WO2010073216A1 - Réacteur pour réactifs liquides non miscibles - Google Patents

Réacteur pour réactifs liquides non miscibles Download PDF

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Publication number
WO2010073216A1
WO2010073216A1 PCT/IB2009/055905 IB2009055905W WO2010073216A1 WO 2010073216 A1 WO2010073216 A1 WO 2010073216A1 IB 2009055905 W IB2009055905 W IB 2009055905W WO 2010073216 A1 WO2010073216 A1 WO 2010073216A1
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WO
WIPO (PCT)
Prior art keywords
reactor
products
liquid phases
oil
plates
Prior art date
Application number
PCT/IB2009/055905
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English (en)
Other versions
WO2010073216A8 (fr
Inventor
Elio Santacesaria
Martino Di Serio
Riccardo Tesser
Rosa Turco
Domenico Verde
Luca Casale
Original Assignee
Mythen Spa
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.)
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Publication date
Application filed by Mythen Spa filed Critical Mythen Spa
Publication of WO2010073216A1 publication Critical patent/WO2010073216A1/fr
Publication of WO2010073216A8 publication Critical patent/WO2010073216A8/fr

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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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/248—Reactors comprising multiple separated flow channels
    • B01J19/249—Plate-type reactors
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/248—Reactors comprising multiple separated flow channels
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L1/00—Liquid carbonaceous fuels
    • C10L1/02—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
    • C10L1/026—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only for compression ignition
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
    • C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
    • C11C3/003—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fatty acids with alcohols
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/24—Stationary reactors without moving elements inside
    • B01J2219/2401—Reactors comprising multiple separate flow channels
    • B01J2219/245—Plate-type reactors
    • B01J2219/2451—Geometry of the reactor
    • B01J2219/2453—Plates arranged in parallel
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/24—Stationary reactors without moving elements inside
    • B01J2219/2401—Reactors comprising multiple separate flow channels
    • B01J2219/245—Plate-type reactors
    • B01J2219/2451—Geometry of the reactor
    • B01J2219/2456—Geometry of the plates
    • B01J2219/2458—Flat plates, i.e. plates which are not corrugated or otherwise structured, e.g. plates with cylindrical shape
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/24—Stationary reactors without moving elements inside
    • B01J2219/2401—Reactors comprising multiple separate flow channels
    • B01J2219/245—Plate-type reactors
    • B01J2219/2451—Geometry of the reactor
    • B01J2219/2456—Geometry of the plates
    • B01J2219/2459—Corrugated plates
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/24—Stationary reactors without moving elements inside
    • B01J2219/2401—Reactors comprising multiple separate flow channels
    • B01J2219/245—Plate-type reactors
    • B01J2219/2461—Heat exchange aspects
    • B01J2219/2462—Heat exchange aspects the reactants being in indirect heat exchange with a non reacting heat exchange medium
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/24—Stationary reactors without moving elements inside
    • B01J2219/2401—Reactors comprising multiple separate flow channels
    • B01J2219/245—Plate-type reactors
    • B01J2219/2474—Mixing means, e.g. fins or baffles attached to the plates
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/24—Stationary reactors without moving elements inside
    • B01J2219/2401—Reactors comprising multiple separate flow channels
    • B01J2219/245—Plate-type reactors
    • B01J2219/2476—Construction materials
    • B01J2219/2477—Construction materials of the catalysts
    • B01J2219/2481—Catalysts in granular from between plates
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/24—Stationary reactors without moving elements inside
    • B01J2219/2401—Reactors comprising multiple separate flow channels
    • B01J2219/245—Plate-type reactors
    • B01J2219/2491—Other constructional details
    • B01J2219/2497—Size aspects, i.e. concrete sizes are being mentioned in the classified document
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10—Feedstock materials
    • C10G2300/1011—Biomass
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P30/00—Technologies relating to oil refining and petrochemical industry
    • Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock

Definitions

  • the invention relates to a reactor for liquid reagents which are immiscible with each other, in particular a reactor for the production of biodiesel.
  • the invention also relates to a plant comprising said reactor and a method for using said reactor.
  • numerous reactions occur between two liquid phases which are immiscible with each other.
  • One reaction of this type which has recently acquired a very important role is, for example, the reaction of oils and/or fats with alcohols in order to obtain so-called biodiesel.
  • the oil phase and the alcohol phase which are partly immiscible, give rise to a two-phase system.
  • Biodiesel which chemically corresponds to a mixture of long-chain fatty acid esters, is obtained by means of a process involving transesterification of vegetable oils and/or animal fats with light alcohols, preferably with methanol, in the presence of alkaline catalysts.
  • the present-day production technology is based on the use of basic homogeneous catalysts such as sodium hydroxide (NaOH), potassium hydroxide (KOH) or sodium methylate (CH 3 ONa).
  • NaOH sodium hydroxide
  • KOH potassium hydroxide
  • CH 3 ONa sodium methylate
  • the transesterification reaction occurs by means of a process with stages during which the triglycerides are converted into diglycerides which are then converted into monoglycerides and finally into glycerol. At the end of the reaction, therefore, a phase consisting of a mixture of esters and a phase containing the glycerol as co-product are obtained.
  • the configuration of the plants and the reaction conditions are generally similar to those described in the patent US 4,303,590.
  • This configuration envisages a first reaction stage conducted at the boiling point of methanol (64.7 0 C) for a reaction time of between 30 and 120 minutes, with a catalyst concentration of between 0.1% and 1% by weight relative to the oil.
  • the produced glycerol is separated from the esteric phase.
  • the latter is subjected to a second transesterification stage for a period of between 5 and 60 minutes.
  • the speed of reaction in transesterification using homogeneous catalysts is very high, so much that in stirred reactors said reaction is often dominated by the transfer of mass owing to the presence of two immiscible phases.
  • a present objective within the industry is to intensify the biodiesel production process and there therefore exists the need to develop a reactor which is characterized by high yields for short residence times and which can be produced in a simple and cost-effective manner.
  • the object of the present invention is to solve at least partially the drawbacks identified in connection with the reactors, the plants and the methods of the known type.
  • an aim of the present invention is to provide a reactor for carrying out reactions between immiscible liquids, such as a reactor for the production of biodiesel, which has a high yield and productivity.
  • Claim 1 by a plant according to Claim 7 and by a method according to Claim 11.
  • Figure 1 shows a schematic view of a plant comprising a reactor according to the invention
  • Figure 2 shows schematically a side view of a single-cavity reactor according to the invention
  • Figure 3 shows schematically the cross-section along the line IIMII of Figure 2;
  • Figure 4 shows schematically a plan view of the reactor according to Figure 2;
  • Figure 5 shows schematically the cross-section along the line V-V of Figure 4.
  • Figure 6 shows a front view of a multiple-cavity reactor according to the invention
  • Figure 7 shows a side view of the reactor according to Figure 6;
  • Figure 8 shows a perspective view of a component of a possible reactor according to the invention.
  • Figure 9 illustrates schematically operation of a possible multiple-cavity reactor according to the invention.
  • the present invention relates to a reactor 20 for at least two reagents supplied in two liquid phases 12 and 13.
  • the reactor comprises an inlet 21 for receiving the two liquid phases 12 and 13; an outlet 22 for discharging the reaction products 14, and a channel 23 for receiving a continuous flow of reagents and/or products.
  • the channel 23 comprises, at least along one section, an interspace or cavity 28 enclosed between two plates 24 arranged at a distance of at least 0.5 mm.
  • the channel 23 comprises means 25 for promoting the turbulence in the continuous flow of reagents and/or products.
  • the reactor 20 also comprises means 26 for producing a heat exchange between the walls and the continuous flow of reagents and/or products.
  • the plates 24 of the reactor 20 according to the invention are arranged at a distance not greater than 10 mm, preferably at a distance of between 1 mm and 3 mm, and even more preferably at a distance of between 1.5 mm and 2 mm.
  • the plate reactor 20 comprises a single cavity 28 enclosed between two plates 24.
  • the plate reactor 20 comprises a plurality of cavities 28, each enclosed between two plates 24.
  • the means 25 for promoting the turbulence in the continuous flow of the reagents and/or the product comprise corrugations or knurled zones on the surface of the plates 24. See, for example, Figures 8 and 9.
  • the distance between the plates 24 may be defined by the contact point of the peaks of the corrugations of one plate on the valleys of the corrugations of the adjacent plate.
  • the means 25 for promoting the turbulence in the continuous flow of the reagents and/or the product comprise filler material between the plates 24.
  • This filler material may be in the form of granules, beads, flakes, filaments, membranes or the like.
  • the filler material between the plates 24 is inert. It therefore does not take part in the chemical reaction between the reagents, but has only the function of promoting the turbulence in the flow, In other embodiments, the filler material between the plates 24 is instead suitable for performing a catalytic activity.
  • the means 26 for producing a heat exchange between the plates 24 and the continuous flow of the reagents and/or the product comprise means 4 for healing the plates to a temperature of between 10 0 C and 300 0 C, and preferably between 50 0 C and 200 0 C.
  • the means for producing the heat exchange are jackets 26 which are arranged against the plates 24 of the reactor.
  • the jackets 26 may for example comprise electric resistances (suitable for heating) and/or a fluid circuit (suitable for heating or cooling).
  • the temperature of the jackets 26 may be controlled by means of a circuit, in a manner known per se, not shown in the figures for the sake of simplicity.
  • the plate reactor 20 may have a form which is similar to that of a plate heat exchanger (see Figures 6 to 9).
  • Plate reactors 20 according to the invention comprise a plurality of plates which are airanged as sho"wn in the diagrams according to Figure 7 (where the reactor is closed) and Figure 9 (where the reactor is open so as to show the flows which are generated inside it).
  • the plate reactor may be sealed or of the type which can be opened so as to allow the inspection, cleaning and/or maintenance thereof. In the case of sealed ⁇ eactors, the hydraulic and mechanical seal between the plates is ensured by means of braze-weld ⁇ ng.
  • elastomer seals 27 allow the formation of two channels for conveying the two fluids involved which may be supplied flowing in the same direction or in opposite directions.
  • Each of the two channels comprises a series of cavities 28 situated between the plates 24 in the manner described above. These cavities may be arranged in parallel and/or in series.
  • the means 26 for producing the heat exchange between the plates 24 and/o ⁇ the product comprise a circuit inside which a service fluid flows at a controlled temperature.
  • the service fluid used in this type of plant may be, in manner known per, diathermic oil, water, ethylene glycol or the like.
  • the means 26 for producing the heat exchange also comprise a boiler 4 for heating and circulating the service fluid at a predetermined temperature.
  • the means 26 for producing the heat exchange comprise a refrigerating unit suitable for cooling and circulating the service fluid at a predetermined temperature.
  • the exchange coefficient is two to three times greater than that of a tube- bundle exchanger and therefore, for the same potential, the dimensions of the plate exchanger are much smaller, allowing it to be positioned in restricted spaces.
  • Plate exchangers are used in particular in those cases where low exchange coefficients, due to the characteristics of the liquid or to low speeds, require special arrangements in order to increase the coefficient itself.
  • the operational limits which are determined by the elastomer seals, normally correspond to temperatures not higher than 200 0 C and pressures not greater than 1.0 Mpa.
  • the temperature may be as high as 300 0 C, while the pressure may reach 2.5 MPa since the only - usually less stringent - limitation is thai determined by the external bolting means.
  • the plates 24, and the associated external bolting means are available in different sizes of surface area per unit and with differently angled fishbone corrugations.
  • the number of plates 24 for each exchanger varies depending on the flowrates and the temperatures of the two fluids.
  • the distance between the plates is achieved by means of moulded bosses which ensure that it remains constant even in the presence of major differences in pressure.
  • the corrugation pattern of the plates induces a type of flow which is highly turbulent for relatively low flowrates.
  • the high turbulence inside the plate exchangers therefore increases considerably the mass and heat transfer speeds at low flowrates.
  • the corrugation pattern induces firstly separation and then merging together of the flow, in each case reproducing the boundary layer, which influences the heat transfer coefficient.
  • the flow inside the cavities 28 between the plates 24 is subject to a series of periodic changes in direction, encountering peaks and valleys.
  • the flow diagram is complex, owing to the presence of a secondary swirling motion, also known as Gortler vortices, along the cross-section and it is considered that the type of local flow controls the transfer.
  • a mixture of the two liquid phases 12 and 13 containing the two reagents is circulated inside a first channel 23.
  • a service fluid may be circulated inside the second channel in order to control the reaction temperature.
  • the present invention also relates to a plant 1 comprising a plate reactor 20 according to the above description.
  • the plant 1 according to the invention also comprises means 2 and 3 for continuous supplying of the two liquid phases 12 and 13 to the reactor 20 and means 6 for continuously discharging the products 14 from the reactor 20.
  • the means 6 for discharging the products 14 may advantageously lead into a storage tank 7 of the closed type.
  • the plant 1 also comprises means 11 for maintaining the internal pressure of the plant between 0.01 and 2.5 MPa, and preferably between 0.1 and 1 Mpa.
  • the means for regulating the internal pressure of the plant comprise a source 11 of nitrogen (N 2 ) under pressure. This source 1 1 of nitrogen is able to fill the part of the storage tank 7 of the closed type which is not occupied by the product 14, It is thus possible to maintain, within the storage tank 7 and the plant 1, a pressure different i ⁇ om the atmospheric pressure.
  • the plant 1 also comprises means 50 for rough pre-m ⁇ xing of the two liquid phases 12 and 13 upstream of the reactor 20.
  • the means 50 for rough pre-mixing of the two liquid phases 12 and 13 comprise a static mixer of the type known per se.
  • the means 50 for rough pre- mixing of the two liquid phases 12 and 13 may also comprise means for preheating the mixture upstream of the reactor 20.
  • the plant 1 may advantageously comprise a branch line for removing samples 15 of the products 14 in order to check their properties.
  • part of the flow of the products 14 can be deviated by means of a three-way valve 9 and the samples 15 may thus be removed at given time intervals.
  • the branch line leading off the main line 6 comprises an efficient condenser 10.
  • the invention also relates to a method for obtaining products 14 from a chemical reaction between at least two reagents supplied in two liquid phases 12 and 13.
  • the method comprises the steps of: supplying the two liquid phases 12 and 13 to a reactor 20 which has a reaction chamber formed as a channel 23 able to receive a continuous flow of the two liquid phases 12, 13 and/or the products 14, the channel 23 comprising, at least along one section, a cavity 28 which is enclosed between two plates 24 arranged at a distance of at least 0.5 mm, and a channel 23 comprising means 25 for promoting the turbulence within the continuous flow of the two liquid phases 12, 13 and/or of the products 14; producing a heat exchange between the plates 24 and the continuous flow of the two liquid phases 12, 13 and/or of the products 14; and collecting the products 14 at the outlet 22 of the reactor 20.
  • a liquid phase 12 comprises an oil and/or a fat of vegetable or animal origin; the other liquid phase 13 comprises a light alcohol; the two liquid phases are therefore immiscible with each other; the reaction consists in transesterification; and the products 14 of the reaction comprise biodiesel and glycerol.
  • the oil of vegetable origin is selected from the group comprising: rapeseed oil, palm oil and sunflower oil, castor oil, soybean oil, cottonseed oil, peanut oil, algae oil, jatropha oil (jatropha curcas).
  • the light alcohol is ethyl alcohol or preferably methyl alcohol.
  • the method also comprises the step of mixing with the two reagents a basic homogeneous catalyst selected from the group comprising: sodium hydroxide (NaOH), potassium hydroxide (KOH) and corresponding alkoxides with a preference for sodium methoxide (CtTjONa) or sodium ethoxide (CjHsONa).
  • a braze-welded plate reactor 20 was used, with a process volume of 202 ml and a service fluid volume of 250 ml, said reactor being formed by twenty plates 24 arranged at an average distance of between 1.5 mm and 2 mm from each other, as described in Figures 6 to 9.
  • This example shows the results achieved, in terms of conversion into methylesters, for the transesterification reaction within the reactor 20 described above.
  • the transesterification reaction was conducted at the temperature of 6O 0 C, using an oil/methanol molar ratio of 1:6 and potassium hydroxide (KOH) as catalyst, with a weight concentration of 1% by weight relative to the oil.
  • KOH potassium hydroxide
  • the oil phase 12 and the methanol phase 13 are conveyed by means of two piston pumps 2 and 3, first into a premixer 50, kept at the reaction temperature, and then into the reactor 20.
  • Samples 15 may be removed at given time intervals by means of a three-way valve 9. These samples 15 are cooled beforehand by means of a condenser filled 10 with Raschig rings.
  • the products 14 can also be conveyed by means of the three-way valve 9 into a storage tank 7 kept at the operating pressure by means of a nitrogen flow.
  • the storage tank 7 is advantageously used for the reactions conducted under pressure. For the reactions at atmospheric pressure said tank may be dispensed with.
  • the oil phase 12 and the methanol phase 13, in which the catalyst was previously dissolved, are conveyed to the reactor 20 and heated to the reaction temperature of
  • the zero time is considered as being that where the desired pressure and temperature are reached.
  • the samples 15 removed during and at the end of the reaction contain the esteric phase, the glycerol phase, the catalyst, the oil and the methanol which are unreacted.
  • each sample was subjected to preliminary treatment.
  • KOH potassium hydroxide
  • the entry flowrate of the liquid phases 12 and 13 was kept constant at a value of 400 ml/min so as to achieve a residence time of 30 seconds.
  • KOH or associated alkoxides in plate reactors 20 where these plates 24 may be smooth or suitably corrugated with an average distance between the walls which may range from 0.5 to 10 mm, preferably 1 and 3 mm, operating with fluid flowrates which will vary with the volume of the reactor, but such as to generate a turbulent condition in the cavity between one plate and another.
  • the reactor 20 With the reactor 20 according to the invention, it is possible to operate within a pressure range of between 0.01 and 2.5 MPa, preferably between 0.1 and 1 MPa and at temperatures of between 1O 0 C and 300 ⁇ C, and preferably between 50 0 C and 200 c C.
  • the reactor 20 With the reactor 20 according to the invention it is possible to fill the cavity 28 inside which the reaction takes place with an inert filler material of suitable size and any shape (balls, flakes, filaments, etc.) in order to improve the local turbulence.
  • an inert filler material of suitable size and any shape (balls, flakes, filaments, etc.) in order to improve the local turbulence.
  • the reactor 20 With the reactor 20 according to the invention it is possible to fill the cavity 28 inside which the reaction takes place with an active material (which may perform a catalytic activity) of suitable size and any shape (balls, flakes, filaments, as well as membranes, etc.), having the dual function of improving the turbulence and providing a catalytic action.
  • an active material which may perform a catalytic activity
  • suitable size and any shape balls, flakes, filaments, as well as membranes, etc.
  • the plate reactor 20 is surprisingly superior in terms of performance to the reactors and microreactors described with reference to the prior art.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

La présente invention concerne un réacteur 20 contenant au moins deux réactifs introduits dans deux phases liquides 12 et 13. Le réacteur comprend un orifice d'entrée 21 pour recevoir les deux phases liquides 12 et 13 ; un orifice de sortie pour décharger les produits réactionnels 14 ; et un canal 23 pour recevoir un flux continu de réactifs et/ou de produits. Le canal 23 comprend, au moins le long d'une de ses sections, une cavité 28 entourée par deux plaques 24 disposées à une distance d'au moins 0,5 mm. Le canal 23 comprend des moyens 25 pour créer une turbulence dans le flux continu de réactifs et/ou de produits. Le réacteur 20 comprend également des moyens 26 pour produire un échange de chaleur entre les parois et le flux continu de réactifs et/ou de produits. L'invention concerne également une installation et un procédé pour obtenir des produits à partir d'une réaction effectuée dans ce réacteur.
PCT/IB2009/055905 2008-12-23 2009-12-22 Réacteur pour réactifs liquides non miscibles WO2010073216A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT002302A ITMI20082302A1 (it) 2008-12-23 2008-12-23 Reattore per reagenti liquidi immiscibili.
ITMI2008A002302 2008-12-23

Publications (2)

Publication Number Publication Date
WO2010073216A1 true WO2010073216A1 (fr) 2010-07-01
WO2010073216A8 WO2010073216A8 (fr) 2010-09-23

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IT (1) ITMI20082302A1 (fr)
WO (1) WO2010073216A1 (fr)

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4303590A (en) 1979-05-30 1981-12-01 Lion Corporation Method for the preparation of a lower alkyl ester of fatty acids
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