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
  • B01J19/18—Stationary reactors having moving elements inside
  • B01J19/1806—Stationary reactors having moving elements inside resulting in a turbulent flow of the reactants, such as in centrifugal-type reactors, or having a high Reynolds-number
• • 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
  • B01J4/00—Feed or outlet devices; Feed or outlet control devices
  • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
• • 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
  • B01J2219/00049—Controlling or regulating processes
  • B01J2219/00051—Controlling the temperature
  • B01J2219/00054—Controlling or regulating the heat exchange system
  • B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
  • B01J2219/00058—Temperature measurement
  • B01J2219/00063—Temperature measurement of 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
  • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J2219/00049—Controlling or regulating processes
  • B01J2219/00051—Controlling the temperature
  • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
  • B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
  • B01J2219/00083—Coils
• • 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
  • B01J2219/00049—Controlling or regulating processes
  • B01J2219/00051—Controlling the temperature
  • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
  • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
  • B01J2219/00094—Jackets
• • 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
  • B01J2219/00049—Controlling or regulating processes
  • B01J2219/00051—Controlling the temperature
  • B01J2219/00132—Controlling the temperature using electric heating or cooling elements
  • B01J2219/00135—Electric resistance heaters
• • 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
  • B01J2219/00049—Controlling or regulating processes
  • B01J2219/00191—Control algorithm
  • B01J2219/00193—Sensing a parameter
  • B01J2219/00204—Sensing a parameter of the heat exchange system
• • 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
  • B01J2219/00049—Controlling or regulating processes
  • B01J2219/00191—Control algorithm
  • B01J2219/00222—Control algorithm taking actions
  • B01J2219/00227—Control algorithm taking actions modifying the operating conditions
  • B01J2219/00238—Control algorithm taking actions modifying the operating conditions of the heat exchange system

Definitions

• the invention relates to a process and system for preparing ionic liquids, particularly to a process and system for preparing ultra pure ionic liquids.
• Ionic liquids are attracting a lot of attention as novel, volatile organic compound free solvent system for carrying out chemical reactions.
• the purity of the ionic liquids is of great importance, because impurities can, for example, have a generally adverse effect on the course of chemical reactions.
• many ionic liquids prepared by existing processes and systems, especially these ionic liquids that are air and water sensitive, e.g. chloroaluminate ionic liquids which tend to be unstable in the presence of air or water always can't meet high purity standards. Therefore, it is desired to provide a process and system for preparing ultra-pure ionic liquids.
• the process includes following steps: purifying
• Embodiments of the present invention further provide a system
• rotor-stator mixer such that the ionic liquid produced by the rotor-stator mixer can be fed into the reactor, a first reactant feeder to feed a first reactant into the reactor, a second reactant feeder to feed a second reactant into the reactor, and a mixing device to mix the ionic liquid from the rotor-stator mixer, the first reactant, and the second reactant in the reactor.
• the first and second reactants dissolve in the ionic liquid and react with each other to produce a product ionic liquid similar to the ionic liquid.
• Embodiments of the present invention further provide a system, which comprises a rotor-stator mixer for mixing a solid reactant with a fluid reactant to produce the ionic liquid, a first feeder for feeding the solid reactant to the rotor-stator mixer, and a second feeder for feeding the fluid reactant to the rotor-stator mixer.
• the first feeder comprises a reservoir for storing the solid reactant and a screw motor to carry the solid reactant from the reservoir to the rotor-stator mixer.
• the second feeder comprises a temperature control device to maintain the fluid reactant in fluid form, and at least two feeding members to alternately feed the fluid reactant to the rotor-stator mixer.
• Embodiments of the present invention further provide a process of preparing an ionic liquid.
• the process includes following steps: purifying an alkyl imidazole, an alkyl halide, and a metal halide; causing a reaction between the alkyl imidazole and the alkyl halide to produce a halide containing an object cation; feeding the metal halide and the halide containing the object cation into a rotor-stator mixer; and mixing the metal halide and the halide containing the object cation to cause them to react with each other in the mixer to produce an ionic liquid.
• FIG. 1 is a schematic diagram showing an overall production procedure of EMICAl.
• FIG. 2 is a diagram showing water contents in MIM purified by different purification procedures.
• FIG. 3 is a schematic diagram showing an MIM purification system.
• FIG. 4 is a diagram showing purification efficiencies of AICI 3 by different sublimation methods.
• FIG. 5 is a schematic diagram showing a sublimation system and a sublimation procedure of AICI 3 .
• FIG. 6 is a schematic diagram showing an autoclave system used for synthesizing EMIC
• FIG. 7 is a diagram showing an EtCl source and an autoclave of the autoclave system of FIG. 6.
• FIG. 8 is a schematic diagram of an HTMX system in which AICI 3 and EMIC are mixed and react to EMICAl.
• FIG. 9 is a diagram showing an EMIC feeder of the HTMX system.
• FIG. 10 is a schematic diagram of a scale-up EMICAl production
• a system and process of the present invention are suitable to cause
• object cation to react with a metal halide to obtain an object ionic liquid.
• Example of ionic liquids that can be produced by said system and process
• EMICAl a whole process of preparing EMICAl is divided in three main steps: source purification (raw-material purification), synthesis of l-ethyl-3-methylimidazolium chloride (EMIC), and synthesis of EMICAl.
• source purification raw-material purification
• EMIC synthesis of l-ethyl-3-methylimidazolium chloride
• a main challenge is to prevent any water to enter the system, and another major issue is to decrease metal content in the EMICAl synthesis step.
• all processes are preferred to be operated in dry and inert atmosphere, and reactants 1 -methylimidazole (MIM) and ethyl chloride (EtCl) are preferred to be dried.
• MIM -methylimidazole
• EtCl ethyl chloride
• the metal impurities in the AlCl 3 may be removed by sublimation.
• setups for the synthesis of EMIC and EMICAl may be designed to decrease the metal content.
• the conversion of MIM in the EMIC synthesis step is preferred to be enhanced to reach almost 100%.
• the first step in the synthesis of ultra pure ionic liquids is raw material purification.
• the raw materials are MIM, EtCl, and AlCl 3 .
• This section will describe the detailed purification procedures for MIM and AlCl 3 .
• EtCl is purified in-situ in the EMIC synthesis step.
• a drying-distillation purification method comprises a drying procedure and a distillation procedure.
• MIM is dried, and then in the distillation procedure, the dried MIM is distilled.
• MIM may be dried by storing MIM over CaH 2 in inert and dry atmosphere, or refluxing MIM over CaH 2 .
• MIM is stored over 4wt% CaH 2 for 7 days in inert and dry atmosphere, and thereby the water content of the MIM can be reduced to about 300 ppm (by mass, and the water contents hereafter are all calculated by mass while metal contents are calculated by mole).
• MIM is refluxed over 4wt% CaH 2 at 250 0 C for 12 hours, and thereby the water content of the MIM can be reduced to about 65 ppm.
• FIG. 2 shows decrease of water content in MIM due to optimization of drying procedure.
• FIG. 3 shows a purification system 3 for carrying out a refluxing-distillation purification method comprising a refluxing procedure (for drying MIM) and a distillation procedure.
• a refluxing procedure for drying MIM
• a distillation procedure for drying MIM
• the three-neck round flask 311 is firstly connected to refluxing devices in order to reflux MIM, and then is connected to distillation devices after refluxing is finished, in order to distill the refluxed MIM.
• (a) Refluxing step Firstly, the three-neck flask 311 and other refluxing devices are cleaned in a KOH-bath over night, rinsed and stored in 0.1 molar HCl bath for 10 minutes, and then washed with deionised water and dried at 70 0 C for 3 hours. After cooling down naturally, they can be installed to form a refluxing system 31 as shown in left section of FIG. 3.
• the refluxing system 31 further comprises a stirrer 313 in the three-neck flask 311 and a heater 314 under the three-neck flask 311.
• One neck 315 of the three-neck flask 311 is used to add MIM and CaH 2 into the three-neck flask 311 and can be stoppered with a plug 316.
• a second neck 317 is connected to a tube 318 loaded with a cooler 319, and the tube 318 is connected to an over pressure valve 320 via a valve 321 for opening and closing a connection between the tube 318 and the over pressure valve 320.
• a third neck 323 is connected to a dry gas/vacuum switch valve 324 via a valve 325 for opening and closing a connection between the neck 323 and the switch valve 324.
• the dry gas/vacuum switch valve 324 is connected to a dry gas/vacuum system and enables the neck 323 to selectively connect with a dry gas or a vacuum pump.
• the stirrer 313 is a magnetically driven stirrer and the dry gas is argon (Ar). All connections are sealed with a small amount of grease and clipped.
• the refluxing system 31 is heated by vacuum/Ar technique (i.e. vacuumed and then refilled with dry argon, which two procedures are repeated for several times).
• vacuuming procedure the valve 321 is closed, the valve 325 is open, and the valve 324 is turned to the vacuum pump.
• Ar refilling procedure the valve 321 is closed, the valve 323 is open, and the valve 324 is turned to Ar line.
• MIM and 8wt% CaH 2 are filled into the flask 311 with continuous Ar flow.
• the neck 315 is closed by the plug 3 l ⁇ and then the system is vacuumed and refilled with dry Ar.
• the vacuuming and refilling procedure is repeated three times.
• devices for distillation include three distillation flasks 331, 333 and 335 with different volumes, a cooler 336, a distilling adapter 337, and a stop flask 339. While the refluxed MIM cools down in Ar flow, these devices are cleaned, assembled, and dried similarly as described above in the refluxing step.
• the distillation flasks 331, 333 and 335 are assembled to the distilling adapter 337 via the cooler 336, and the distilling adapter 337 are provisionally connected to the stop flask 339 before the three-neck flask 311 being connected in.
• valves 321, 323 and 343 are connected to Ar line, the flask 339 is taken away from the distilling adapter 337, the tube 318 is taken away from the neck 317 of the three-neck flask 311, and then the neck 317 is connected to the distilling adapter 337 under the protection of dry Ar.
• the three-neck round flask 311 and the distilling adapter 337 are insulated with an aluminum foil (not shown).
• the distillation flasks 331, 333 and 335, the cooler 316 and the distilling adapter 337 are vacuumed and refilled by Ar for four times while being heated with heat gun.
• Distillation of MIM is carried out in vacuum at a certain temperature.
• MIM is controlled to distill in vacuum of about 8.5x10 " mbar or below at a temperature of about 35 0 C.
• Distilled MIM is allowed into any one of the three flasks 331, 333 and 335.
• the distilled MIM is allowed into the smallest flask 335, then into the middle-volume flask 333, and finally into the largest flask 331 after the flask 333 is filled with a certain distilled MIM.
• valve 345 is connected to Ar line and the flask 331 is separated from the distilling adapter 337 with the protection of dry Ar and sealed with "parafilm".
• Main impurities OfAlCl 3 are hydroxides (formed with water), sulfates and metals such as Fe, Cr, Ni, Zn, Mn, Mg, Cu, Pb, etc. Sublimation in dry environment can get rid of all these impurities.
• FIG. 4 depicts purification efficiencies of different sublimation methods.
• the third method is described below by way of example.
• FIG. 5 depicts a system 5 and a schematic procedure of AlCl 3 sublimation.
• the sublimation system comprises a sublimation flask 51 , a heater 52, and a cooler 53.
• the sublimation flask 51 is connected to a valve 55, and the valve 55 is connected to a valve 56, which is connected with a high pressure valve 57 and a vacuum/Ar switch valve 58.
• the vacuum/Ar switch valve 58 is connected to a vacuum/Ar system.
• glassware such as the flask 51 is cleaned, assembled and dried with a heat gun in vacuum.
• AlCl 3 and additives are added into the sublimation flask 51.
• 5 g Al powder is soaked into 100 ml 0.1 mol/1 HCl aqueous solution for 2 hours in order to remove oxide layers on the top surface.
• the fresh Al powder is dried at 60 0 C for 5 hours under Ar protection.
• 100 g Of AlCl 3 , 3 g NaCl and 3 g Al powder are filled into a 500 ml plastic bottle and mixed by using vortex mixer at 900 rpm for 0.5 h.
• the mixture is transferred into the sublimation flask 51 under continuous Ar flow.
• the sublimation flask 51 is closed and its inside atmosphere is replaced by three times vacuuming and refilling with Ar.
• the mixture OfAlCl 3 and additives may need vacuuming pretreatment for 12 h.
• the pretreatment is carried out by connecting the sublimation flask 51 to the vacuuming line and increasing the temperature of the sublimation flask 51 to 90 0 C.
• the sublimation flask 51 is refilled with Ar and connected to the over pressure valve 57 which controls a pressure of sublimation.
• the sublimation is carried out at 1 bar.
• the valve 55 is closed, the cooler 53 is turned on, and the temperature of the heater 52 is increased to 210 0 C and kept for about 2 hours until the sublimation OfAlCl 3 stops.
• the over pressure valve 57 is closed and the system 5 is allowed to cool down with continuous Ar flow.
• the purified AlCl 3 is taken out in the glove box.
• the purified AlCl 3 is grinded using a glass mortar and screen into 20-60 mesh powders, and then added into a sample bottle, sealed with paraffin film and stored in a desiccator in Ar atmosphere and P 4 O 10 as desiccants.
• MIM reacts with ethyl chloride to EMIC, a highly hydrophilic ionic liquid.
• the synthesis of EMIC is preferably carried out in an autoclave or the like since a high pressure (e.g. 8 bar) may be reached during the reaction, and the whole process is preferably operated in dry and inert environment since a main requirement for EMIC synthesis is to be water free (less then 50 ppm water). Furthermore, a conversion of MIM is needed to be very high (e.g. 99.999%) and a total metal content is needed to be very small (e.g. below 50 ppm).
• FIG. 6 shows an autoclave system 6 used for synthesizing EMIC.
• the autoclave system 6 includes an autoclave 61, an ethyl chloride source (e.g. an EtCl storage bottle) 63 immersed in an oil bath 64, an MIM source (e.g. an MIM storage bottle) 65, and an EMIC bottle 67 for sampling EMIC, all of which are placed in a hood so that any emitted gas can be vented.
• the autoclave 61 is equipped with an Ar/vacuum system. Ar is dried in a cascade of silica gel, KOH, molecular sieve 4A, and 50% P 4 O 10 in glass beads, and is then distributed together with a vacuum line in four channels in the hood. One line is permanently connected to the autoclave 61 and a second with the EtCl storage bottle 63. The other two lines are connected with the MIM source 65 and EMIC bottle 67 during sample taking, respectively.
• an ethyl chloride source e.g
• EtCl is in-situ purified in the autoclave system 6.
• Main impurities in EtCl are water and HCl.
• EtCl actually has a boiling point of 12 0 C and is therefore easy to purify.
• the raw EtCl is condensed into the storage bottle 63 for the EMIC synthesis reaction.
• the raw EtCl passes a KOH-column, which removes the HCl by forming water and KCl, then passes a column filled with P 4 O 1O and glass beads, which removes the water, and then enters into the EtCl storage bottle 63.
• EtCl flows from the storage bottle 63 to the autoclave 61.
• the whole system 6 may be operated at a pressure up to 8 bar, therefore it is preferred to use 2 ⁇ m gas filters 601, 603 and 605 after the P 4 O 10 columns to prevent contamination by the desiccant.
• the inside of the autoclave 61 may be coated with a material which is inert to reactants and resultants of the EMIC synthesis reaction and is capable of withstanding the reaction temperature and pressure.
• the inside of the autoclave 61 is "Teflon" coated.
• the autoclave system 6 is leak checked.
• the leak check includes check in vacuum and check at high pressure. Then the autoclave system 6 is dried.
• Valve V6 is closed to disconnect the EtCl source 63 from the rest of the system and the oil bath 64 is cooled to a temperature of about - 30 0 C at Ar flow (V7 and V14 are opened).
• the bottle 63 Before being fed with EtCl, the bottle 63 is vacuumed. During vacuuming, V14 is closed and Vl 8 opened. Then V7 is closed and V30, V31 , and Vl to V5 are opened to make raw EtCl flow through purification columns into the storage bottle 63. After a predetermined portion of EtCl condensed into the bottle 63, Vl to V5 and V30, V31 are closed.
• the MIM storage bottle 65 is connected to the autoclave 61 with continuous Ar flow (V9, V 12, V 11 , bottle valve 651, and V 15 open). Then V 11 is closed and Vl 5/Vl 9 is used to replace the atmosphere in the bottle 65 with dry Ar. Vl 1 is opened and MIM enters the autoclave 61 under pure Ar flow. In order to control the amount of MIM, the bottle 65 is placed on a scale.
• the bottle 67 is kept at vacuum pressure (valve 671 is closed) and VlO slowly opened to let EMIC out.
• Ar is allowed to enter the bottle 67 by opening V13 and the valve 671.
• the silicon cover is removed under Ar flow and the bottle 67 quickly covered with a glass stop.
• the atmosphere in the bottle 67 is replaced by three times by the vacuum/Ar technique.
• the bottle 67 is sealed with "parafilm" and ready for purification.
• the reaction between MIM and ethyl chloride for producing EMIC is highly exothermic.
• a reaction temperature of the reaction is above 90 0 C, cross products such as dimethyl- and diethyl-imidazoliumchlorid may be formed. Therefore, the reaction temperature (Tl in FIG. 7) is preferably controlled below 90 0 C (e.g. at 80 0 C) as long a reaction rate is fast enough. Therefore, the autoclave 61 may be externally heated but innerly cooled. In one embodiment, the autoclave 61 is externally heated to 80 0 C and innerly cooled with water.
• the concentration of EtCl entering the autoclave 61 is self-controlled by its partial pressure, which pressure can be controlled by temperature (T2 in FIG. 7) in the EtCl storage bottle 63. In one embodiment, the temperature T2 is controlled by an oil bath for the EtCl storage bottle 63.
• an optimized condition is as follows:
• Tl 80 0 C for 24 h
• Tl 90 0 C (24 h to 72 h);
• T2 120 °C (24 h to 72 h);
• the next step is the reaction of EMIC with AICI 3 to EMICAl.
• a challenge for this reaction is to uniformly mix the solid AlCl 3 with EMIC, which is heated to a fluid form.
• the reaction is carried out in a rotor-stator mixer, in particular, a high-shearing force rotor-stator mixer, such as the high throughput mixer (HTMX) developed by Accelergy Corporation of Palo Alto, California.
• HTMX high throughput mixer
• An HTMX system 8 including a said HTMX 81 (referred as mixer 81 hereafter for short) is shown in FIGs. 8 and 9.
• the mixer 81 of the HTMX system 8 comprises two substantially cylindrical members 811 and 812.
• Member 811 which serves as a rotor, is mounted within member 812, which serves as a stator.
• a space is formed between members 811 and 812 and acts as an annular reaction chamber for mixing EMIC with AlCl 3 and causing them to react to produce EMICAl.
• the reaction temperature may be controlled by an oil bath 813. More details of the mixer are described in Chinese Patent Application Number CN200610172190.0, which is incorporated here by reference.
• the HTMX system 8 further includes a feeder 83 that feeds the solid AlCl 3 to the mixer 81.
• the AlCl 3 powder is stored in a reservoir 831 of the feeder 83 and is slowly fed into the mixer 81 by a screw motor 832 of the feeder 83.
• a stirrer placed at the end of the screw motor 832 can ensure a homogeneous flow of the solid AlCl 3 into the mixer.
• the feeder 83 is placed together with the mixer 81 in an inert/dry gas chamber 84 with a continuous dry Ar flow at a flow rate of, for example, 1 1/minute and at a pressure of, for example, 2 bar.
• the HTMX system 8 further includes another feeder 85 that feeds the EMIC in a fluid form into the mixer 81.
• the feeder 85 includes a reservoir 851 used to store the EMIC and two syringes 853 and 854 and used to feed the EMIC to the mixer 81. Since EMIC is solid at room temperature, all the lines for EMIC, including the reservoir 851 and syringes 853 and 854 are heated. In one embodiment, they are heated above 80 0 C.
• the syringe 853 feeds EMIC into the mixer 81, yet the syringe 854 is refilled with EMIC by increasing Ar pressure to the reservoir 851.
• the syringe 853 is refilled with EMIC and the second syringe 854 feeds the EMIC into the mixer 81. These two states are repeated, and therefore a continuous EMIC feeding may be realized.
• the HTMX system 8 further comprises an EMICAl collecting bottle 871 and a waste bottle 872, both of which are connected with the mixer 81 and an Ar/vacuum system. There is a valve 873 switchable between the two bottles 871 and 872. The connection and disconnection procedure, respectively are carried out as described before. This method ensures that no air or moisture contacts the product EMICAl.
• the whole process of EMICAl synthesis contains the following several operations: (a) cleaning and drying the whole system; (b) starting the reaction; (c) collecting samples. A whole procedure will be described hereafter by way of example.
• All parts of the HTMX system 8 needs to be disassembled and cleaned. They are washed first with water and acetone then dried in an oven at 120 0 C for several hours. After being dried, they are assembled again.
• the mixer 81 is heated to 100 0 C at vacuum for 90 min. Then after at least three times of vacuum/Ar refill procedures, the HTMX system 8 is protected by continuous Ar flow with a flow rate of, for example, lOOO ml/min.
• the EMIC reservoir 851 and the syringes 853 and 854 are heated to 120 0 C to melt EMIC into a fluid and maintain it in fluid form.
• the HTMX system needs to be dissembled and cleaned.
• EMICAl is used as a seed solvent to dissolve AlCl 3 powder and EMIC fluid or powder, and causing the AlCl 3 powder and EMIC fluid or powder to mix with each other and react with each other to produce more product EMICAl.
• a scale-up system may be developed to use the EMICAl prepared by a mixer, such as an HTMX system, as a seed solvent to dissolve AlCl 3 powder and EMIC fluid or powder, and thereby to produce a product EMICAl similar to the EMICAl prepared by the HTMX system in a large scale, wherein "similar” used herein means the product EMICAl (EMICAl is a short for EMIC-11AICI 3 as mentioned before) may have a same or a different valve of "n" to that of the EMICAl prepared by the HTMX system ("n" is a ratio between EMIC to AlCl 3 in EMICAl).
• the scale-up system 10 comprises an aforementioned HTMX system 101, a reactor system 102 including a reactor 103 such as an autoclave, in which a large scale EMICAl production can be carried out, an AlCl 3 feeder 104 to feed AlCl 3 into the reactor 103 and an EMIC feeder 105 to feed the EMIC into the reactor 103.
• the HTMX system 101 is used to prepare seed EMICAl which is fed into the reactor 103 as a solvent.
• the AlCl 3 feeder 104 may be similar to the feeder 83 in the HTMX system 8.
• the reactor system 102 may further comprise a stirrer/mixer 106 for mixing the seed EMICAl and the reactants AlCl 3 and EMIC.

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• 2007
  • 2007-09-29 CN CN 200710181069 patent/CN101230041B/zh not_active Expired - Fee Related
  • 2007-09-29 WO PCT/CN2007/070832 patent/WO2008043309A1/en active Application Filing

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