, !, ri) of the first partial evaporator. A device characterized in that it has a vacuum conduit (10, Iu, 31.Co3). A short-circuit conduit (-
〇 is G which lies between the raw material product conduit (3φ) at the front of the heat exchanger (4I), which has a blocking member, and the raw material product conduit (J) at the rear of the heat exchanger (4'). ) The apparatus according to claim 1, wherein the raw material mixture is evaporated into a falling film or a thin film evaporator (
It is preheated to the boiling point in the open surface heater (1) heated by the outflow heating medium from the heater (1).
Is there a vacuum conduit (-g) for 1)? 21 or a plurality of falling film or thin film evaporators (J,
t> are mutually arranged below the distillation column. S or the device according to item 6. g゛ Steam conduit that maintains pressure (41q, ffJ,
74. Apparatus according to claim 1.ff, A or 3, in which a pipe and a condenser ('p''*3y') are provided. ,
Apparatus according to claim 1, wherein this main conduit (60) is connected to a steam cleaning device having a downstream vessel. lO finishing product conduit (3t, Jλ) and/or finishing conduit <at, Sλ) or finishing conduit (at, lit
,! r(2) is now led to the collecting conduit and 06
An apparatus according to any one of claims 9 to 9. 11. The device according to claim 10, wherein the open surface heater (1) is adapted to be connected to a separate container via a vacuum conduit (xr;).