EP2675751A1 - Utilisation de chlorure d'hydrogène liquide comme agent réfrigérant dans un procédé de production du chlore - Google Patents

Utilisation de chlorure d'hydrogène liquide comme agent réfrigérant dans un procédé de production du chlore

Info

Publication number
EP2675751A1
EP2675751A1 EP12703847.9A EP12703847A EP2675751A1 EP 2675751 A1 EP2675751 A1 EP 2675751A1 EP 12703847 A EP12703847 A EP 12703847A EP 2675751 A1 EP2675751 A1 EP 2675751A1
Authority
EP
European Patent Office
Prior art keywords
hydrogen chloride
stream
chlorine
oxygen
flow
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP12703847.9A
Other languages
German (de)
English (en)
Inventor
Hans-Jürgen PALLASCH
Heiner Schelling
Peter Van Den Abeel
Till EINIG
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BASF SE
Original Assignee
BASF SE
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by BASF SE filed Critical BASF SE
Priority to EP12703847.9A priority Critical patent/EP2675751A1/fr
Publication of EP2675751A1 publication Critical patent/EP2675751A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00—Halogens; Halogen acids
    • C01B7/01—Chlorine; Hydrogen chloride
    • C01B7/03—Preparation from chlorides
    • C01B7/04—Preparation of chlorine from hydrogen chloride
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00—Halogens; Halogen acids
    • C01B7/01—Chlorine; Hydrogen chloride
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00—Halogens; Halogen acids
    • C01B7/01—Chlorine; Hydrogen chloride
    • C01B7/07—Purification ; Separation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00—Halogens; Halogen acids
    • C01B7/01—Chlorine; Hydrogen chloride
    • C01B7/07—Purification ; Separation
    • C01B7/0706—Purification ; Separation of hydrogen chloride
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00—Halogens; Halogen acids
    • C01B7/01—Chlorine; Hydrogen chloride
    • C01B7/07—Purification ; Separation
    • C01B7/0706—Purification ; Separation of hydrogen chloride
    • C01B7/0712—Purification ; Separation of hydrogen chloride by distillation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00—Halogens; Halogen acids
    • C01B7/01—Chlorine; Hydrogen chloride
    • C01B7/07—Purification ; Separation
    • C01B7/0743—Purification ; Separation of gaseous or dissolved chlorine

Definitions

  • the invention relates to a process for the production of chlorine from hydrogen chloride, in which liquid hydrogen chloride is used as the refrigerant, and to the use of liquid hydrogen chloride as a refrigerant in processes for producing chlorine.
  • the product gas mixture is cooled down to the extent that the reaction water and hydrogen chloride in the form of concentrated hydrochloric acid condense out.
  • the hydrochloric acid formed is separated and the remaining gas mixture freed by washing with concentrated sulfuric acid or by drying with zeolites of residual water.
  • the now anhydrous gas mixture is then compressed and cooled so that chlorine condenses out, but oxygen and other low-boiling gas components remain in the gas phase.
  • the liquefied chlorine is separated off and optionally further purified.
  • EP-A 0 765 838 discloses a process for working up the reaction gas formed from hydrogen chloride, hydrogen chloride, oxygen and water vapor in the oxidation of hydrogen chloride, in which the reaction gas leaving the oxidation reactor is so is cooled far, that water of reaction and hydrogen chloride condense in the form of concentrated hydrochloric acid, the concentrated hydrochloric acid is separated from the reaction gas and discharged, the remaining, essentially freed of water and a part of the hydrogen chloride reaction gas is dried, the dried reaction gas of chlorine , Oxygen and hydrogen chloride compressed to 1 to 30 bar and the compressed reaction gas is cooled and thereby largely liquefied, wherein not auskondensierbare components of the reaction gas are at least partially recycled to the oxidation reactor.
  • the dried and compressed reaction gas mixture is liquefied in a so-called chlorine recuperator designed as an expansion cooler, except for a residual proportion of about 10 to 20%.
  • the separated in the chlorine recuperator liquid main stream of chlorine is then cleaned in a distillation column, in which the chlorine is freed of residual dissolved hydrogen chloride, oxygen and inert gases.
  • the withdrawn at the top of the distillation column, consisting essentially of hydrogen chloride, chlorine, oxygen and inert gases gas is returned to the compression stage.
  • the non-condensed at the chlorine recuperator gas components including the residual chlorine content are partially liquefied in a post-cooling stage at a significantly lower temperature.
  • the remaining waste gas from unreacted hydrogen chloride, oxygen and inert gases is recycled to the oxidation reactor.
  • WO 2007/134716 and WO 2007/085476 describe the advantageous effect of the presence of HCl in the chlorine separation.
  • the condensation stage for water and HCl is operated so that a beneficial amount of hydrogen chloride with the process gas passes through the drying stage in the compressor and the subsequent chlorine separation.
  • part of the gaseous hydrogen chloride is taken from the feed stream to the process and fed directly into the chlorine separation, bypassing the other process stages.
  • a process for the production of chlorine from hydrogen chloride is described in WO 2007/085476.
  • the process comprises the steps of: a) feeding a hydrogen chloride-containing stream a1 and an oxygen-containing stream a2 into an oxidation zone and catalytic oxidation of hydrogen chloride to chlorine, whereby a product gas stream a3 containing chlorine, water, oxygen, carbon dioxide and inert gases is obtained; b) contacting the product gas stream a3 in a phase contact apparatus with aqueous hydrochloric acid I and partially separating water and hydrogen chloride from the stream a3, wherein a gas stream b containing hydrogen chloride, chlorine, water, oxygen, carbon dioxide and optionally inert gases remains, wherein at least 5 % of the hydrogen chloride contained in the stream a3 remains in the gas stream b; c) drying the gas stream b, leaving a substantially anhydrous gas stream c containing hydrogen chloride, chlorine, oxygen, carbon dioxide and optionally inert gases; d) partial liquefaction
  • step d) the dried gas stream c, which consists essentially of chlorine and oxygen and also contains hydrogen chloride and inert gases (carbon dioxide, nitrogen), is compressed in multiple stages to about 10 to 40 bar.
  • the compressed gas is cooled to temperatures of about -10 to -40 ° C.
  • the compressed and partially liquefied, two-phase mixture is finally separated in a mass transfer apparatus.
  • the non-liquefied gas stream in this case in countercurrent or in co-current with the liquid, which consists essentially of chlorine and dissolved carbon dioxide, hydrogen chloride and oxygen, brought into contact.
  • the non-liquefied gases accumulate in the liquid chlorine until the thermodynamic equilibrium is reached, so that a separation of inert gases, in particular of carbon dioxide, via the exhaust gas of the subsequent chlorine distillation can be achieved.
  • the liquefied chlorine which generally has a chlorine content of> 85 wt .-%, is subjected to a distillation at about 10 to 40 bar.
  • the bottom temperature is about 30 to 1 10 ° C, the head temperature depending on the hydrogen chloride content in the liquefied chlorine between about -5 to -8 ° C and about -25 to -30 ° C.
  • Hydrogen chloride is condensed at the top of the column and allowed to run back into the column.
  • the HCI reflux achieves almost complete chlorine separation, minimizing chlorine loss.
  • the chlorine taken off at the bottom of the column has a purity of> 99.5% by weight.
  • refrigerators are usually used. Suitable as a refrigerant are fully halogenated hydrocarbons, as described for example in US 5,490,390. Fully halogenated hydrocarbons are very inert.
  • the partially halogenated hydrocarbons used as replacement refrigerants are more reactive and therefore harbor the danger of undesired chemical reactions in the case of leaks in chlorine plants.
  • Ammonia is also a refrigerant suitable for chillers.
  • the direct use of ammonia for the chlorine condensation prohibits, since in the case of leaks to NCI 3 formation can occur, which can decompose explosively even in low concentrations.
  • One option for preventing the direct contact of chlorine and refrigerant in the event of leakage is the use of double-tube and gap-space safety heat exchangers.
  • Another possibility is the provision of an intermediate, closed, secondary refrigerant circuit operated with an inert refrigerant, as described in US 5,490,390.
  • chlorine as the substance to be cooled C0 2 is suitable as an inert refrigerant.
  • the object of the invention is to provide an improved process for the production of chlorine from hydrogen chloride, which is economically and safety advantageous.
  • the object of the invention is also to provide an alternative refrigerant for the separation of chlorine by condensation from the process gas streams chlorine-producing plants. The problem is solved by a process for the production of chlorine from hydrogen chloride with the steps:
  • step e Separating the liquid stream f2 by distillation in a column into a chlorine stream gl and a stream g2 consisting essentially of hydrogen chloride, oxygen and carbon dioxide, the cooling and partial liquefaction of the gas stream d occurring in step e) by indirect heat exchange with the liquid hydrogen chloride stream a, wherein at least a portion of the liquid hydrogen chloride stream a evaporates and this portion forms a gaseous hydrogen chloride stream a '.
  • the hydrogen chloride stream a and the gas stream d do not come into direct contact with each other, which would lead to a mixing of the streams.
  • the heat exchange takes place rather in a heat exchanger. This can be constructed as desired. Suitable heat exchangers are, for example Shell-and-tube heat exchangers, U-tube heat exchangers, spiral or plate heat exchangers.
  • HCl is particularly well suited as chlorine-inert material refrigerant for chlorine-producing plants.
  • HCl can be condensed relatively easily by condensation at 10 to 25 bar with a conventional refrigeration system at condensation temperatures of -10 to -40 ° C.
  • the use of such liquefied hydrogen chloride provides the "cold" required for the condensation of chlorine in the low-temperature range (temperature ⁇ 20 ° C) in a simple manner by evaporation.
  • the vaporized HCl does not have to be completely immersed in the HCI oxidation plant Run, so cooled again, optionally compressed and condensed, but can be discharged as a gaseous feedstock in the HCI oxidation system.
  • HCl as a resource is that HCl and chlorine do not undergo chemical reactions in the event of possible leakage in the heat exchanger.
  • Another advantage is that low temperatures can be achieved according to the vapor pressure curve of HCl during evaporation of the HCl.
  • evaporation temperatures of the HCl of -32, -42 ° C and -51 ° C respectively.
  • chlorine can be produced at low pressure or in the presence of gases, e.g. Nitrogen, carbon dioxide, oxygen, argon and hydrogen condense completely.
  • the chlorine partial pressures in the gas phase which can be reached with the above-mentioned temperatures of -32, -42 ° C and -51 ° C, are 1, 1 1, 0.71 resp 0.45 bar.
  • the pressure at which the liquid hydrogen chloride stream a is 1 to 30 bar, preferably 5 to 15 bar, and is correspondingly the temperature of the liquid hydrogen chloride stream -80 to -10 ° C, preferably -50 to -20 ° C.
  • the chlorine partial pressures which can be achieved with these low temperatures are advantageous in particular in the oxidation of hydrogen chloride with oxygen in the Deacon process, since condensation takes place there in the presence of process and inert gases and at the same time the most complete separation of the chlorine from the remaining gases is desired is.
  • most of the remaining, uncondensed gas stream is recycled to the hydrogen chloride oxidation, remaining in the gas flow, non-separated chlorine in the HCI oxidation reactor would reduce the possible HCI conversion.
  • part of the uncondensed gas stream is discharged from the process in order to limit the accumulation of inert gases, in particular of nitrogen and carbon dioxide. In the discharge stream (Purge gas stream) contained chlorine but increases the cost of post-treatment of the discharge stream.
  • the associated chlorine losses also reduce the chlorine yield of the process.
  • the liquid hydrogen chloride stream can be easily prepared by condensation at 10 to 25 bar with a conventional refrigeration system at condensation temperatures of -10 to -40 ° C. This advantageously takes place in combination with, for example, an isocyanate or polycarbonate system, since the low inert gas content of less than 10% by volume of the hydrogen chloride as by-product obtained in these systems enables a simple condensation of the hydrogen chloride.
  • Particularly advantageous is the composite with a distillative purification of hydrogen chloride, since hydrogen chloride is already obtained with higher purity in the vicinity of the dew point.
  • the by-produced HCl in the polycarbonate or isocyanate plant is compressed in a process step of the process, purified, e.g. Purified by distillation and condensed.
  • the liquefied HCl is used after relaxation for cooling in the chlorine separation of the HCl oxidation and thereby evaporated.
  • the gaseous HCI stream is divided according to the operational requirements into a feed gas stream for HCI oxidation and a recycle stream, which is recycled to the polycarbonate or isocyanate plant and liquefied there again.
  • hydrogen chloride is used in the process according to the invention, which is obtained in a process as effluent, in which hydrogen chloride is formed as coproduct.
  • Such methods are for example
  • the vaporized HCI stream does not have to be completely circulated, ie completely recompressed and condensed, but can be fed into the HCI oxidation as a gaseous feedstock.
  • evaporated HCl can be completely and partially recompressed and condensed.
  • the HCI gas stream can be recycled to the HCI compression stage or HCI purification stage of a polycarbonate or isocyanate unit.
  • the hydrogen chloride used as the refrigerant has a purity of> 95% by volume, preferably of> 99% by volume.
  • carbon dioxide and traces of carbon monoxide or nitrogen may be included.
  • the liquid hydrogen chloride stream a is produced in a process for producing polycarbonates. In a further embodiment of the method according to the invention, the liquid hydrogen chloride stream a is produced in a process for the preparation of isocyanates.
  • WO04 / 056758 describes a process for the partial or complete separation of a mixture consisting of hydrogen chloride and phosgene, optionally solvents, low boilers and inert gases, as is customary in the preparation of isocyanates by reaction of amines with phosgene accrues.
  • phosgene is obtained as the bottom product in a distillation column.
  • a suitable solvent preferably the solvent of the isocyanate synthesis
  • At least part of the gaseous hydrogen chloride stream a ' is fed as the hydrogen chloride-containing stream b1 into the oxidation zone in step b). This part is generally 10 to 90% of the hydrogen chloride stream a. In a further embodiment of the invention, at least part of the gaseous hydrogen chloride stream a 'is liquefied again and used again as a coolant stream. This part is generally 10 to 90% of the hydrogen chloride stream a.
  • a hydrogen chloride-containing stream b1 is fed with an oxygen-containing stream b2 into an oxidation zone and catalytically oxidized.
  • At least part of the hydrogen chloride b1 fed into step b) can originate from the refrigerant stream a vaporized in the chlorine separation step e).
  • hydrogen chloride is oxidized with oxygen in an exothermic equilibrium reaction to chlorine to produce water vapor.
  • Typical reaction temperatures are between 150 and 500 ° C, usual reaction pressures are between 1 and 25 bar.
  • oxygen is expedient to use oxygen in superstoichiometric amounts. For example, a two- to four-fold excess of oxygen is customary.
  • Suitable catalysts include, for example, ruthenium oxide, ruthenium chloride or other ruthenium compounds on silica, alumina, titania or zirconia as a carrier. Suitable catalysts can be obtained, for example, by applying ruthenium chloride to the support and then drying or drying and calcining. Suitable catalysts may, in addition to or instead of a ruthenium compound, also contain compounds of other noble metals, for example gold, palladium, platinum, osmium, iridium, silver, copper or rhenium. Suitable catalysts may further contain chromium (III) oxide.
  • the catalytic hydrogen chloride oxidation may be carried out adiabatically or preferably isothermally or approximately isothermally, batchwise, preferably continuously, as flow or fixed bed processes. Preferably, it is carried out in a Wrbel Anlagenktor at a temperature of 320 to 450 ° C and a pressure of 2 to 10 bar.
  • Ruthenium compounds or copper compounds on support materials are particularly suitable as heterogeneous catalysts, preference being given to optionally doped ruthenium catalysts.
  • Suitable support materials are, for example, silicon dioxide, graphite, rutile or anatase titanium dioxide, zirconium dioxide, aluminum oxide or mixtures thereof, preferably titanium dioxide, zirconium dioxide, aluminum oxide or mixtures thereof, particularly preferably gamma or alpha alumina or mixtures thereof.
  • the supported copper or ruthenium catalysts can be obtained, for example, by impregnating the support material with aqueous solutions of CuCl 2 or RuCl 3 and optionally a promoter for doping, preferably in the form of their chlorides.
  • the shaping of the catalyst can take place after or preferably before the impregnation of the carrier material.
  • alkali metals such as lithium, sodium, potassium, rubidium and cesium, preferably lithium, sodium and potassium, more preferably potassium, alkaline earth metals such as magnesium, calcium, strontium and barium, preferably magnesium and calcium, more preferably magnesium, rare earth metals such Scandium, yttrium, lanthanum, cerium, praseodymium and neodymium, preferably scandium, yttrium, lanthanum and cerium, more preferably lanthanum and cerium, or mixtures thereof.
  • Preferred promoters are calcium, silver and nickel. Particularly preferred is the combination of ruthenium with silver and calcium and ruthenium with nickel as a promoter.
  • the volume ratio of hydrogen chloride to oxygen at the reactor inlet is generally between 1: 1 and 20: 1, preferably between 2: 1 and 8: 1, more preferably between 2: 1 and 5: 1.
  • a step c) the product gas stream b3 is brought into contact with aqueous hydrochloric acid I in a phase contact apparatus and water and hydrogen chloride partially separated from the stream b3, leaving a gas stream b containing hydrogen chloride, chlorine, water, oxygen, carbon dioxide and optionally inert gases.
  • the product gas stream b3 is cooled, and water and hydrogen chloride are at least partially separated from the product gas stream b3 as aqueous hydrochloric acid.
  • the hot product gas stream b3 is cooled by contacting it with dilute hydrochloric acid I as quenching agent in a suitable phase contactor, for example a packed or tray column, a jet scrubber or a spray tower, absorbing a portion of the hydrogen chloride in the quench.
  • a suitable phase contactor for example a packed or tray column, a jet scrubber or a spray tower, absorbing a portion of the hydrogen chloride in the quench.
  • Quenching and absorbing agent is hydrochloric acid, which is not saturated with hydrogen chloride.
  • the phase contact apparatus is operated with circulating hydrochloric acid I.
  • at least a portion of the aqueous hydrochloric acid circulating in the phase contact apparatus for example 1 to 20%, is removed from the phase contact apparatus and subsequently distilled, gaseous hydrogen chloride and an aqueous hydrochloric acid II depleted in hydrogen chloride being produced. NEN, and wherein the hydrogen chloride in step b) recycled and at least a portion of the aqueous hydrochloric acid II is recycled to the Phasentakingatat.
  • the gas stream c leaving the phase contact apparatus contains chlorine, hydrogen chloride, water, oxygen, carbon dioxide and in general also inert gases. This can be freed in a subsequent drying step d) by bringing into contact with suitable drying agents of traces of moisture. Suitable drying agents are, for example, concentrated sulfuric acid, molecular sieves or hygroscopic adsorbents. There is obtained a substantially anhydrous gas stream d containing chlorine, oxygen, carbon dioxide and optionally inert gases.
  • the dried gas stream d is cooled and optionally compressed, whereby a cooled and optionally compressed stream e is obtained.
  • the dried gas stream d which was previously optionally compressed and precooled, is cooled by cooling with a liquid hydrogen chloride stream in one or more heat exchangers.
  • the cooled stream e generally has a pressure in the range of 2 to 35 bar, preferably 3 to 10 bar, and a temperature in the range of -80 to -10 ° C, preferably -50 to -20 ° C.
  • the dried gas stream d is generally cooled in several stages and compacted.
  • the dried and optionally compressed gas stream d can be first cooled with cooling water or cold water to a temperature of about 40 to 5 ° C. Subsequently, the optionally compressed and precooled gas stream d can be cooled in one or more heat exchangers with liquid hydrogen chloride as the refrigerant to the final temperature of generally -80 to -10 ° C, preferably -50 to -20 ° C. Between the cold water cooling and the cooling with liquid hydrogen chloride, the compressed gas stream d can be precooled with the non-liquefied gas stream f1.
  • the stream e is separated into a gas stream f1 containing chlorine, oxygen, carbon dioxide and optionally inert gases and into a liquid stream f2 containing chlorine, hydrogen chloride, oxygen and carbon dioxide.
  • the liquid stream f2 is separated by distillation in a column into a chlorine stream g1 and a stream g2 consisting essentially of hydrogen chloride, oxygen and carbon dioxide.
  • a portion of the hydrogen chloride is condensed at the top of the column and allowed to run back as a reflux in the column, whereby a stream g2 is obtained with a chlorine content ⁇ 1 wt .-%.
  • a partial stream separated from the stream f1 as a purge gas stream is brought into contact with a solution containing sodium hydrogencarbonate and sodium hydrogen sulfite having a pH of from 7 to 9, chlorine and hydrogen chloride being removed from the gas stream.
  • the invention also relates to the use of liquid hydrogen chloride as refrigerant for cooling and optionally liquefaction of chlorine by indirect heat exchange in chlorine-producing process.
  • Chlorine-producing processes are, for example, the heterogeneous catalytic hydrogen chloride oxidation with oxygen or the electrochemical hydrogen chloride oxidation (hydrogen chloride electrolysis).
  • the liquid hydrogen chloride can be used as a refrigerant in a secondary cooling circuit and heat is delivered via a heat exchanger to a primary cooling circuit, wherein the primary cooling circuit is cooled by a chiller, that is its heat to the refrigerator and thus ultimately to the environment.
  • Conventional refrigerants such as partially halogenated hydrocarbons can be used as the refrigerant of the primary cooling circuit.
  • FIGS. 1 a, b and c show by way of example schematic arrangements comprising a primary cooling circuit and a secondary cooling circuit operated with hydrogen chloride as the coolant.
  • a conventional refrigerant e.g.
  • a refrigerated refrigerator operated by a partially halogenated hydrocarbon comprises the apparatuses: refrigerant compressor V1, refrigerant condenser, e.g. water-cooled, W1, expansion valve and the heat exchanger W2 common to the secondary cooling circuit.
  • the secondary cooling circuit comprises the heat exchangers W2 and W3, wherein the heat absorbed by the process in the heat exchanger W3 is released via the heat exchanger W2 to the refrigerant of the refrigerator.
  • the current denoted by 1 is the process flow generated during chlorine production, which is to be cooled and optionally condensed, the stream denoted by 2 the cooled or condensed liquid process stream.
  • Figures 1 a, b and c differ in the manner in which the secondary cooling circuit is operated.
  • FIG. 1 a HCl is vaporized in heat exchanger W3 and condensed again in heat exchanger W2.
  • the transport of the gas or liquid is purely convective or hydraulic.
  • FIG. 1 b as in FIG. 1 a, HCl evaporates in the heat exchanger W 3 and condenses again in the heat exchanger W 2. Due to pressure differences between the heat exchangers W2 and W3, gaseous HCl must be compressed on the way from W3 to W2 from the compressor V2. The pressure maintenance in the W2 is carried out by the pressure-holding valve, is relaxed over the condensed liquid HCl on the way to the heat exchanger W3.
  • the secondary cooling circuit in FIG. 1c is operated without phase transition with completely liquefied HCl.
  • Liquid HCl is heated in the heat exchanger W3 only so far that the boiling temperature is not reached.
  • the cooling of the liquid then takes place in W2.
  • the transport of the liquid HCl in the secondary cooling circuit is effected by the pump PL

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Catalysts (AREA)

Abstract

L'invention concerne un procédé de production du chlore à partir de chlorure d'hydrogène, comprenant les étapes suivantes : a) préparation d'un flux de chlorure d'hydrogène liquide (a) en tant que flux d'agent réfrigérant; b) introduction d'au moins un flux renfermant du chlorure d'hydrogène (b1) et d'un flux renfermant de l'oxygène (b2) dans une zone d'oxydation du chlorure d'hydrogène, et oxydation catalytique du chlorure d'hydrogène en chlore, ce qui permet d'obtenir un flux de produit gazeux (b3) renfermant du chlore, de l'eau, de l'oxygène, du dioxyde de carbone et des gaz inertes; c) mise en contact du flux de produit gazeux (b3), dans un appareil de mise en contact de phases, avec de l'acide chlorhydrique aqueux (I), et séparation partielle de l'eau et du chlorure d'hydrogène contenus dans le flux (b3), ce qui fournit un flux gazeux restant (c) renfermant du chlorure d'hydrogène, du chlore, de l'eau, de l'oxygène, du dioxyde de carbone, et éventuellement des gaz inertes; d) déshydratation du flux gazeux (c), ce qui fournit un flux gazeux restant (d), sensiblement anhydre, renfermant du chlorure d'hydrogène, du chlore, de l'oxygène, du dioxyde de carbone, et éventuellement des gaz inertes; e) liquéfaction partielle du flux gazeux (d) par compression et refroidissement, ce qui permet d'obtenir un flux au moins partiellement liquéfié (e); f) séparation gaz/liquide du flux (e) en un flux gazeux (f1) renfermant du chlore, de l'oxygène, du dioxyde de carbone, du chlorure d'hydrogène, et éventuellement des gaz inertes, et en un flux liquide (f2) renfermant du chlorure d'hydrogène, du chlore, de l'oxygène et du dioxyde de carbone, et éventuellement recyclage d'au moins une partie du flux gazeux (f1) à l'étape b); g) séparation du flux liquide (f2) par distillation dans une colonne, en un flux de chlore (g1) et en un flux (g2), essentiellement constitué de chlorure d'hydrogène, d'oxygène et de dioxyde de carbone; le refroidissement et la liquéfaction partielle du flux gazeux (d) à l'étape (e) s'effectuant par échange de chaleur indirect avec le flux de chlorure d'hydrogène liquide (a), au moins une partie du flux de chlorure d'hydrogène liquide (a) étant évaporée, et cette partie étant obtenue sous forme de flux gazeux de chlorure d'hydrogène (a').
EP12703847.9A 2011-02-18 2012-02-16 Utilisation de chlorure d'hydrogène liquide comme agent réfrigérant dans un procédé de production du chlore Withdrawn EP2675751A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP12703847.9A EP2675751A1 (fr) 2011-02-18 2012-02-16 Utilisation de chlorure d'hydrogène liquide comme agent réfrigérant dans un procédé de production du chlore

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP11155048 2011-02-18
EP12703847.9A EP2675751A1 (fr) 2011-02-18 2012-02-16 Utilisation de chlorure d'hydrogène liquide comme agent réfrigérant dans un procédé de production du chlore
PCT/EP2012/052684 WO2012110597A1 (fr) 2011-02-18 2012-02-16 Utilisation de chlorure d'hydrogène liquide comme agent réfrigérant dans un procédé de production du chlore

Publications (1)

Publication Number Publication Date
EP2675751A1 true EP2675751A1 (fr) 2013-12-25

Family

ID=45592415

Family Applications (1)

Application Number Title Priority Date Filing Date
EP12703847.9A Withdrawn EP2675751A1 (fr) 2011-02-18 2012-02-16 Utilisation de chlorure d'hydrogène liquide comme agent réfrigérant dans un procédé de production du chlore

Country Status (6)

Country Link
EP (1) EP2675751A1 (fr)
JP (1) JP2014514228A (fr)
KR (1) KR20140007899A (fr)
CN (1) CN103476705A (fr)
BR (1) BR112013021065A2 (fr)
WO (1) WO2012110597A1 (fr)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3421426A1 (fr) 2017-06-29 2019-01-02 Covestro Deutschland AG Procédé à haute performance énergétique destiné à produire de la vapeur de phosgène
CN109453764A (zh) * 2018-11-16 2019-03-12 西安元创化工科技股份有限公司 用于氯化氢氧化制氯气的二氧化钌催化剂及其制备方法
CN109879251B (zh) * 2019-03-07 2024-05-03 南京工程学院 一种基于能量综合利用的氯化氢合成系统
EP4326672A1 (fr) * 2021-04-21 2024-02-28 Basf Se Procédé de préparation de chlore
CN115583631A (zh) * 2022-10-13 2023-01-10 鹤壁德瑞科技有限公司 一种三氟化氯的制备方法及装置

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL129282C (fr) * 1963-10-21
GB1139523A (en) * 1966-02-10 1969-01-08 Pullman Inc Recovery of halogens from gaseous mixtures
US5490390A (en) 1994-05-13 1996-02-13 Ppg Industries, Inc. Liquefaction of chlorine or other substances
DE19535716A1 (de) 1995-09-26 1997-03-27 Bayer Ag Verfahren zur Aufarbeitung der Reaktionsgase bei der Oxidation von HCI zu Chlor
DE10260084A1 (de) 2002-12-19 2004-07-01 Basf Ag Auftrennung eines Stoffgemisches aus Clorwasserstoff und Phosgen
DE102005008612A1 (de) * 2005-02-23 2006-08-24 Basf Ag Verfahren zur Herstellung von Chlor
DE502007001903D1 (de) 2006-01-27 2009-12-17 Basf Se Verfahren zur herstellung von chlor
DE102006023581A1 (de) 2006-05-19 2007-11-22 Bayer Materialscience Ag Verfahren zur Abtrennung von Chlor aus dem Produktgas eines HCI-Oxidationsprozesses

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2012110597A1 *

Also Published As

Publication number Publication date
BR112013021065A2 (pt) 2019-09-24
JP2014514228A (ja) 2014-06-19
KR20140007899A (ko) 2014-01-20
CN103476705A (zh) 2013-12-25
WO2012110597A1 (fr) 2012-08-23

Similar Documents

Publication Publication Date Title
EP1981806B1 (fr) Procédé de production de chlore
EP1981619B1 (fr) Procédé pour obtenir du chlorure d'hydrogène exempt d'hydrocarbures (chlorés) et des hydrocarbures (chlorés) exempts de phosgène à partir d'un flux de chlorure d'hydrogène contenant des hydrocarbures (chlorés) et du phosgène
EP1529033B1 (fr) Procede integre de production d'isocyanates
EP1866239B1 (fr) Procede pour produire du chlore
EP2024279B1 (fr) Procédé de séparation du chlore contenu dans le gaz produit au cours d'un processus d'oxydation de chlorure d'hydrogène
EP1542923B1 (fr) Procede a lit fixe pour produire du chlore par oxydation catalytique en phase gazeuse de chlorure d'hydrogene
EP0765838A1 (fr) Procédé de traitement des gaz réactionnels lors de l'oxydation de HCl en chlore
EP2675751A1 (fr) Utilisation de chlorure d'hydrogène liquide comme agent réfrigérant dans un procédé de production du chlore
WO2008125236A2 (fr) Intégration thermique dans un procédé deacon
EP2177476B1 (fr) Procédé de séparation d'oxyde de carbone à partir d'un gaz brut HCl
EP2139808A2 (fr) Procédé destiné à extraire des composants condensables de flux gazeux contenant du chlore et à les réintroduire dans ces flux gazeux
EP2027064A1 (fr) Procédé de production de chlore à partir de gaz chlorhydrique et d'oxygène
EP2029477A1 (fr) Procédé d'oxydation de chlorure d'hydrogène avec de l'oxygène
EP1656322A1 (fr) Procede de production de chlore
DE10252859A1 (de) Verfahren zur Herstellung von 1,2-Dichlorethan und von Vinylchlorid
EP2675752A1 (fr) Procédé de distillation pour séparer le chlore présent dans des flux gazeux contenant de l'oxygène et du chlore
WO2007134720A1 (fr) Procédé de fabrication de chlore à partir de chlorure d'hydrogène et d'oxygène
US20120213693A1 (en) Use of liquid hydrogen chloride as refrigerant in processes for preparing chlorine
DE10234908B4 (de) Verfahren zur Herstellung von Chlor aus einem (Chlor)kohlenwasserstoffe enthaltenden Chlorwasserstoffstrom
US20120213692A1 (en) Distillation process for separating chlorine from gas streams comprising oxygen and chlorine
DE102011005897A1 (de) Verfahren zur Bereitstellung von Chlor für chemische Umsetzungen

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20130918

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

DAX Request for extension of the european patent (deleted)
17Q First examination report despatched

Effective date: 20170103

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN

18D Application deemed to be withdrawn

Effective date: 20170516