Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
  • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
  • B01J8/0278—Feeding reactive fluids
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
  • B01J8/005—Separating solid material from the gas/liquid stream
  • B01J8/006—Separating solid material from the gas/liquid stream by filtration
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
  • B01J8/005—Separating solid material from the gas/liquid stream
  • B01J8/007—Separating solid material from the gas/liquid stream by sedimentation
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
  • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
  • B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
  • B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
  • B01J8/222—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid in the presence of a rotating device only
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
  • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
  • B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
  • B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
  • B01J8/224—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid the particles being subject to a circulatory movement
  • B01J8/228—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid the particles being subject to a circulatory movement externally, i.e. the particles leaving the vessel and subsequently re-entering it
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
  • B01J2208/00008—Controlling the process
  • B01J2208/00017—Controlling the temperature
  • B01J2208/00106—Controlling the temperature by indirect heat exchange
  • B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
  • B01J2208/00176—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles outside the reactor
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
  • B01J2208/00008—Controlling the process
  • B01J2208/00017—Controlling the temperature
  • B01J2208/00106—Controlling the temperature by indirect heat exchange
  • B01J2208/00265—Part of all of the reactants being heated or cooled outside the reactor while recycling
  • B01J2208/00283—Part of all of the reactants being heated or cooled outside the reactor while recycling involving reactant liquids
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
  • B01J2208/00008—Controlling the process
  • B01J2208/00017—Controlling the temperature
  • B01J2208/00106—Controlling the temperature by indirect heat exchange
  • B01J2208/00265—Part of all of the reactants being heated or cooled outside the reactor while recycling
  • B01J2208/00292—Part of all of the reactants being heated or cooled outside the reactor while recycling involving reactant solids
  • B01J2208/003—Part of all of the reactants being heated or cooled outside the reactor while recycling involving reactant solids involving reactant slurries
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
  • B01J2208/00796—Details of the reactor or of the particulate material
  • B01J2208/00805—Details of the particulate material
  • B01J2208/00814—Details of the particulate material the particulate material being provides in prefilled containers
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
  • B01J2208/00796—Details of the reactor or of the particulate material
  • B01J2208/00893—Feeding means for the reactants
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
  • B01J2208/00796—Details of the reactor or of the particulate material
  • B01J2208/00893—Feeding means for the reactants
  • B01J2208/00902—Nozzle-type feeding elements

Definitions

• the invention relates to a process for the conversion of equilibrium limited reactions according to the preamble of claim 1 and a reaction apparatus for imple ⁇ wetting of equilibrium-limited reactions according to the preamble of patent claim 6.
• the object of the invention is to provide a process and a reaction plant for the implementation of equilibrium-limited reactions which, compared with the prior art, bring about a higher yield in the reaction process and require less technical effort.
• the object is achieved in a method for the implementation of equilibrium-limited reactions according to claim 1 and in a reaction apparatus for the implementation of equilibrium-limited reactions with the features of claim 6.
• a catalyst material in a reactor is arranged ⁇ , further, are introduced into the reactor starting materials, Example ⁇ , in gas form, whereby they react in particular on a catalyst surface to products , wherein the reaction proceeds until an equilibrium state is reached or approximated.
• a sorption agent is introduced into the reactor, which in particular selectively sorbs the products of the reaction and thus removes the immediate reaction equilibrium. In this way, another set of products can be made to handle that
• the invention is characterized in that the laden with products sorbent is collected in a collection zone in the reactor and that the catalyst material is arranged in the reactor so that it is separated from the collection zone. This allows a continuous feed and discharge of the sorbent and a continuous further reaction of the reactants to products on the catalyst surface, without that catalyst material Mix al and sorbent together and must be separated consuming.
• sorbent is understood to mean the term "adsorbent and absorption medium" , whereby adsorption refers to the enrichment of substances from gases or liquids on the surface of a solid, generally at the interface between two phases. Absorption is a phenomenon in which the substances penetrate into the interior of a solid body or a FLÜS ⁇ stechnik and are bound there physically or chemically.
• the sorbents used are to a large extent absorbents, although various adsorbents may also be expedient for the process according to the invention.
• the loaded with the products sorbent is led by Sam ⁇ melzone in a phase separator, where the products are separated from the sorbent. This is conveniently done by a pressure drop in the phase separator, the products escape from the sorbent.
• the sorbent is separated from the product recycled to the reactor, which causes egg ne recycling the sorbent and affects cost ⁇ low.
• the starting materials are introduced in gaseous form into the reactor and the reactions carried out in the gas phase and that the sorbent is the Katalysa ⁇ tormaterials contactlessly passed through the reactor with respect to.
• This is particularly useful for certain pairings of Katalysa ⁇ door material and sorbent material which could physika ⁇ cally or chemically react with each other.
• the sorbent is an ionic liquid, in particular [PBu4] [NTf2] [PBuMe3] [NTf2].
• the reactor reactor is configured in one embodiment of the invention in the form of a dead-end, in which the gas concentration in the reactor is measured continuously and at a depletion Eduktgaskomponente this component is ent ⁇ speaking dosed.
• Another component of the invention consists in a reaction apparatus for the implementation of equilibrium-limited reactions with the features of claim 6, wherein said reaction apparatus comprises a reactor and a reactant inlet device attached to the reactor. Furthermore, a catalyst material and a sorption agent for sorption of a product formed during the reaction are present in the reactor.
• the invention is characterized in that ei ⁇ ne sorbent collection zone is provided and a Vorrich ⁇ device for separating the catalyst material from the collection zone is arranged in the reactor.
• the Sorptionsstoffsammelzone and active separation of the catalyst material from the Sorptionsffensammelzone thus cause the Sorptionsmit ⁇ tel, can be separated from the reactor as previously described regarding the method according to the invention easily without that the catalyst must be laboriously removed from the sorbent.
• the collecting zone is located in a lower and in an upper region of the reactor and is separated by a separating ge ⁇ network of a reaction zone of the reactor. This causes the sorbent, in particular the sorbent loaded with the product, to pass through the sorbent
• the separation network acts like a filter.
• two reactor types for the implementation of the described method and the described reaction device have been found to be expedient, it is on the one hand to a so-called slurry reactor, wherein in the reactor is a carrier liquid in particular, for example, a heat transfer oil, in which both the Sorptionsmate ⁇ rial and the reactants and the catalyst material are are contributed and are mixed together.
• the Sorpti ⁇ onsmaterial is again separated from the support material by a discontinuation due to the density difference.
• it is a so-called fixed bed reactor in which no carrier liquid is present and the catalyst material is in the reactor.
• Insbesonde ⁇ re when using a fixed bed reactor it is expedient ⁇ SSIG that the sorbent is advantageously distributed. Since ⁇ at a contact with the catalyst material can be allowed or deliberately avoided.
• FIG. 2 shows a reaction apparatus with a slurry reactor in which the catalyst material is separated from the sorbent-collecting zone by a dividing network and
• Figure 3 shows a reaction apparatus with a fixed bed reactor and a separation network to the sorbent collection zone.
• reaction types two different reaction types are expedient for the reaction, one is a gas phase reactor or a fixed bed reactor, which is shown for example in FIG. 3 and called a liquid phase reactor or slurry reactor, which is shown in FIGS 2 is described.
• the reaction apparatus 1 shown in FIG. 1 has a reactor 2, which is designed in the form of a liquid-phase reactor or as a so-called slurry reactor 26.
• the reactor 2 comprises a Eduktzuschreibvoriques 16, via the educts 6 are introduced and a stirring device 34.
• a separator 18 for a catalyst material 4 In the reactor 2 is a separator 18 for a catalyst material 4, wherein the separating device is designed in the form ei ⁇ nes basket 19.
• a carrier liquid 28 is present in the reactor 2 in a reaction zone 24 in which a sorbent 10 is distributed in finely dispersed form in addition to the educts 6.
• the reactor 2 has a calming zone or collection zone 12 in which the sorbent 10 can be GESAM ⁇ melt and discharged.
• the reactor 2 in this case according to Figure 1 in the embodiment of a slurry reactor 26, with a liquid phase in the form of a carrier liquid 28, for example in the form of a heat carrier oil such as Witco fills be ⁇ .
• the catalyst material 4 for example in the form a catalyst powder or catalyst pellets is configured, located in the catalyst basket 19.
• the Maschenwei ⁇ te of the basket is small enough to retain the catalyst material 4 inside the basket 19th
• a stirring device 34 such as a Gaseintragsrlaborer, ensures a good mixing of the gaseous reactants 6 and the liquid phase, in particular the carrier liquid 28 in an upper portion of the reac ⁇ gate 2.
• the gaseous reactants are preferably supplied through a Gaseintragsrlocher herein as component the generally illustrated Eduktezubowvoriques 16 consists.
• the gaseous starting materials 6 and the carrier liquid 28 are in a well-mixed state.
• the catalyst basket 19 may be stationary or rotate therewith be brought ⁇ . The latter variant ensures further Verrin ⁇ delay the diffusion limitation in the interface of the catalyst material 4. However, it should be a good contact of reactants 6 and the catalyst material be possible.
• the addition of the Sorp ⁇ tion material 10 can be finely-divided, for example in the form of injection nozzles, as comparable through the spray nozzles 32 in figure 3 is light. Furthermore, the fine distribution of the Sorp ⁇ tion material can also be generated via the stirrer.
• the FLÜS ⁇ SiGe sorbent material 10 is selected so that this egg ⁇ ne very good solubility for the reaction products has, but has only a limited solubility for the reactants to 6 ⁇ . Further, a difference in density between the Trä ⁇ ger wellkeit and the sorbent for better phase separation ⁇ appropriate. Further, the surface of the Kataly ⁇ sator materials should have tion means 10 a good wettability for the liquid sorption. This leads to the minimization of so ⁇ called film diffusion limitations.
• the figure 1 shows the case that the sorbent has a hö ⁇ here density than the carrier fluid 28, resulting in that settles at rest in the lower-reduced zone, the sorbent 10 in the reactor 2 and into a lower region 22 of the reactor 2 in a collection zone that is free or very low in turbulence.
• the sorbent 10 collected there is loaded with products 8 from the reaction taking place in the reaction zone 24.
• loaded Sorptionsmit ⁇ tel 10 can be selectively withdrawn from the reactor 2 through a valve 42. Outside the reactor 2, the solubility of the product in the sorbent 10 is reduced by a pressure reduction, which is why the product 8 can outgas from the sorption agent 10, which takes place in a phase separator 14.
• the products 8 are withdrawn in gaseous form from the phase separator 14, here in the form of a liquid separator, and the emptied sorbent 10 is conveyed back into the reactor 2 via a pump 40.
• a heat removal in the overall system is necessary, this can be done directly in the reactor 2, which can be done for example by a heat exchange device 36, wherein also in the circulation of the sorbent 10, as shown for example in Fi gur ⁇ 2, the heat dissipation in the form of a heat exchange device 36 can, which is arranged between the phase separator 14 and the pump 40.
• a thermoregulation is particularly necessary if it is an exothermic reaction, which requires a pressure and temperature control in the reactor 2.
• a heat dissipation between Phasenabschei ⁇ and pump 40 may be appropriate, since here the lowest system pressure prevails and the pump 40 is thermally less loaded.
• FIG. 2 shows a reaction device 1 which is similar in many parts to that of FIG. However, there is the difference that in the reactor 2, the catalyst Mate ⁇ material 4 is finely dispersed. Through a network 20, which constitutes the separation device 18, the catalyst material 4 is separated from the collection zone 12 of the sorbent 10.
• the heat exchanger devices 36 and 36 ⁇ arranged in different positions in FIGS. 1 and 2 are independent of the other differences in the reaction device 1 in FIGS. 1 and 2. The arrangements can be freely combined and are merely examples of advantageous attachments.
• the separating device 18 causes the sorbent 10 loaded with the product 8 to collect on the one hand in the collecting zone 12 and at the same time be separated from the catalyst material 4, with the result that that no complicated separation process between the catalyst material and the sorption material is necessary, which means a significant reduction in the design complexity of the entire reaction plant 1.
• the permeation of the sorbent 10, which is in liquid form, into the collecting zone, which is heterogeneous in the carrier liquid, is made possible.
• catalyst 28 present and finely dispersed catalyst remains behind.
• the pore or the mesh of the net 20 should thus be smaller than the size of Kataly ⁇ sator material present as a powder or as pellets.
• This design according to Figure 2 and also shown in FIG 3 allows a distribution of the catalyst material 4 in the upper Reakti ⁇ onsvolumen, ie in the reaction zone 24 of the reactor 2, thus allowing the reaction in the entire upper Yousvolu ⁇ men of the catalyst 2 and not only inside the basket 18, which is shown in FIG.
• fluid mechanics must ensure that the turbulences in the reactor 2 lead to the distribution of the catalyst material 4 without comminuting it.
• a Ausgestal ⁇ tung form according to FIG 2 therefore requires a higher mechanical strength and stress resistance of the see Katalysatormateri ⁇ as.
• the height of the fixed bed 44 is dimensioned so that the ascending starting materials are reacted 6 along the fixed bed 44, wherein the Pro-products ⁇ 8 are taken continuously from the downward flowing sorbent 10th
• This construction leads to a generally high fixed bed 44 and a high demand for catalyst material 4.
• a small height of the fixed bed 44 may be useful when there is good internal circulation of gas.
• a good mixing is then ensured, so that the starting materials 6, which are located above the fixed bed 44, repeatedly passed through the catalyst ⁇ material 4.
• Typical by-products of this synthesis are water, dimethyl ether, methyl formate and ethanol.
• mainly copper-zinc oxide-alumina catalysts are used for the reaction.
• the described sorption material 10 should therefore satisfy the following requirements in particular: It should have a high absorption capacity for methanol and its by-products, above all for water. Furthermore, it should have a low absorption capacity of the educts, namely the carbon monoxide, the
• a high Stabili ⁇ ty under the reaction conditions notably the reaction temperature between 150 ° C and 300 ° C and a reaction ⁇ pressure between 1 bar and 300 bar should sen the means aufwei-.
• the so-called copper-zinc oxide-alumina catalyst material is suitable here.
• a low vapor pressure for the downstream product separation in the phase separator 14 is advantageous.
• a low miscibility with the heat transfer oil for obtaining defined phase boundaries in the settling phase when used in a slurry reactor is useful. This is usually ensured by a high polarity in the sorbent. Therefore, a highly polar sorbent 10 is useful.
• Ionic liquids have a good uptake capacity for polar substances, such as water and methanol, and very low vapor pressures, which allows separation of methanol and water by lowering the pressure.
• polar organic substances with high boiling points. Examples for this are:
• reaction apparatus described and the method described have the following advantages:
• a circulation of the sorbent 10 can remain permanently in operation. The reaction can be started quickly by supplying educts 6. The circulation can also be used to keep the system warm if the chemical reaction does not occur.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Engineering & Computer Science (AREA)
• Combustion & Propulsion (AREA)
• Physical Or Chemical Processes And Apparatus (AREA)
• Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
• Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
• Gas Separation By Absorption (AREA)

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• 2015
  • 2015-08-18 DE DE102015215662.1A patent/DE102015215662A1/de not_active Withdrawn
• 2016
  • 2016-07-07 CN CN201680048014.8A patent/CN107921395B/zh not_active Expired - Fee Related
  • 2016-07-07 US US15/752,673 patent/US10618021B2/en not_active Expired - Fee Related
  • 2016-07-07 WO PCT/EP2016/066117 patent/WO2017029024A1/de active Application Filing
  • 2016-07-07 MX MX2018002024A patent/MX2018002024A/es unknown
  • 2016-07-07 AU AU2016309524A patent/AU2016309524B2/en not_active Ceased
  • 2016-07-07 MA MA042252A patent/MA42252A/fr unknown
  • 2016-07-07 KR KR1020187007207A patent/KR102116731B1/ko active IP Right Grant
  • 2016-07-07 JP JP2018508633A patent/JP6661005B2/ja not_active Expired - Fee Related
  • 2016-07-07 EP EP16739436.0A patent/EP3313564A1/de not_active Withdrawn
  • 2016-07-07 TN TNP/2018/000053A patent/TN2018000053A1/en unknown
• 2018
  • 2018-02-09 CL CL2018000369A patent/CL2018000369A1/es unknown
  • 2018-02-12 SA SA518390908A patent/SA518390908B1/ar unknown

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