DE102008020386B4 - Apparatus and method for producing a chlorinated alkane - Google Patents

Abstract

Device for producing a chlorinated alkane, the device comprising the following parts: a) a container (0) b) a vertically arranged separating device (9) by which at least part of the container is divided into at least two communicating rooms (12, 15), the at least two communicating spaces being in fluid communication with one another at least at two points, as a result of which the reaction medium travels naturally through the path formed by the at least two spaces (12, 15), and c) at least two addition devices (16, 17) in the first (12) of the at least two communicating rooms.

Description

The invention relates to an apparatus and a method for producing a chlorinated alkane, in particular 1,2-dichloroethane, according to the claims.

1,2-dichloroethane, hereinafter referred to as EDC, serves mainly as an intermediate for the preparation of monomeric vinyl chloride, hereinafter referred to as VCM. From VCM ultimately polyvinyl chloride, PVC, can be produced. The conversion of EDC to VCM produces hydrogen chloride HCl. EDC is therefore preferably prepared from ethene C ₂ H ₄ and chlorine Cl _{2 in} such a way that a balanced balance is achieved with respect to the hydrogen chloride HCl produced and consumed in the reactions in accordance with the following reaction equations: Cl ₂ + C ₂ H ₄ -> C ₂ H ₄ Cl ₂ (pure EDC) + 180 kJ / mol (1) C ₂ H ₄ Cl ₂ (cleavage EDC) -> C ₂ H ₃ Cl (VCM) + HCl - 71 kJ / mol (2) C ₂ H ₄ + 2 HCl + [1/2] O ₂ -> C ₂ H ₄ Cl ₂ (crude EDC) + H ₂ O + 238 kJ / mol (3)

The procedure for producing VCM with balanced HCl balance, hereinafter referred to as "balanced VCM method", has several steps:
In a direct chlorination, part of the required EDC is produced from ethene and chlorine in the presence of a homogeneous catalyst and released as so-called pure EDC.

In an oxychlorination, the other part of the EDC is produced from ethene, hydrogen chloride and oxygen and released as so-called crude EDC.

In a fractional EDC purification, the crude EDC, together with the recycle EDC recirculated from the VCM fractionation and optionally together with the pure EDC, are freed from the by-products formed in the oxychlorination and the by-products formed in the EDC pyrolysis to win suitable for use in the EDC pyrolysis, so-called feed EDC. Optionally, the pure EDC originating from the direct chlorination can also be co-distilled in the high boiler column of the EDC distillation.

In an EDC pyrolysis, the gap EDC is thermally cleaved. The cracked gas reactor exit mixture contains VCM, hydrogen chloride HCl and unreacted EDC, as well as by-products.

In a VCM fractionation, the desired product as pure VCM is separated from the cracking gas and the other essential fissile gas constituents hydrochloric acid HCl and unconverted EDC recovered as recyclables separately and recirculated as a recyclable use as back-HCl or back EDC in the balanced VCM process ,

The reaction medium used in direct chlorination is a circulating stream of the reaction product EDC in most industrial scale processes. The circulating stream can be generated in a loop reactor with external or internal circulation. Furthermore, the circulation flow can be generated by forced circulation or natural circulation. The catalyst used is primarily ferric chloride. In addition, sodium chloride can be used as an additive. Sodium chloride is able to reduce the formation of high boilers.

In the natural circulation evaporator, the liquid circulates exclusively due to differences in density between liquid and liquid-vapor mixture and / or liquid-gas mixture within the communicating process spaces (in physics, this is called the "effect of the communicating tubes"). The pressure p on the vessel wall as a whole depends only on the filling level h, the density ρ (Rho) of the medium and the gravitational acceleration g. At any altitude there is a different pressure and thus a different force on the vessel wall. Simply stated, the medium pressure results in density × height × gravitational acceleration (p = ρ × g × h). If different pressures occur due to the different densities in the respective process spaces, the resulting force causes the movement of the liquid, it is pushed upwards in the space of lower density. Behind this is a kinematic principle: A force is always the cause of a movement. If such a movement actually occurs, the force is from this moment = 0. (Cause -> Effect.)

The energy absorbed by the reaction heats the liquid, which in turn boils, creates a two-phase mixture and transports the liquid to the upper part of the process space - the thermosyphon principle. For the liquid circulation therefore no pump is required.

The direct chlorination in Siede reactors with natural circulation, without additional pump, is for example in DE 10 20040 630 90 A1 . DE 199 10 964 A1 and DE 10 2004 029 147 A1 described. Further prior art is in DE 196 41 562 A1 described. The described direct chlorination booster reactors with natural circulation require a high design Material use and space requirements and have high production costs.

The object of the invention is therefore, in particular, to provide an economical process for the direct chlorination of an alkene with chlorine (in particular for the production of EDC). In particular, the object is to provide a device for producing a reaction product, with which this method can be realized and which overcomes in particular the disadvantages mentioned above.

• a) einen Behälter (0)
• b) eine im Wesentlichen vertikal angeordnete Trenneinrichtung (9) durch die zumindest ein Teil des Behälters in mindestens zwei kommunizierende Räume (12, 15) unterteilt wird, wobei die mindestens zwei kommunizierenden Räume zumindest an zwei Stellen miteinander in Fluidverbindung (und/oder Strömungsverbindung) stehen wodurch das Reaktionsmedium die durch die mindestens zwei Räume (12, 15) gebildete Strecke im Naturumlauf durchläuft, und
• c) mindestens zwei Zugabeeinrichtungen (16, 17) im ersten (12) der mindestens zwei kommunizierenden Räume.

This object is achieved by a device for chlorinating at least one alkene to at least one chlorinated alkane, comprising the following parts:

• a) a container ( 0 )
• b) a substantially vertically arranged separating device ( 9 ) through the at least part of the container into at least two communicating spaces ( 12 . 15 ), wherein the at least two communicating spaces are in fluid communication (and / or flow communication) with each other at least at two locations whereby the reaction medium communicates through the at least two spaces ( 12 . 15 ) passes through formed range in natural circulation, and
• c) at least two addition devices ( 16 . 17 ) in the first ( 12 ) of the at least two communicating rooms.

Preferably, the container is ( 0 ) around a cylindrical container, which is particularly preferably arranged substantially vertically.

Preferably, the two communicating rooms ( 12 . 15 ) above and below the separator ( 9 ) are in fluid communication with each other, more preferably one ( 12 ) of the at least two communicating rooms ( 12 . 15 ) may be formed as a reaction space, in particular the first space ( 12 ).

The separating device ( 9 ) around a mechanical separator.

With further preference, the separating device ( 9 ) around a partition.

Further preferably, the separating device ( 9 ) formed as a tube.

According to a further preferred embodiment, the separating device ( 9 ), such. B. the partition or pipe in the lower area, z. B. in the lower half of the container ( 0 ) arranged.

If the device contains at least two feed devices, it is preferable if a release route ( 19 ) is provided, in which the added starting material can dissolve in the reaction medium.

Preferably, the Lösestrecke ( 19 ) above the ethene addition device.

According to the invention, one or both feed devices ( 16 . 17 ), for example, in the lower region, preferably in the lower fourth of the first space ( 12 ) can be arranged.

More preferably, the at least one feed device ( 16 . 17 ) at least one, in a tangential direction facing outflow opening ( 330 ), so that one in the first room ( 12 ) can be set in rotation by a medium emerging from the at least one outflow opening mass flow. Alternatively, the feed device can be set in motion.

Further preferred is in the first room ( 12 ) at least one mixing device ( 10 . 11 ) arranged. Particularly preferably, the mixing device is arranged above the feed device (s). The mixing device is preferably one or more static mixing devices.

More preferably, the container ( 0 ) a liquid space ( 18a ) and a steam room ( 18 ), wherein the separating device ( 9 ) in the liquid space ( 18a ) of the container ( 0 ) is arranged.

More preferably, the device comprises a discharge device, which is designed to the reaction product ( 1 ) gas or as a vapor, liquid or both gaseous and liquid auszuschleusen.

More preferably, the first room ( 12 ) with a steam room ( 18 ), from which the reaction product ( 1 ) can be discharged.

The two rooms ( 12 . 15 ) are so completely submerged in the liquid that a natural circulation of the liquid in the liquid space ( 18a ) between the rooms 12 and 15 is possible. For this purpose, the liquid should above the upper edge of the separator ( 9 ) survive.

Also, in the steam room ( 18 ) of the container ( 0 ) one or more filters ( 2 ) like one or more coalescing filters ( 2 ) and / or one or more separation devices ( 6 ) such as one or more valve trays, trays, beds or packings and / or one or more demisters ( 3 ) and or one or more droplet separators ( 4 ) can be arranged. These are preferably arranged in front of the discharge device, so that the product first passes through these devices before it is discharged.

Furthermore, in the steam room ( 18 ) one product (eg EDC) reflux ( 5 ) can be arranged.

Furthermore, the device according to the invention can provide a level control ( 8th ) (eg a LIC controller), e.g. B. can serve to adjust and / or regulation of natural circulation. With the LIC controller z. For example, the height of the medium above the separating element of the process chambers can be regulated, which sets a different average density difference between the communicating spaces, which in turn results in a change in the equilibrium of forces which causes a change in the velocity of the circulating medium. To control the natural circulation and a throttle element can be installed, for example in the form of a shutter as in a furnace train control.

Furthermore, the device according to the invention may contain a device via the withdrawn reaction medium ( 20 ) via a pump ( 21 ) and a cooler ( 22 ) a discontinuous discharge stream ( 23 ) can be supplied. Alternatively or additionally, this withdrawn reaction medium ( 20 ) also a solution stream ( 24 ) are fed into the one or more starting materials (in particular chlorine) via a mixing device ( 25 ), which is shaped, for example, as an injector. Subsequently, the reaction medium thus enriched with starting material can be fed via an addition device ( 16 ) are returned to the reactor.

Furthermore, the object of the present invention is achieved by a process for the preparation of a reaction product from at least two educts, which is characterized in that the process is carried out in a device according to the invention.

• a) das erste Edukt über eine erste Zugabeeinrichtung (17) und das zweite Edukt über eine zweite Zugabeeinrichtung (16) in den ersten der mindestens zwei kommunizierenden Räume (12) gegeben werden,
• b) der Behälter (0) eine vorzugsweise im Wesentlichen vertikal angeordnete Trenneinrichtung (9) enthält, durch die zumindest ein Teil des Behälters in mindestens zwei kommunizierende Räume (12, 15) unterteilt wird, wobei die mindestens zwei kommunizierenden Räume zumindest an zwei Stellen (vorzugsweise oberhalb und unterhalb der Trenneinrichtung) miteinander in Fluidverbindung stehen,
• c) der erste Raum (12) und der zweite Raum (15) ein Reaktionsmedium enthalten, welches das Reaktionsprodukt und gegebenenfalls einen Katalysator bzw. ein Katalysatorsystem enthält, und
• d) das Reaktionsmedium die durch die mindestens zwei Räume (12, 15) gebildete Strecke im Naturumlauf durchläuft.

In particular, the present invention relates to a process for the preparation of a chlorinated alkane, from at least two starting materials, which is characterized in that

• a) the first starting material via a first feed device ( 17 ) and the second educt via a second feed device ( 16 ) in the first of the at least two communicating rooms ( 12 ) are given,
• b) the container ( 0 ) a preferably substantially vertically arranged separating device ( 9 ) through which at least a part of the container in at least two communicating spaces ( 12 . 15 ), wherein the at least two communicating spaces are in fluid communication with each other at least at two locations (preferably above and below the separation means),
• c) the first room ( 12 ) and the second room ( 15 ) contain a reaction medium which contains the reaction product and optionally a catalyst or a catalyst system, and
• d) the reaction medium passing through the at least two spaces ( 12 . 15 ) passes through formed range in natural circulation.

The reaction product is more preferably 1,2-dichloroethane and the educts are chlorine and ethene.

The starting materials are preferably dissolved in the reaction medium.

Weather preferably, the starting materials and the reaction medium after the addition of the educts are mixed, for. B. by a static mixer.

According to the invention, the first starting material (eg chlorine) is fed via a first feed device ( 17 ) and the second educt (eg ethene) via a second feed device ( 16 ) in the first of the at least two communicating rooms ( 12 ).

Again preferably, the reaction product is discharged through a vapor space, more preferably gaseous and / or liquid.

More preferably, the natural circulation can be regulated via a floor control.

More preferably, a portion of the reaction medium can be discharged and optionally cooled. This discharged and optionally cooled reaction medium can be mixed with an educt (for example chlorine) and introduced into the container ( 0 ) to be led back.

More preferably, the reaction medium is in liquid form, wherein above the reaction medium is a vapor space from which the reaction product can be discharged liquid and / or gaseous.

More preferably, the lower portion of the container ( 0 ) so filled with a liquid that in the container ( 0 ) a liquid space ( 18a ) and a steam room ( 18 ), and the separating device ( 9 ) completely in the liquid space ( 18a ) is arranged.

The product to be released preferably passes through one or more devices for droplet and / or aerosol separation.

The process according to the invention is particularly preferably carried out in a device according to the invention.

The present invention particularly preferably relates to a process for the preparation of a chlorinated alkane (eg EDC) from chlorine and alkene (eg ethene), which comprises circulating a reaction medium comprising a chlorinated alkane and optionally a catalyst or a catalyst system, one through at least two communicating spaces ( 12 . 15 ) undergoes formed reaction path in natural circulation, wherein the communicating spaces ( 12 . 15 ) with a vapor space arranged on the upper side ( 18 ), from which the reaction product ( 1 ) is discharged either gaseous or liquid or both gaseous and liquid, and preferably the two communicating spaces in a container ( 0 ) are formed by a substantially vertically arranged separating device such that the two communicating spaces are preferably in fluid communication with each other above and below the separating device.

Preferred catalysts or catalyst systems are FeCl ₃ , NaCl and O ₂ .

Preferably, a catalyst system is used which is composed of FeCl ₃ , NaCl and O ₂ . Ferric chloride preferably is present in the reactor circulation medium at a concentration of up to 2500 ppm. Sodium chloride acts in particular as a promoter; it restricts z. As the formation of by-products, and thus preferably increases the selectivity of the reaction. Sodium chloride and iron chloride are preferably used in a molar ratio of about 0.5. The oxygen is z. B. the reaction zones in the form of air together with chlorine. Owing to its biradical character, the oxygen serves, in particular, as a free-radical scavenger and reduces or suppresses z. B. radical side reactions of chlorine with EDC.

A reaction to produce the reaction product may be carried out in a cylindrical container as described above ( 0 ) occur. The container ( 0 ) may look like a conventional column. A natural circulation in the container is achieved by two communicating spaces ( 12 . 15 ) be created. One of the two communicating rooms can be charged with educts. The educt-loaded reaction space ( 12 ) may correspond to the riser of a conventional reactor loop. The two communicating spaces can be created by the introduction of a partition plate as a partition, a central tube as a separation tube or any other geometric arrangement that is suitable to produce communicating spaces.

By integrating several process steps, such as the introduction and solution of the educts chlorine and ethene in the solvent EDC, the natural circulation of the solvent EDC, the reaction, and the droplet and aerosol deposition in a z. B. cylindrical, vertical container results in the advantage that, while maintaining the advantages of a conventional boilers with natural circulation a very compact design can be achieved. In particular, by the column shape a small footprint is needed. The device can be erected for example on a frame. This eliminates the need for an extensive steel construction. This in turn leads to lower production costs and a smaller footprint. Furthermore, a small hold-up (liquid content of the reactor) can be achieved, resulting in an advantage in an environmental assessment.

The approach of the invention makes it possible to produce a reaction product with a low material input and at low production costs; it is suitable, for example, for producing EDC, in particular with high purity.

The Eduktaufgabe can accordingly DE 10 2004 029 147 by the installation of sequential addition sections (adding device (s) ( 16 . 17 ), Detachment distance ( 19 ), Mixer ( 10 . 11 )) or reaction sections, which leads to a significant reduction of the reaction distances and thus opens up a further possibility to make the reaction space in an economic size.

A spatial separation of the reaction space and downwardly flowing EDC can be achieved by a simple separating plate, for example, approximately in the center of the z. B. cylindrical column part can be introduced. The reaction space, that is, the upward flow of the natural circulation, may, for example, have a somewhat larger cross-section than the downwardly flowing part, since in this subarea the greater mass and above all volume flow is moved. By this measure, the dynamic pressure loss can be minimized. The optimum aspect ratio can be determined by a flow simulation. Also by simulation calculation, the opening degree, or distance between separating plate and column bottom, and the length of the separating plate can be determined. Due to analogous conclusions of already built reactors with natural circulation in conventional technology, the typical length of the separating plate or separator tube z. B. be about 15 m. The opening cross section at the bottom of the column should preferably correspond at least to the cross-section of the communicating process spaces.

The natural circulation sets itself, as in a conventional loop reactor, by the density difference in the two rooms. Due to the gaseous educts which are added to the reaction space and due to the higher temperature resulting from the heat of reaction, a lower average density sets in the reaction space. This is the driving force for the natural circulation.

Instead of a divider, the spatial separation within the column can also be achieved by other design elements. Fluidically favorable z. B. a central separation tube, since it has the advantage of rotational symmetry.

Further advantages and embodiments of the invention will become apparent from the description and the accompanying drawings.

It is understood that the features mentioned above and those yet to be explained below can be used not only in the particular combination given, but also in other combinations or in isolation, without departing from the scope of the present invention.

The invention is illustrated schematically by means of exemplary embodiments in the drawings and will be described in detail below with reference to the drawings.

1 shows a reactor with separation pipe according to an embodiment;

2 shows a reactor with a partition according to another embodiment;

3a shows a cross-sectional view of a Eduktaufgabevorrichtung according to another embodiment;

3b shows a longitudinal sectional view of a Eduktaufgabevorrichtung according to another embodiment;

3c shows a feed opening according to another embodiment;

4 shows a cross section of a reactor with separation pipe according to another embodiment; and

5 shows a cross section of a reactor with a partition wall according to another embodiment.

1 shows a direct chlorination reactor containing a standing cylindrical container ( 0 ), in which liquid EDC circulates. One possible direction of rotation is in 1 indicated by arrows. In the container, the reaction in space ( 12 ) be performed. Furthermore, the addition points for chlorine ( 16 ) and ethene ( 17 ).

A regulation of the natural circulation can, for example, by means of a level control ( 8th ) (LIC control), which can also be used to set the natural circulation speed. The height of the medium above the separating element of the process chambers is preferably regulated by means of the LIC controller, as a result of which a different mean density difference of the media between the communicating spaces sets, which in turn results in a change in the equilibrium of forces which causes a change in the speed of the circulating medium , To control the natural circulation and a throttle element can be installed, for example in the form of a shutter as in a furnace train control.

In the lower part of the reactor is a separation tube ( 9 ), which moves the reactor into an ascending and descending flow space ( 12 . 15 ).

Gaseous, pressurized ethene ( 14 ) can be connected via control valves to at least one ethene access point ( 17 ). The at least one ethene addition point can be designed in such a way that fine bubbles can form, which can be found in the dissolution section (FIG. 19 ) can dissolve quickly in the EDC. The bubbles are in 1 symbolically indicated by dots. The Ethen-Verteiler or Sparger ( 17 ) and the dissolution lines ( 19 ) can optionally be arranged several times in succession.

The chlorine to be introduced ( 13 ) can first be solved in EDC. For this purpose, a partial flow ( 20 ) of the generated EDC from the downflowing space ( 15 ) and then removed from the pump ( 21 ) in the cooler ( 22 ). The stripped EDC can be transformed into an EDC stream ( 23 ) and into a solution stream ( 24 ). In the EDC stream ( 23 ) may also be a discontinuous discharge stream. The solution stream ( 24 ) may subsequently be added to the 25 ), where the gaseous chlorine ( 13 ) can be supplied. The chlorine solution can be regulated to the at least one chlorine addition point ( 16 ) and with nozzles in the reaction space ( 12 ) are injected, with the largest possible turbulence can be generated.

Above the at least one chlorine addition point ( 16 ) can join the reaction section, in which the reaction in the pure Liquid phase can take place. In order to improve the mixing, static mixers ( 10 ) and ( 11 ) be integrated.

In the upper part of the separation tube ( 9 ) can connect to the reaction zone of the boiling range. This is in 1 indicated by blistering. The vaporous EDC can enter the vapor space ( 18 ) evaporate the reactor and as a vaporous EDC product ( 1 ) are discharged.

For leaching a possibly entrained catalyst, which is dissolved for example in aerosols, optionally one or more separating trays ( 6 ) are used. For example, sieve or valve trays, but also column packings or random packings can be used for this purpose. For this separator ( 6 ) a backwash option can be provided.

For further droplet and aerosol separation, serial laminar separators ( 4 ), Demister ( 3 ) and aerosol filters ( 2 ) to be ordered.

The product (EDC) can finally be discharged at the upper end of the reactor (EDC vapor stream 1 )

Before starting up the reactor, it is preferably filled with pure EDC (in particular feed quality).

2 shows a device according to another embodiment of the present invention. In the 2 shown device differs from the in 1 shown device only in the shape of the separator ( 9 ). According to this embodiment, the separating device ( 9 ) designed as a partition.

The 3a and 3b show schematic diagrams of a Eduktaufgabevorrichtung for generating a rotating medium stream, according to an embodiment of the present invention.

By means of a feed-in line ( 314 ) can a feed-in medium be a saver ( 317 ). For example, it may be one of the in the 1 and 2 shown austerity ( 16 . 17 ) act. The Sparger ( 317 ) has feed-in bores ( 330 ) on. For the sake of clarity, only one of the feed bores ( 330 ) provided with a reference numeral. According to this embodiment, the feed bores ( 330 ) of the Sparger ( 317 ) all in the same direction.

3c shows an opening angle α (to the horizontal) of a feed bore ( 330 ). For example, the angle α may have a value of 30 ° or 40 °. Other suitable aperture angles, for example between said values, may also be used.

4 shows a cross section through a boiling reactor according to an embodiment of the device according to the invention. The boiling reactor is designed as a separation tube reactor or central tube reactor. In the container ( 0 ) is the separating device in the form of a separating tube ( 9 ) educated. The separation pipe ( 9 ) is preferably centered in the container ( 0 ) arranged. Through the separation tube ( 9 ), the interior of the container can be subdivided into two sections which are only located at the upper and lower ends of the separating tube (FIG. 9 ) are in fluid communication with each other so as to form two communicating spaces.

Through the arrows is a possible flow direction within the separation tube ( 9 ) and within the reflux space which exists between the inner wall of the container ( 0 ) and the outer wall of the separation tube ( 9 ) is formed, indicated. Accordingly, a within the separation tube ( 9 ), and move down a medium within the reflux space.

For example, the diameter of the container can be 2.7 m and the diameter of the separating tube 2.0 m. Characterized a cross sectional area of the container A _ges = 5.72 m ^2, a cross sectional area of the shroud pipe _to A = 3.14 m ² and a cross-sectional area of the return space _from A = 2.58 m ² can result.

5 shows a cross section through a boiling reactor according to a werteren embodiment of the device according to the invention. The boiling reactor is designed as a partition wall reactor. In the container ( 0 ) is the separating device in the form of a partition ( 9 ) educated. The partition ( 9 ) can in the container ( 0 ) be arranged so that they the interior of the container ( 0 ) divided into two sections. The two sections can only at the top and bottom of the partition ( 9 ) communicate with each other to form two communicating spaces. The partition can z. B. be arranged in the container so that the two spaces ( 12 . 15 ) have different sizes.

The arrows indicate a possible flow direction within the two sections. Thus, a medium located within the larger portion may move up and a medium within the smaller portion may move down.

For example, the diameter of the container can be 2.7 m and the partition ( 9 ) Can divide the interior of the container so that a cross sectional area of the larger section _on A = 3.14 m ² and a cross-sectional area of the smaller section A _ab = 2.58 m ^2.

The present invention provides an apparatus for direct chlorination of at least one alkene to at least one chlorinated alkane by means of chlorine, wherein the reaction of alkene and chlorine to form a chlorinated alkane and the transport of the solvent, which may correspond to the chlorinated alkane, in a standing cylindrical container , which is characterized in that at least two communicating spaces are prepared by a mechanical separation device, for example in the form of a separation tube or a partition, in which adjusts itself by the Eduktaufgabe and the exothermic reaction density difference, a natural circulation.

For this purpose, a multiplicity of addition sections and furthermore static and / or dynamic mixing devices can be arranged in the room unit in which the liquid rises.

The adding device, z. As sparger for the chlorinated alkane and chlorine, may be designed so that the outflow holes or nozzles of the adding device have in a tangential direction, so that by the exiting mass flow of the mixture of chlorinated alkane and chlorine, a pulse is formed, which is the upward-flowing solvent medium set in rotation and thereby sets a cross-mixing.

In another embodiment, the present invention provides a process for producing high purity chlorinated alkanes from dissolved chlorine and dissolved alkane which are contacted with each other using a recirculating liquid reaction medium consisting essentially of a chlorinated alkane and a catalyst or catalyst system and passes through at least one vertically arranged, designed as a communicating room unit reaction path, wherein the communicating room units are connected to a vapor space on the upper side, from which the reaction product is discharged either gaseous or liquid or both gaseous and liquid.

The described embodiments are described by way of example only and may be combined. The shapes and dimensions shown may be replaced by suitable others. The described devices may be suitable for carrying out the process according to the invention for producing a reaction product. The inventive approach is not limited to the preparation of the reaction products described but can be used to prepare further reaction products from appropriately suitable starting materials.

LIST OF REFERENCE NUMBERS

0

container

1

EDC vapor stream

2

coalescencefilter

3

demister

4

Droplet

5

EDC return (optional)

6

Valve shelves (optional), for example only: other types of shelves or beds or packs can be used

7

EDC liquid surface, boiling

8th

Level control, also for setting the natural circulation speed

9

Separating device (eg dividing wall or separating tube)

10

Static mixer

11

Static mixer

12

1st room (reaction room)

13

chlorine task

14

Ethenaufgabe

15

2nd room

16

EDC / chloro-Sparger

17

Ethene sparger

18

steam room

18a

liquid room

19

dissolving section

20

stripped EDC

21

EDC pump

22

EDC cooler

23

(discontinuous) discharge stream

24

Solution stream, EDC

25

Chlorine mixing device (injector)

314

feeder

317

sparger

330

feed openings

Claims (16)

Device for producing a chlorinated alkane, the device comprising the following parts: a) a container ( 0 ) b) a vertically arranged separating device ( 9 ) through the at least part of the container into at least two communicating spaces ( 12 . 15 ), wherein the at least two communicating spaces in fluid communication with each other at least at two points whereby the reaction medium through the at least two spaces ( 12 . 15 ) passes through the natural circulation path, and c) at least two addition devices ( 16 . 17 ) in the first ( 12 ) of the at least two communicating rooms. Apparatus according to claim 1, characterized in that it is in the container ( 0 ) by one cylindrical container, which is preferably arranged vertically. Device according to one of the preceding claims, characterized in that the two communicating spaces ( 12 . 15 ) with each other above and below the separator ( 9 ) are in fluid communication. Device according to one of the preceding claims, characterized in that it is in the separating device ( 9 ) is a partition wall or a pipe. Device according to one of the preceding claims, characterized in that the separating device ( 9 ) in the lower area, in particular in the lower half of the container ( 0 ) is arranged. Device according to one of the preceding claims, characterized in that at least one feed device ( 16 . 17 ) in the lower region, preferably in the lower fourth of the first space ( 12 ) is arranged. Device according to one of the preceding claims, characterized in that the two addition devices ( 16 . 17 ) are arranged one above the other. Device according to one of the preceding claims, characterized in that in the first space ( 12 ) at least one mixing device ( 10 . 11 ), in particular a static mixing device. Device according to one of the preceding claims, characterized in that the container ( 0 ) a liquid space ( 18a ) and a steam room ( 18 ), wherein the separating device ( 9 ) in the liquid space ( 18a ) of the container ( 0 ) is arranged. Device according to one of the preceding claims, characterized by a discharge device, which is designed to produce the reaction product ( 1 ) gaseous, liquid or gaseous as well as liquid auszuschleusen. Device according to one of the preceding claims, characterized in that in the vapor space ( 18 ) of the container ( 0 ) at least one filter ( 2 ) like a coalescing filter ( 2 ) and / or at least one demister ( 3 ) and / or at least one droplet separator ( 4 ) and / or at least one separating device ( 6 ) is arranged as a separating tray, a bed or a pack. Process for the preparation of a chlorinated alkane, from at least two educts, characterized in that a) the first educt via a first feed device ( 17 ) and the second educt via a second feed device ( 16 ) in the first of the at least two communicating rooms ( 12 ), b) the container ( 0 ) a vertically arranged separating device ( 9 ) through which at least a part of the container in at least two communicating spaces ( 12 . 15 ), wherein the at least two communicating rooms are in fluid communication with each other at least at two points, c) the first space ( 12 ) and the second room ( 15 ) contain a reaction medium containing the reaction product and optionally a catalyst or a catalyst system, and d) the reaction medium passing through the at least two spaces ( 12 . 15 ) passes through formed range in natural circulation. A method according to claim 12, characterized in that the reaction medium by a mixing device ( 10 . 11 ), in particular a static mixer, is mixed. Method according to one of claims 12 to 13, characterized in that the lower region of the container ( 0 ) is filled with a liquid that in the container ( 0 ) a liquid space ( 18a ) and a steam room ( 18 ) is formed, and that the separating device ( 9 ) completely in the liquid space ( 18a ) is arranged. Method according to one of claims 12 to 14, characterized in that the container ( 0 ) comprises a discharge device through which the reaction product ( 1 ) is discharged through the gas space gaseous, liquid or both gaseous and liquid. Method according to one of claims 12 to 15, characterized in that the reaction product is 1,2-dichloroethane and the starting materials are chlorine and ethene.

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