Device and method for producing partially chlorinated alkanes

Abstract

The invention relates to a device and a method for producing partially chlorinated alkanes by means of a direct chlorination of alkenes. In particular, the invention relates to a device and a method for producing 1,2-dichloroethane by means of a direct chlorination of ethene (synonym: ethylene). The invention is characterized in that a loop reactor is used for the direct chlorination, wherein the outlet for the produced partially chlorinated alkane is provided on a vertical position of the loop reactor (in the operating state) on a lateral wall of the loop reactor, the vertical position being situated below half the height of the loop reactor.

Description

[0001] thyssenkrupp Uhde GmbH, thyssenkrupp AG, WESTLAKE VINNOLIT GMBH &

[0002] CO. KG

[0003] P149529PC00

[0004] Apparatus and method for the production of partially chlorinated alkanes

[0005] The present invention relates to an apparatus and a method for the production of partially chlorinated alkanes by direct chlorination of alkenes. In particular, the present invention relates to an apparatus and a method for the production of 1,2-dichloroethane by direct chlorination of ethene (synonym: ethylene). The invention is characterized in that a loop reactor is used for the direct chlorination, wherein the discharge for the produced partially chlorinated alkane is arranged at a vertical position of the loop reactor (in the operating state) on a side wall of the loop reactor that is located below half the height of the loop reactor.

[0006] 1,2-Dichloroethane is often produced in a so-called stand-alone direct chlorination plant and transported to the site of an "unbalanced" plant complex. Stand-alone direct chlorination plants offer operators of chlorine-alkali electrolysis plants the possibility of further processing the resulting chlorine on-site without having to construct a plant complex for the production of vinyl chloride.

[0007] The direct chlorination plant is usually operated with a certain excess of ethylene to ensure complete chlorine reaction and prevent even small amounts of chlorine from being discharged from the reactor. This excess ethylene is discharged from the plant along with the reactor exhaust gas, which also contains inert elements present in the feedstocks, such as oxygen, hydrogen, nitrogen, and alkanes that are inert with respect to the direct chlorination reaction. To prevent the formation of explosive gas mixtures, an inert gas is added to the reactor exhaust gas. In plants combined with oxychlorination, this inert gas is ethylene. The exhaust gas from the direct chlorination process is mixed with the ethylene feed stream for the oxychlorination process and further processed to produce 1,2-dichloroethane.

[0008] Stand-alone direct chlorination plants do not have this option – nitrogen must be used as the inerting medium. Nevertheless, the reaction requires an excess of ethylene – ideally as small as possible for cost reasons – to ensure complete chlorine removal. The smaller this excess, the more economically the plant can be operated. However, with very low ethylene excesses, the likelihood increases that traces of chlorine will be carried out at the top of the reactor due to fluctuations in the boiling point of the reaction medium, leading to a reduction in product quality. Therefore, a process is needed that can be operated with very low ethylene excesses while simultaneously producing a high-quality product.

[0009] This problem is solved by the features of claim 1. The dependent claims represent advantageous further developments.

[0010] The present invention thus relates to a device for the production of partially chlorinated alkanes, comprising a loop reactor which has a first feed for an alkene to be chlorinated, a second feed for a chlorinating agent and a first discharge for the produced partially chlorinated alkane, wherein the first discharge for the produced partially chlorinated alkane is arranged in a vertical position of the loop reactor on a side wall of the loop reactor which is located below half the height of the loop reactor.

[0011] To meet the requirements described above and to solve the problem underlying the invention, it is proposed according to the invention to draw off an EDC side stream from the lower part of the reactor downpipe and subject it to flash evaporation. The evaporated fraction can be fed directly as vapor into a downstream column or condensed and then further processed. Since a large portion of any remaining chlorine can be stripped from the reactor recirculation stream during boiling in the upper part of the reactor downpipe, the 1,2-dichloroethane flowing downwards in the reactor downpipe contains significantly less chlorine. Any remaining chlorine can react with dissolved ethylene during the additional residence time in the reactor downpipe, so that the 1,2-dichloroethane drawn off by flash evaporation can no longer contain any amounts of chlorine that could impair product quality.

[0012] The 1,2-dichloroethane vaporized at the reactor head can be condensed and returned to the reactor, with the heat of condensation being utilized through suitable heat recovery measures. The liquid phase from the flash evaporation can be further cooled and ultimately used to dissolve the chlorine. Heat recovery measures can also be applied during the further cooling of this stream.

[0013] According to a preferred embodiment, the first discharge for the produced partially chlorinated alkane is arranged in a vertical position of the loop reactor, which is located at a height of 10 to 50%, preferably 15 to 45%, more preferably 20 to 40%, and particularly preferably 30 to 40% of the height of the loop reactor.

[0014] Another preferred embodiment provides that a riser pipe is arranged in the loop reactor, dividing the loop reactor into an inner riser zone and an outer fall zone. Alternatively, the loop reactor can also be provided with a riser pipe and a spatially separate fall pipe to form an outer circulation, with fluid connecting to each other at both ends, for example via a lower deflection zone and an upper separation zone. In this case, the riser pipe forms a riser zone and the fall pipe a fall zone of the loop reactor.

[0015] According to a further preferred embodiment, the first feed for an alkene to be chlorinated and the second feed for a chlorinating agent each open into the riser pipe, with the opening of the first feed for an alkene to be chlorinated preferably being arranged below the opening of the second feed for a chlorinating agent.

[0016] Another preferred embodiment provides that the first discharge of the produced partially chlorinated alkane takes place from the falling zone.

[0017] Preferably, a product stream extracted via the first discharge is directed into a phase separation vessel, preferably with a pressure relief valve upstream.

[0018] Another preferred embodiment provides that the phase separation vessel has a first discharge arranged at the bottom, through which a liquid first partial stream of a partially chlorinated alkane can be discharged and the first partial stream is directed to a mixing device, e.g. a liquid jet gas compressor, wherein the mixing device is designed to mix the chlorinating agent with the first partial stream of the partially chlorinated alkane, and a mixture stream generated in the mixing device subsequently flows into the loop reactor via the second feed.

[0019] For example, the first partial flow may be passed through a heat sink and / or a cooler before being fed into the mixing device, and / or a pump may be provided to convey the first partial flow.

[0020] Another preferred embodiment provides that a branch of the first partial stream is directly returned to the loop reactor, the branch preferably opening into the fall zone, and particularly preferably opening into the fall zone below the first discharge into the fall zone.

[0021] According to a further preferred embodiment, the phase separation vessel has a second outlet arranged at the top, through which a gaseous second partial stream of a partially chlorinated alkane can be discharged.

[0022] Another preferred embodiment provides that the second partial stream is fed via a product condenser as condensed partially chlorinated alkane to a stripping column to obtain a purified stream of the partially chlorinated alkane.

[0023] Preferably, the stripping column has a bottom outlet through which the purified stream of the partially chlorinated alkane can be discharged, particularly preferably via a stripping column sump pump.

[0024] In preferred embodiments, the stripping column is provided to have a feed for an inert gas and / or a circulating evaporator, wherein a partial stream of the purified stream of the partially chlorinated alkane is returned to the stripping column and heated by means of the circulating evaporator.

[0025] Furthermore, it can preferably be provided that the stripping column has a top-side outlet through which gaseous products can be discharged from the stripping column, the outlet leading into a condenser.

[0026] Another preferred embodiment provides that the product condenser and / or the return tank each have an outlet for gaseous products that is led into the condenser.

[0027] According to a further preferred embodiment, the condenser has an outlet for condensed products which is led into a stripper head condensate tray.

[0028] Another preferred embodiment provides that the condenser and / or the stripper head condensate tray each have an outlet for gaseous products, which is directed into a freezer.

[0029] According to a further preferred embodiment, the freezer is provided to have a return system for condensed products into the stripper head condensate reservoir and a discharge option for non-condensable products.

[0030] Another preferred embodiment provides that the stripper head condensate reservoir has a bottom outlet through which a liquid product stream can be returned to the loop reactor, preferably by means of a stripper head condensate pump.

[0031] According to a further preferred embodiment, the recirculated product stream is provided to flow into the fall zone of the loop reactor, with the outlet preferably being arranged above the first discharge.

[0032] In preferred embodiments, the second partial stream is supplied to the product condenser via a high-boiling column, preferably with a pressure regulating valve arranged upstream of the high-boiling column.

[0033] It is also advantageous that the high-boiling column has a top-side outlet for a top stream, through which gaseous components can be discharged from the device.

[0034] According to a further preferred embodiment, the product condenser for condensing the partially chlorinated alkane is connected downstream of the top-side outlet for a top-side flow, and a return vessel for collecting the condensed partially chlorinated alkane is preferably connected downstream of the product condenser.

[0035] Another preferred embodiment provides that the reflux tank has a bottom outlet through which the condensed semi-chlorinated alkane can be withdrawn from the reflux tank and divided into a first partial stream of the condensed semi-chlorinated alkane and a second partial stream of the condensed semi-chlorinated alkane, wherein the first partial stream of the condensed semi-chlorinated alkane is recycled to the high-boiling column and the second partial stream of the condensed semi-chlorinated alkane is fed to a stripping column, wherein a reflux pump is preferably provided for conveying the condensed semi-chlorinated alkane withdrawn from the reflux tank.

[0036] Another preferred embodiment provides that the loop reactor has a second outlet located at the top for gaseous partially chlorinated alkane. According to a further preferred embodiment, the gaseous partially chlorinated alkane discharged via the second outlet located at the top is fed to a heat exchanger for condensation and, as condensed partially chlorinated alkane, is fed to a storage tank via a feeder.

[0037] According to a further preferred embodiment, the storage container and / or the feed of the condensed partially chlorinated alkane into the storage container has an inert gas addition device.

[0038] Another preferred embodiment provides that the feed tank has a bottom feed tank outlet through which the condensed partially chlorinated alkane is preferably returned to the loop reactor via a feed tank sump pump.

[0039] According to a further preferred embodiment, the feed vessel has a top-side feed vessel outlet for the discharge of an exhaust gas stream, wherein the exhaust gas stream is preferably directed directly into the condenser of the high-boiling column and / or the stripping column.

[0040] Another preferred embodiment provides that the high-boiling column has a bottom outlet through which a stream of liquid products is discharged, preferably by means of a sump pump.

[0041] According to a further preferred embodiment, the flow of liquid products is provided in a first high-boiling column partial flow and a second high-boiling column partial flow, wherein the first high-boiling column partial flow is fed into the circulating evaporator of the high-boiling column and is evaporated there and subsequently returned to the high-boiling column, and liquid products are discharged from the device with the second high-boiling column partial flow.

[0042] The present invention is characterized in more detail below, without limiting the invention to the parameters specifically described.

[0043] The present invention relates in particular to an apparatus and a process achievable therewith for the direct chlorination of ethylene to 1,2-dichloroethane, which, due to its special reaction control, allows for particularly high yields of 1,2-dichloroethane and high product purities even at a high reaction temperature, typically 120°C. The special feature of the process is the dissolution of the gaseous raw materials chlorine and ethylene in the reaction medium 1,2-dichloroethane in a homogeneous liquid phase prior to the actual reaction. The reactor is a gas lift loop reactor with internal or external circulation, wherein the reaction medium is circulated in natural circulation. The produced quantity of 1,2-dichloroethane is withdrawn as vapor at the reactor head. Ethylene is added to the main circulation stream in the reactor riser pipe, thus facilitating natural circulation. Simultaneously, the ethylene dissolves in the circulating 1,2-dichloroethane as it travels along the riser pipe.To dissolve the chlorine, a partial stream of 1,2-dichloroethane is taken from the reaction cycle and cooled to a temperature of typically 45-60 °C, at which the chlorine is readily soluble and side reactions such as further chlorination to 1,1,2-trichlorethane are suppressed.

[0044] In general, direct chlorination plants are operated within the integrated production plant for vinyl chloride, which, in addition to direct chlorination, includes other plants such as the oxychlorination of ethylene to 1,2-dichloroethane and the thermal cracking of 1,2-dichloroethane to vinyl chloride and hydrogen chloride, as well as distillation plants for purifying the intermediate product 1,2-dichloroethane and the final product vinyl chloride.

[0045] However, it is also possible to operate such a plant complex without direct chlorination (so-called unbalanced operation). In this case, the demand for 1,2-dichloroethane is met from external sources.

[0046] Exemplary embodiments of devices according to the invention are described below with reference to the accompanying figures: Fig. 1 schematically shows a first embodiment of a device for the production of partially chlorinated alkanes comprising a loop reactor with internal circulation, and

[0047] Fig. 2 schematically shows a second embodiment of a device for the production of partially chlorinated alkanes comprising a loop reactor with external circulation.

[0048] Fig. 1 shows a loop reactor with circulating liquid EDC as the reaction medium, in which chlorine as chlorinating agent 2 and ethylene are reacted to form 1,2-dichloroethane (EDC). The ethylene is fed in gaseous form via a first feed 3 for an alkene to be chlorinated into the lower part of the riser 4 and dissolves in the circulating EDC within a riser zone 5 of the reactor. An EDC stream is drawn from the reactor downpipe 6 below half the height of the loop reactor 1 via a first outlet for partially chlorinated alkane 7 and expanded via an expansion valve 8 into a phase separation vessel 9. The EDC, vaporized by the expansion, is fed as a gaseous second partial stream of the partially chlorinated alkane 10 via a pressure regulating valve 11 into a column 12 for the removal of high-boiling byproducts ("high-boiling column").The liquid EDC, cooled by flash evaporation, can be further cooled by a suitable heat sink 14 for heat recovery before being cooled in the recirculating chiller 15 to the temperature required for chlorine dissolution. After cooling, the EDC stream is fed to a mixing device 16, preferably as the driving jet of a liquid jet gas compressor for drawing in and dissolving the chlorine. Depending on the selected operating parameters, a partial flow of the EDC stream 13 from the flash evaporation can be returned directly to the reactor 1 via a branch 17a. The EDC recirculation pump 18 is used to circulate the liquid EDC from the flash evaporation tank 9.

[0049] Vaporous EDC is drawn off at the top of reactor 1 via a discharge 19 for gaseous, partially chlorinated alkane and subsequently condensed in a heat exchanger 20. The heat exchanger 20 can serve as the circulating evaporator for the high-boiling column 12. The heat removed can at least partially cover the heat demand of the column 12. The condensed EDC is collected in a storage tank 22 (EDC condensate tank) via a feed for condensed partially chlorinated alkane and pumped back into reactor 1 by means of the EDC condensate pump 23. The condensed EDC also contains inerts such as oxygen, hydrogen, and nitrogen, which can be separated and discharged from the condensate tank. To prevent the formation of explosive gas mixtures, nitrogen is added to the outlet stream of the circulating evaporator 20 via an inert gas injection device 41.

[0050] In the high-boiling column 12, components with higher boiling points than EDC are drawn off at the bottom. The second high-boiling column partial stream 24, containing the high-boiling components, is pumped to the plant boundary for further processing by the bottom pump 25. The EDC drawn off as the top stream 26 of the high-boiling column is condensed by the EDC product condenser 27, collected in the reflux tank 28, and partially returned to the top of the high-boiling column 12 as a first partial stream of the condensed partially chlorinated alkane 30 by the reflux pump 29.

[0051] The remaining condensed EDC is fed as a second partial stream of the condensed partially chlorinated alkane 31 onto the top of the stripping column 32, where low-boiling substances can be removed from the EDC. The purified EDC stream 33 is drawn off at the bottom of the stripping column 32 and conveyed as product to the plant boundary by means of the sump pump 34.

[0052] The stripping column 32 is preferably heated by means of a circulating evaporator 35. Low-pressure steam (STL) is preferably used as the heating medium, which condenses in the circulating evaporator 35 preferably to low-pressure condensate (CPL). Alternatively or additionally, stripping with nitrogen is also possible, which is supplied via an inert gas feeder 36. If nitrogen is used as an alternative for stripping, the circulating evaporator 35 can be omitted. The vaporous, low-boiling-point overhead stream of the stripper 37 first passes through a condenser 38 (stripper overhead condenser) and then the deep cooler 39. Before entering the coolers, the inert-containing exhaust gas stream 40 from the condensate receiver 22 is mixed with the stripper overhead stream 37. The liquid phases condensed in the coolers 38 and 39 are collected in the stripper head condensate reservoir 42 and pumped back into the reactor by means of the stripper head condensate pump 43.The exhaust gas flow exiting coolers 38 and 39 is directed to the plant boundary via a discharge option for non-condensable products 44 for further treatment.

[0053] Fig. 2 shows a second embodiment of the device according to the invention. The second embodiment differs from the first embodiment according to Fig. 1 in that the loop reactor 1 is designed with an external circulation. For this purpose, the loop reactor has a riser pipe 4 and a downpipe 6a arranged spatially separately from it. Riser pipe 4 and downpipe 6a each form a rising zone 5 and a falling zone 6, respectively, for the circulating reaction medium. Riser pipe 4 and downpipe 6a are in fluid communication with each other at both ends, via a lower deflection zone and an upper separation zone.

[0054] Furthermore, the statements relating to Fig. 1 apply accordingly to the second embodiment shown in Fig. 2.

[0055] In a further embodiment of the invention, not shown, the separation of high-boiling substances in the high-boiling column 12 is omitted. The vaporous EDC stream 10 from the flash evaporation is then condensed by means of at least one heat exchanger, whereby the latent heat of the EDC can optionally be used for heat recovery. The condensed, liquid EDC is then fed directly to the top of the EDC stripper. The EDC drawn off in vapor form at the reactor top no longer serves to heat the high-boiling column, but can also be condensed – with the latent heat optionally being used for heat recovery – and returned to the reactor.

[0056] Furthermore, the explanations regarding the first two exemplary embodiments apply accordingly.

[0057] Reference numeral list 1 Loop reactor

[0058] 2 Chlorinating agents, especially chlorine

[0059] 2a Second feed for a chlorinating agent

[0060] 3. First feed for an alkene to be chlorinated, in particular ethylene

[0061] 4 riser pipe

[0062] 5 ascent zone

[0063] 6 Fall zone

[0064] 6a Downpipe

[0065] 7. First removal for partially chlorinated alkane

[0066] 8. Relief valve

[0067] 9 phase separation tanks

[0068] 10 gaseous second partial stream of the partially chlorinated alkane

[0069] 11 Pressure regulating valve

[0070] 12 High-boiler column

[0071] 13. Discharge for liquid first partial stream of the partially chlorinated alkane

[0072] 14 Heat sinks, optional, for heat recovery

[0073] 15 coolers

[0074] 16 Mixing device, in particular liquid jet gas compressor

[0075] 17 liquid first partial stream of the partially chlorinated alkane

[0076] 17a Branch for partial flow back to the reactor

[0077] 18 pump

[0078] 19 Discharge for gaseous, partially chlorinated alkane

[0079] 20 heat exchangers

[0080] 21 Feed for condensed semichlorinated alkane

[0081] 22 storage containers

[0082] 23 EDC condensate pump

[0083] 24 second high-boiling column partial stream

[0084] 25 Sump pump High-boiling column

[0085] 26 Top-flow high-boiling column, vaporous

[0086] 27 Product condenser for semichlorinated alkane

[0087] 28 Return tanks High-boiling column

[0088] 29 Return pump

[0089] 30 first partial stream of the condensed semichlorinated alkane

[0090] 31 second partial stream of the condensed semichlorinated alkane

[0091] 32 Stripping column 33 Purified stream of the partially chlorinated alkane

[0092] 34. Sump pump of the stripping column

[0093] 35 Circulating evaporators of the stripping column

[0094] 36 Inert gas supply

[0095] 37 Stripper head stream, vaporous

[0096] 38 Capacitor

[0097] 39 freezers

[0098] 40 Exhaust gas flow from the condensate reservoir

[0099] 41 Inert gas addition device

[0100] 42 Stripper head condensate template

[0101] 43 Stripper head condensate pump

[0102] 44 Discharge option for non-condensable products

Claims

thyssenkrupp Uhde GmbH, thyssenkrupp AG, WESTLAKE VINNOLIT GMBH & CO. KG P149529PC00 Patent claims 1. Apparatus for the production of partially chlorinated alkanes, comprising a loop reactor (1) having a first feed (3) for an alkene to be chlorinated, a second feed (2a) for a chlorinating agent (2) and a first discharge (7) for the produced partially chlorinated alkane, characterized in that the first discharge (7) for the produced partially chlorinated alkane is arranged in a vertical position of the loop reactor (1) on a side wall of the loop reactor (1) which is located below half the height of the loop reactor (1).

2. Device according to claim 1, characterized in that the first discharge (7) for the produced partially chlorinated alkane is arranged on a vertical position of the loop reactor (1) which is located at a height of 10 to 50%, preferably 15 to 45%, more preferably 20 to 40%, particularly preferably 30 to 40% of the height of the loop reactor (1).

3. Device according to one of the preceding claims, characterized in that a riser pipe (4) is arranged in the loop reactor (1) which divides the loop reactor (1) into an inner rising zone (5) and an outer falling zone (6), or that the loop reactor (1) has a riser pipe (4) and a falling pipe (6a) arranged spatially separately therefrom for the formation of an outer circulation, which are in fluid contact with each other at both ends, wherein the riser pipe (4) forms a rising zone (5) and the falling pipe (6a) a falling zone (6) of the loop reactor (1).

4. Device according to the preceding claim, characterized in that the first feed (3) for an alkene to be chlorinated and the second feed (2a) for a chlorinating agent (2) each open into the riser pipe (4), wherein the opening of the first feed (3) for an alkene to be chlorinated is preferably arranged below the opening of the second feed (2a) for a chlorinating agent (2).

5. Device according to one of the two preceding claims, characterized in that the first discharge (7) for the produced partially chlorinated alkane takes place from the falling zone (6).

6. Device according to one of the preceding claims, characterized in that a product stream extracted via the first discharge (7) is fed into a phase separation vessel (9), preferably with a pressure relief valve (8) upstream.

7. Device according to the preceding claim, characterized in that the phase separation vessel (9) has a first discharge (13) arranged at the bottom, through which a liquid first partial stream (17) of a partially chlorinated alkane can be discharged and the first partial stream (17) is directed to a mixing device (16), e.g. a liquid jet gas compressor, wherein the mixing device (16) is designed to mix the chlorinating agent (2) with the first partial stream (17) of the partially chlorinated alkane, wherein a mixture stream generated in the mixing device (16) subsequently flows into the loop reactor (1) via the second feed (2a).

8. Device according to the preceding claim, characterized in that the first partial flow (17) is passed through a heat sink (14) and / or a cooler (15) before being fed into the mixing device (16) and / or a pump (18) is provided for conveying the first partial flow (17).

9. Device according to one of the two preceding claims, characterized in that a branch (17a) of the first partial stream is directly returned to the loop reactor (1), wherein the Branch (17a) preferably opens into the fall zone (6), and particularly preferably opens into the fall zone (6) below the first discharge (7).

10. Device according to one of the preceding claims, characterized in that the phase separation vessel (9) has a second outlet arranged at the head end, through which a gaseous second partial stream (10) of a partially chlorinated alkane can be discharged.

11. Device according to the preceding claim, characterized in that the second partial stream (10) is fed via a product condenser (27) as condensed partially chlorinated alkane to a stripping column (32) to obtain a purified stream (33) of the partially chlorinated alkane.

12. Device according to the preceding claim, characterized in that the stripping column (32) has a bottom outlet through which the purified stream (33) of the partially chlorinated alkane can be discharged, preferably via a stripping column sump pump (34).

13. Device according to one of the two preceding claims, characterized in that the stripping column (32) has a feed (36) for an inert gas and / or a circulating evaporator (35), wherein a partial stream of the purified stream (33) of the partially chlorinated alkane is returned to the stripping column (32) and heated by means of the circulating evaporator (35).

14. Device according to one of claims 11 to 13, characterized in that the stripping column (32) has a top outlet through which gaseous products can be discharged from the stripping column (32), the outlet opening into a condenser (38).

15. Device according to the preceding claim, characterized in that the product condenser (27) has an outlet for gaseous products which is led into the condenser (38).

16. Device according to one of the two preceding claims, characterized in that the condenser (38) has an outlet for condensed products which is led into a stripper head condensate reservoir (42).

17. Device according to one of claims 14 to 16, characterized in that the condenser (38) and / or the stripper head condensate reservoir (42) each have an outlet for gaseous products which is led into a deep freezer (39).

18. Device according to the preceding claim, characterized in that the freezer (39) has a return for condensed products into the stripper head condensate reservoir (42) and a discharge option for non-condensable products (44).

19. Device according to one of claims 16 to 18, characterized in that the stripper head condensate reservoir (42) has a bottom outlet through which a liquid product stream can be returned to the loop reactor, preferably by means of a stripper head condensate pump (43).

20. Device according to the preceding claim, characterized in that the recirculated product stream opens into the fall zone (6) of the loop reactor (1), wherein the opening is preferably arranged above the first discharge (7).

21. Device according to one of claims 11 to 20, characterized in that the second partial stream (10) is supplied to the product condenser (27) via a high-boiling column (12), wherein a pressure regulating valve (11) is preferably arranged upstream of the high-boiling column (12).

22. Device according to the preceding claim, characterized in that the high-boiling column (12) has a top-side outlet for a top stream (26) through which gaseous components can be discharged from the device.

23. Device according to the preceding claim, characterized in that the product condenser (27) for condensing the partially chlorinated alkane is connected downstream of the top-side outlet for a top-side stream (26), wherein a return vessel (28) for collecting the condensed partially chlorinated alkane is preferably connected downstream of the product condenser (27).

24. Device according to the preceding claim, characterized in that the return vessel (28) has a bottom outlet through which the condensed semi-chlorinated alkane can be withdrawn from the return vessel and divided into a first partial stream (30) of the condensed semi-chlorinated alkane and a second partial stream (31) of the condensed semi-chlorinated alkane, wherein the first partial stream (30) of the condensed semi-chlorinated alkane is recycled to the high-boiling column (12) and the second partial stream (31) of the condensed semi-chlorinated alkane is fed to a stripping column (32), wherein a return pump (29) is preferably provided for conveying the condensed semi-chlorinated alkane withdrawn from the return vessel (28).

25. Device according to one of the preceding claims, characterized in that the loop reactor (1) has a second head-side arranged discharge (19) for gaseous partially chlorinated alkane.

26. Device according to the preceding claim, characterized in that the gaseous partially chlorinated alkane discharged via the second head-side discharge (19) is supplied to a heat exchanger (20) for condensation and is supplied as condensed partially chlorinated alkane to a storage container (22) via a feeder (21).

27. Device according to the preceding claim, characterized in that the storage container (22) and / or the feed (21) of the condensed semichlorinated alkane into the storage container (22) has an addition device (41) for inert gas.

28. Device according to one of the two preceding claims, characterized in that the feed tank (22) has a bottom feed tank outlet through which the condensed partially chlorinated alkane is preferably returned to the loop reactor (1) via a feed tank condensate pump.

29. Device according to one of claims 26 to 28, characterized in that the storage container (22) has a top-side storage container outlet for discharging an exhaust gas flow (40), wherein the exhaust gas flow (40) is preferably directed directly into the condenser (38).

Images