Method for preparing ion liquor

Method for preparing ion liquor

  • CN 1,958,574 B
  • Filed: 11/16/2006
  • Issued: 05/02/2012
  • Est. Priority Date: 11/16/2006
  • Status: Active Grant
First Claim
Patent Images

1. a preparation method of ionic liquid is characterized in that, used a kind of continuous microwave reactor is constructed as follows:

  • it has commentaries on classics wave microwave oven (19) and microwave cavity cavity (4), also has;

    Reactant mixing tank (1);

    Magnetic stirring apparatus (2);

    Constant flow pump (3);

    Reactor drum (5);

    Refrigerating unit (6);

    Product tripping device (7);

    Product collection device (8);

    Feed-pipe (9);

    Extraction line (10);

    Side pipe (11);

    Push pipe (12);

    Phlegma flows into pipe (13);

    Phlegma flows out pipe (14);

    Reactor drum carriage (15);

    Microwave rf generator (16);

    Glass Containers (17);

    Iron stand (18);

    Stirrer (20);

    Loading hopper (21);

    Side opening (22);

    Apical pore (23);

    Condensate stream incoming interface (24);

    Condensate stream outgoing interface (25);

    Charging interface (26);

    Discharging interface (27);

    Plug I (28);

    Pump head (29);

    Plug II (30) and baiting valve (31);

    Microwave cavity cavity (4) is the microwave cavity cavity that changes wave microwave oven (19);

    Microwave rf generator (16) is welded in the bottom of microwave cavity cavity (4);

    Microwave rf generator (16) is gone up and is placed the Glass Containers that fills water (17) that a protection microwave rf generator promptly is used for load;

    Sidepiece and top at microwave cavity cavity (4) are drilled with side opening (22) and apical pore (23) respectively;

    Weld side pipe (11) and push pipe (12) on this side opening (22) and this apical pore (23) respectively;

    The diameter of side pipe (11) and push pipe (12) and oscillation frequency and the wavelength that length depends on microwave oven, its length be greater than microwave oven wavelength 1/2, its internal diameter be less than microwave oven wavelength 1/4;

    Reactor drum (5) is the hard glass bend pipe, and it is positioned in the refrigerating unit (6), and the two ends of reactor drum (5) are respectively charging interface (26) and discharging interface (27);

    The two ends of refrigerating unit (6) are respectively condensate stream incoming interface (24) and condensate stream outgoing interface (25);

    Condensate stream incoming interface (24) flows into pipe (13) with condensate stream outgoing interface (25) and phlegma and phlegma outflow pipe (14) is tightly connected;

    Refrigerating unit (6) places on the reactor drum carriage (15);

    Reactor drum carriage (15) contains four foot supports of groove for Glass tubing curves, the diameter of groove radian and refrigerating unit (6) is complementary, and reactor drum carriage (15) is positioned on the microwave rf generator (16);

    The charging interface (26) of one end of feed-pipe (9) and reactor drum (5) is tightly connected;

    Feed-pipe (9) passes from side pipe (11) again;

    Be fixed in then in the pump head (29) of constant flow pump (3), the other end of feed-pipe (9) is closely holed and is passed plug I (28), communicates with reactant mixing tank (1);

    The discharging interface (27) of one end of extraction line (10) and reactor drum (5) is tightly connected, and extraction line (10) passes from side pipe (11) again, and the other end of extraction line (10) is closely holed and passed plug II (30), communicates with product tripping device (7);

    Reactant mixing tank (1) is positioned on the magnetic stirring apparatus (2), places stirrer (20) in the reactant mixing tank (1), and the lower end of loading hopper (21) is also closely passed from the plug I (28) of the bottleneck of reactant mixing tank (1), communicates with reactant mixing tank (1);

    Magnetic stirring apparatus (2) is positioned on the constant flow pump (3);

    Product tripping device (7) has baiting valve (31), and product collection device (8) places on the iron stand (18) under product tripping device (7);

    Ion liquid step of described preparation and condition are;

    Can form the cation A of positively charged +Organic materials with can form electronegative negatively charged ion B -Inorganic material press A +;

    B -Mol ratio is that 1.0;

    1.0 proportioning is mixed;

    Flow in the reactant mixing tank (1) through loading hopper (21);

    Stir;

    Through in feed-pipe (9) inflow reactor (5), the flow velocity of regulating magnetic stirring apparatus (2) makes it to stir under the drive of constant flow pump (3), and the flow velocity of regulating constant flow pump (3) makes reaction mass at reactor drum (5) flowing time in is 2~

    3 minutes, and it is 60~

    70 ℃

    with the temperature of reaction that reaches in the controlling reactor (5) that the interior feeding of refrigerating unit (6) water carries out heat exchange, and reactant flows into product tripping device (7) by reactor drum (5) through extraction line (10) under the drive of constant flow pump (3);

    Static layering;

    Lower floor'"'"'s material flows into the product collection device (8) that places product tripping device (7) following, obtains the viscous liquid mixture, and using therewith, the ethyl acetate extraction of viscous liquid mixture equal volume separates 2~

    3 times;

    Collect lower floor'"'"'s liquid phase;

    After removing the solvent ethyl acetate in lower floor'"'"'s liquid phase under reduced pressure, 60~

    80 ℃

    of continuous vacuum dryings 6~

    8 hours obtain ionic liquid;

    The ionic liquid of described preparation is for having general formula;

    A +B -Compound, A in the formula +Be organic cation, B -Be inorganic anion;

    The pure form of said ionic liquid under 1 normal atmosphere has and is lower than 100 ℃

    fusing point.

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