CN109317070B - Preparation device and preparation method of mining ionic liquid inhibitor - Google Patents
Preparation device and preparation method of mining ionic liquid inhibitor Download PDFInfo
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- CN109317070B CN109317070B CN201811451312.9A CN201811451312A CN109317070B CN 109317070 B CN109317070 B CN 109317070B CN 201811451312 A CN201811451312 A CN 201811451312A CN 109317070 B CN109317070 B CN 109317070B
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Abstract
The invention provides a mining ionic liquid inhibitor preparation device which comprises an ionic liquid inhibitor raw material storage tank, a reaction furnace, a finished product storage tank, a water tank and a proportioning tank which are sequentially communicated through PE mining pipelines, wherein the proportioning tank is connected with the water tank through PE mining pipelines, the reaction furnace is connected with a water circulation heating and cooling device, a constant-speed stirrer is arranged on the proportioning tank, a visible window, a liquid level sensor, a temperature sensor, a time controller and an audible and visual alarm are arranged on the reaction furnace, the liquid level sensor, the pressure sensor, the temperature sensor, the time controller and the audible and visual alarm are all electrically connected with a controller, and a movable filter plate and a movable water flow cleaning device are arranged in the reaction furnace. The invention can directly prepare and configure the ionic liquid inhibitor with different concentrations required by the mine, saves economic cost for mine enterprises, has simple structure, does not need too much manual operation, and can be popularized and used.
Description
Technical Field
The invention relates to the field of coal spontaneous combustion prevention and control, in particular to a device and a method for preparing a mining ionic liquid inhibitor.
Background
The coal fire disaster not only threatens the life safety of mine staff, but also causes a great deal of coal resource waste. How to utilize effective technical means and application technology to prevent spontaneous combustion of coal is very important to ensure safety of mine staff. There are studies showing that: the ionic liquid inhibitor can destroy the active structure in the coal, can effectively inhibit spontaneous combustion of the coal, and essentially achieves the purpose of preventing and controlling spontaneous combustion of the coal. However, if the ionic liquid is sprayed directly on the surface of the coal body as a retarder, the cost is very high. Therefore, from the viewpoints of economy and practicality, it is necessary to invent an apparatus for preparing an ionic liquid retarder from raw materials.
Disclosure of Invention
Aiming at the above requirements, the invention provides the preparation device of the mining ionic liquid inhibitor, which has the advantages of exquisite structure, convenient use, good effect of preparing the ionic liquid inhibitor, economic preparation cost and popularization and application.
In order to solve the technical problems, the invention adopts the following technical scheme: the utility model provides a mining ionic liquid stopping agent preparation facilities, its characterized in that, through the raw materials storage tank, reacting furnace, finished product holding vessel and the proportioning tank of the vertical setting of PE mining pipeline intercommunication in proper order, the reacting furnace is through the mining piping connection hydrologic cycle heating cooling device of PE, the proportioning tank is through the mining piping connection of PE there is the water tank, be provided with portable filter and portable rivers belt cleaning device in the reacting furnace, install the constant speed agitator on the proportioning tank, the quantity of raw materials storage tank is a plurality of, a plurality of raw materials storage tanks are connected with the reacting furnace in parallel.
Preferably, the furnace wall of the reaction furnace is composed of two layers of steel plates, a feed inlet and a discharge outlet which penetrate through PE mining pipelines are formed in the furnace wall of the reaction furnace, an interlayer cavity is formed between the two layers of steel plates of the furnace wall, the interlayer cavity is connected with a water circulation heating and cooling device through a high-temperature water pipe, a temperature sensor and a liquid level sensor are arranged on the inner wall of the reaction furnace, and a visual window, a time controller, an audible-visual alarm and an emptying valve are sequentially arranged on the outer wall of the reaction furnace.
Preferably, the movable filter plate is horizontally arranged in the reaction furnace, a plurality of rows of filter holes are uniformly formed in the movable filter plate, fixed blades and movable blades which are mutually spliced and used for plugging the filter holes are arranged on the filter holes, the fixed blades are fixed on the filter holes, the movable blades on the same row of filter holes are fixedly connected with thin dowel bars, one ends of all the thin dowel bars are gathered together and are fixedly connected with thick dowel bars which are horizontally arranged, the thick dowel bars are connected with a switch rod through telescopic rods which are vertically arranged, one end of the switch rod penetrates out of the furnace wall of the reaction furnace, an inverted T-shaped chute is formed in the upper surface of the movable filter plate, and a connecting rod which is in sliding fit with the chute is arranged in the chute and is fixedly connected with the thick dowel bars; a plurality of movable pulleys are arranged on the periphery of the movable filter plate, and a track which is matched with the movable pulleys in an up-and-down sliding way is vertically arranged on the inner wall of the reaction furnace at the position corresponding to the movable pulleys;
the movable water flow cleaning device comprises a plurality of water inlets formed in the bottom end of the inner wall of the reaction furnace, each water inlet is connected with a flushing nozzle through a water hose, the interlayer cavity is communicated with the flushing nozzle, an electromagnetic valve for controlling the opening and closing of the flushing nozzle is arranged on each water inlet, the electromagnetic valve is electrically connected with a control switch arranged on the outer wall of the reaction furnace, a booster for increasing water pressure is arranged in the flushing nozzle, one end of a steel cable is fixedly connected with the flushing nozzle, the other end of the steel cable sequentially passes through a movable pulley and one end of a fixed pulley and one end of a rocking handle are fixedly connected, the fixed pulley is fixedly arranged at the inner top of the reaction furnace, and the rocking handle is fixedly arranged on the outer wall of the reaction furnace.
Preferably, the telescopic rod is formed by connecting a plurality of sections of rods with different diameters.
Preferably, the water circulation heating and cooling device comprises a hot water container and a cold water container, a heat exchanger is arranged between the hot water container and the cold water container, the hot water container and the cold water container are respectively connected to an interlayer cavity of the reaction furnace through high-temperature water pipelines, and automatic control valves are arranged at water outlets of the hot water container and the cold water container.
Preferably, the temperature sensor, the liquid level sensor, the time controller, the audible and visual alarm and the automatic control valve on the water circulation heating and cooling device are all electrically connected with the controller.
Preferably, the liquid level meter is all installed on raw materials storage tank, finished product holding vessel, water tank and the ratio jar lateral wall, rubber slip steamboat is all installed to raw materials storage tank, finished product holding vessel and water tank bottom, install electronic flange formula lining fluorine ball valve A, explosion-proof turbine flowmeter A and explosion-proof centrifugal pump A in proper order between raw materials storage tank and the reacting furnace, install electronic flange formula lining fluorine ball valve B, explosion-proof turbine flowmeter B and explosion-proof centrifugal pump B in proper order between reacting furnace and the finished product holding vessel, install electronic flange formula lining fluorine ball valve C, explosion-proof turbine flowmeter C and explosion-proof centrifugal pump C in proper order between finished product holding vessel and the ratio jar, install electronic flange formula lining fluorine ball valve D, explosion-proof turbine flowmeter D and explosion-proof centrifugal pump D in proper order between water tank and the ratio jar, install electronic flange formula lining fluorine ball valve E and explosion-proof turbine flowmeter E on the ratio jar export.
Preferably, the raw material storage tank is a steel lining plastic storage tank, and the material of the reaction furnace is NS333 type corrosion resistant alloy steel.
Preferably, a sealing ring is arranged at the position of the reaction furnace where the switch rod is arranged.
Preferably, the electric flange type fluorine lining ball valve adopts an LDBAAF25 type electric flange type ball valve, so that the electric control time and labor saving of a switch can be realized, and the electric flange type fluorine lining ball valve has the characteristic of explosion prevention and is suitable for mines.
Preferably, the explosion-proof turbine flowmeter adopts an LWGY-C turbine flowmeter with the advantages of high precision, long signal transmission distance and the like, and is used for strictly monitoring the flow of the ionic liquid raw material flowing through the PE pipeline.
Preferably, the explosion-proof centrifugal pump adopts a BAW-80-30 high-power centrifugal pump with the power of 100KW, has the characteristics of high flow and high lift, and provides continuous power for mixing various ionic liquid raw materials and mixing the ionic liquid and water.
Preferably, the internal pressure sensor and the internal temperature sensor on the reaction furnace use the GT25XX explosion-proof stage pressure sensor and the MFS10 pipe clamp NTC temperature sensor, and can accurately measure the pressure and the temperature in the reaction furnace when raw materials react.
Preferably, the time controller on the reaction furnace uses an Enlaields industrial timer and has various output control functions of intelligent timing, timing and alarming.
Preferably, the audible and visual alarm on the reaction furnace uses a Hangya YS-BBJ type explosion-proof audible and visual alarm, and the high boron silicon steel glass lampshade with special process treatment has good explosion-proof performance and is suitable for mines.
Preferably, a water inlet switch of the water flow cleaning device on the reaction furnace uses a BZA1-5 mining flameproof control button, and can be used in an environment with methane and coal dust explosive gas mixture.
Preferably, the liquid level sensor on the reaction furnace uses a mining GUY10 liquid level sensor and is matched with a warning device to send out a warning signal when the liquid level exceeds or falls below a designated position.
Preferably, a process for preparing [ BMIM][BF 4 ]A method of ionic liquid retarder, comprising the steps of:
firstly, respectively storing N-methylimidazole, bromo-N-butane, ethyl acetate and sodium fluoborate solution in four raw material storage tanks, injecting two raw materials of the two ionic liquid inhibitor into a reaction furnace along a mining PE pipeline under the action of an explosion-proof centrifugal pump, and accurately controlling the proportion of the two raw materials through an explosion-proof turbine flowmeter in the process to ensure that the ratio of the two raw materials is 1:1.1, adding the mixture into a reaction furnace;
secondly, enabling high temperature water to flow out of a hot water container of the water circulation heating and cooling device, enabling the high temperature water to enter an interlayer cavity of the reaction furnace through a high temperature water pipeline, raising the reaction temperature to 80 ℃, starting timing by a time controller, and finishing the reaction after 0.5 h; the movable filter plate is in a closed state in the reaction process, meanwhile, the temperature of the reaction is monitored at any time through a temperature sensor, once the temperature is abnormal, a controller sends a command signal to an audible and visual alarm, after the reaction is finished, the controller controls a water circulation heating and cooling device to convert heating into cooling, low-temperature water flows out of a cold water container and enters an interlayer cavity of a reaction furnace, so that a product after the reaction is cooled, and the temperature sensor is continuously monitored at the moment, so that the temperature in the reaction furnace is strictly controlled;
thirdly, after the reaction furnace is cooled to room temperature, ethyl acetate is added into the reaction furnace for a plurality of times, the reaction product in the second step is washed for a plurality of times, repeated washing is carried out for a plurality of times, and after standing for half an hour, an intermediate product [ BMIM ] Br which is positioned on the movable filter plate and is obtained after the reaction of N-methylimidazole and bromo-N-butane and residual ethyl acetate at the bottom of the reaction furnace are obtained, wherein the residual ethyl acetate also contains impurities and byproducts generated in the second step of reaction, then the movable filter plate is closed, an emptying valve is opened to discharge unreacted ethyl acetate through the emptying valve, and then a movable water flow cleaning device is started by opening an electromagnetic valve to clean the residual impurities;
fourth, adding sodium fluoborate solution and [ BMIM ] in the reaction furnace]Br is 1:1.2, then reacts for 0.5h at 45 ℃, then stands for 0.5h, at the moment, the layering liquid level of the reactant is observed through a visual window, the movable filter plate is opened after the reactant is moved to a proper position through a movable rocker, the movable filter plate is closed after separation is finished, and a target product [ BMIM (b-Me) on the movable filter plate is obtained at the moment][BF 4 ]The ionic liquid and the byproduct sodium bromide at the bottom of the reaction furnace are opened, and an emptying valve is opened (the byproduct sodium bromide is discharged, and the target product [ BMIM ]][BF 4 ]The ionic liquid is sucked into a finished product storage tank for standby through an explosion-proof centrifugal pump;
fifth step, [ BMIM ]][BF 4 ]The ionic liquid and the water tank respectively enter the proportioning tank through the explosion-proof centrifugal pump C and the explosion-proof centrifugal pump D, are uniformly mixed after being stirred by the constant-speed stirrer, and the flow rates of the water and the ionic liquid can be regulated through the explosion-proof turbine flowmeter C and the explosion-proof turbine flowmeter D in the process, so that different concentrations [ BMIM ] can be realized][BF 4 ]The ionic liquid inhibitor is proportioned.
Compared with the prior art, the invention has the following advantages:
1. the invention has the advantages of exquisite structure, high automation degree, high efficiency of preparing the ion inhibitor and preparation of [ BMIM ]][BF 4 ]The ionic liquid inhibitor has good inhibition effect, simple and convenient installation and popularization and application.
2. The movable filter plate designed by the invention is provided with a plurality of filter holes, a blade for blocking the filter holes is divided into two halves, one half is fixed on the filter holes, the other half is fixed on the thin dowel bar, a plurality of thin dowel bars are assembled and fixed on the thick dowel bar, the thick dowel bar is connected with a switch bar by a telescopic rod, the switch bar is operated manually to realize the opening and closing of the filter holes, and the movable filter plate is also moved up and down by arranging a track and a movable pulley, so that the effect of separating byproducts and target products can be achieved, and the space ratio of the byproducts and the target products in the reaction furnace can be adjusted at will.
3. The movable water flow cleaning device designed by the invention has the advantages that the flushing nozzle in the movable water flow cleaning device is fixed on the movable pulley, the water inlet is formed in the movable pulley, the water pipe is connected to the water inlet, one end of the water pipe is connected with the flushing nozzle, the other end of the water pipe is connected with the cavity between the two layers of furnace walls of the reaction furnace, the movable water flow cleaning device can directly use the high temperature water in the cavity between the two layers of furnace walls of the reaction furnace, a pipeline and the water inlet which are connected with an external flushing water source are not required to be independently formed, the movable water flow cleaning device is convenient and rapid, and can move up and down along with the movable filter plate, so that the flushing effect is ensured at any time.
4. The invention designs a water circulation heating and cooling device, which is connected with a hot water container and a cold water container through a heat exchanger, so that the water circulation heating and cooling device can rapidly realize the heating and cooling circulation of water, high temperature water provided by the water circulation heating and cooling device is injected into a cavity between two layers of furnace walls of a reaction furnace, the reaction temperature of the reaction furnace can be controlled, a water source can be provided for a movable water flow cleaning device, and the water circulation heating and cooling device is controlled by a PC end controller, so that the automatic and accurate operation is realized.
5. The invention is provided with a plurality of raw material storage tanks for storing different raw materials, and each section of pipeline is provided with the electric flange type fluorine lining ball valve, the explosion-proof turbine flowmeter and the explosion-proof centrifugal pump, so that the flow of liquid flowing through the pipeline can be accurately controlled, the electric control is realized, and the invention also has an explosion-proof function, so that the liquid conveying process is safe and controllable.
6. The invention is provided with the proportioning tank, can prepare the ionic liquid inhibitor with different concentrations according to actual demands, can effectively increase the utilization rate of the ionic liquid inhibitor and reduce the cost.
The invention is described in further detail below with reference to the drawings and examples.
Drawings
FIG. 1 is a schematic structural view of a production apparatus of the present invention.
Fig. 2 is a schematic view of the connection structure of the thin dowel bar, the movable blade and the fixed blade in the manufacturing apparatus of the present invention.
Fig. 3 is a schematic view of the connection structure of the thick dowel bar and the telescopic bar in the manufacturing apparatus of the present invention.
FIG. 4 is a schematic diagram showing the connection structure of the mobile filter plate and the mobile water flow cleaning device in the production apparatus of the present invention.
Fig. 5 is a schematic diagram of the connection structure of the movable filter plate and the thick force transmission rod in the preparation device of the invention.
Reference numerals illustrate:
1-a raw material storage tank; 2-a liquid level meter; 3-rubber sliding small wheels;
4-an electric flange type fluorine lined ball valve; 5-an explosion-proof turbine flowmeter; 6-explosion-proof centrifugal pump;
7-PE mining pipelines; 8, a reaction furnace; 9—a visual window;
10-mobile filter plate; 11-a mobile water flow cleaning device; 12-moving blades;
13-a thin dowel bar; 14-rocking handle; 15-a switch lever;
16-a control switch; 17-thick dowel bars; 18-a telescopic rod;
19-a water circulation heating and cooling device; 20-a blow-off valve; 21-a high-temperature water pipe;
22-a cold water container; 23-a finished product storage tank; 24-water tank;
25-constant speed stirrer; 26-proportioning tank; 27-controller.
28-a hot water container; 29-an electric flange type fluorine lining ball valve B; 30—an explosion-proof turbine flowmeter B;
31-a mobile pulley; 32-explosion-proof centrifugal pump B; 33-an electric flange type fluorine lining ball valve C;
34-flushing the spray head; 35-an explosion-proof turbine flowmeter C36-a fixed pulley;
37-explosion-proof centrifugal pump C; 38-an electric flange type fluorine lining ball valve D; 39—an explosion-proof turbine flowmeter D;
40-explosion-proof centrifugal pump D; 41-an electric flange type fluorine lining ball valve E; 42-explosion-proof turbine flowmeter E;
43-wire rope; 44-a connecting rod; 45-fixed blades.
Detailed Description
As shown in fig. 1 to 5, the invention comprises a raw material storage tank 1, a reaction furnace 8, a finished product storage tank 23 and a proportioning tank 26 which are sequentially communicated through a PE mining pipeline 7, wherein the reaction furnace 8 is connected with a water circulation heating and cooling device 19 through the PE mining pipeline 7, the proportioning tank 26 is connected with a water tank 24 through the PE mining pipeline 7, a movable filter plate 10 and a movable water flow cleaning device 11 are arranged in the reaction furnace 8, a constant-speed stirrer 25 is arranged on the proportioning tank 26, the number of the raw material storage tanks 1 is four, the four raw material storage tanks 1 are connected with the reaction furnace 8 in parallel, different raw materials for preparing ionic liquid stopping agents are respectively filled in the four raw material storage tanks 1, raw material reactions occur in the reaction furnace 8, the prepared ionic liquid stopping agents are stored in the finished product storage tank 23, and the proportioning tank 26 can prepare ionic liquid stopping agents with different concentrations for coal fires.
In this embodiment, the oven of reaction furnace 8 comprises two-layer steel sheet, offer feed inlet and the discharge gate that pass the mining pipeline 7 of PE on the reaction furnace 8 oven, form the intermediate layer cavity between the two-layer steel sheet of oven, the intermediate layer cavity is connected with hydrologic cycle heating cooling device 19 through high temperature water pipe 21, be provided with temperature sensor and liquid level sensor on the reaction furnace 8 inner wall, be provided with visual window 9, time control appearance, audible-visual annunciator and blow valve 20 on the reaction furnace 8 outer wall in proper order.
In this embodiment, the movable filter plate 10 is horizontally disposed in the reaction furnace 8, a plurality of rows of filter holes are uniformly formed on the movable filter plate 10, fixed blades 45 and movable blades 12 for blocking the filter holes are disposed on the filter holes in a mutually spliced manner, the fixed blades 45 are fixed on the filter holes, the movable blades 12 disposed on the same row of filter holes 12 are fixedly connected with the thin dowel bars 13, one ends of all the thin dowel bars 13 are gathered together and are fixedly connected with the thick dowel bars 17 disposed horizontally, the thick dowel bars 17 are connected with the switch bars 15 through the telescopic rods 18 disposed vertically, one ends of the switch bars 15 penetrate out of the furnace wall of the reaction furnace 8, an inverted-T-shaped chute is formed on the upper surface of the movable filter plate 10, a connecting rod 44 in sliding fit with the chute is disposed in the chute, and the connecting rod 44 is fixedly connected with the thick dowel bars 17; a plurality of movable pulleys 31 are arranged on the periphery of the movable filter plate 10, the periphery of the movable filter plate 10 is clung to the inner wall of the reaction furnace 8, and a track which is vertically arranged on the inner wall of the reaction furnace 8 and corresponds to the movable pulleys 31 and is matched with the movable pulleys 31 in an up-down sliding way is arranged on the inner wall of the reaction furnace 8.
In this embodiment, the movable water flow cleaning device 11 includes a plurality of water inlets formed at the bottom end of the inner wall of the reaction furnace 8, each water inlet is connected with a flushing nozzle 34 through a water hose, so that the interlayer cavity is communicated with the flushing nozzle 34, an electromagnetic valve for controlling the opening and closing of the flushing nozzle 34 is disposed on each water inlet, the electromagnetic valves are controlled by a control switch 16 disposed on the outer wall of the reaction furnace, a booster for increasing water pressure is disposed in the flushing nozzle 34, one end of a steel cable 43 is fixedly connected with the flushing nozzle 34, the other end of the steel cable 43 sequentially passes through a movable pulley 31 and a fixed pulley 36 to be fixedly connected with one end of the rocking handle 14, and after the steel cable 43 connected to all the flushing nozzles 34 passes through the movable pulley 31 to be converged, passes through the fixed pulley 36 to pass through the furnace wall of the reaction furnace 8 to be fixed on the rocking handle 14, and the rocking handle 14 is rocked, so that the movable filter plate 10 and the flushing nozzle 34 can be pulled to move up and down. The fixed pulley 36 is fixedly arranged at the inner top of the reaction furnace 8, and the rocking handle 14 is fixedly arranged on the outer wall of the reaction furnace 8.
In this embodiment, the flexible water pipe is a corrosion-resistant flexible pipe.
In this embodiment, the rocking handle 14, the switch lever 15 and the electromagnetic valve are all arranged on the outer wall of the reaction furnace 8.
In this embodiment, the water circulation heating and cooling device 19 includes a hot water container 28 and a cold water container 22, a heat exchanger is installed between the hot water container 28 and the cold water container 22, the hot water container 28 and the cold water container 22 are respectively connected to the interlayer cavity of the reaction furnace 8 through a high-temperature water pipeline 21, and water outlets of the hot water container 28 and the cold water container 22 are respectively provided with an automatic control valve.
In this embodiment, the temperature sensor, the liquid level sensor, the time controller, the audible and visual alarm and the automatic control valve on the water circulation heating and cooling device 19 are all electrically connected with the controller 27.
In this embodiment, liquid level table 2 is all installed on raw materials storage tank 1, finished product holding vessel 23, water tank 24 and the ratio jar 26 lateral wall, rubber slip steamboat 3 is all installed to raw materials storage tank 1, finished product holding vessel 23 and water tank 24 bottom, install electronic flange formula lining fluorine ball valve A4, explosion-proof turbine flowmeter A5 and explosion-proof centrifugal pump A6 in proper order between raw materials storage tank 1 and the reacting furnace 8, install electronic flange formula lining fluorine ball valve B29, explosion-proof turbine flowmeter B30 and explosion-proof centrifugal pump B32 in proper order between reacting furnace 8 and the finished product holding vessel 23, install electronic flange formula lining fluorine ball valve C33, explosion-proof turbine flowmeter C35 and explosion-proof centrifugal pump C37 in proper order between finished product holding vessel 23 and the ratio jar 26, install electronic flange formula lining fluorine ball valve D38, explosion-proof turbine flowmeter D39 and explosion-proof centrifugal pump D40 in proper order between water tank 24 and the ratio jar 26, offer the ratio jar export on the ratio jar export, install electronic flange formula lining fluorine ball valve E41 and explosion-proof turbine flowmeter E42 in proper order.
In this embodiment, the raw material storage tank 1 is a steel lining plastic storage tank, and the reaction furnace 8 is made of NS333 type corrosion resistant alloy steel.
In the embodiment, the electric flange type fluorine lining ball valve 4 adopts an LDBAAF25 type electric flange type ball valve, can realize electric control, has the characteristic of explosion prevention, and is suitable for mines.
In this embodiment, the explosion-proof turbine flowmeter 5 adopts an LWGY-C turbine flowmeter having advantages of high accuracy, long signal transmission distance, and the like, and is used for strictly monitoring the flow rate of the ionic liquid raw material flowing through the PE pipeline.
In the embodiment, the explosion-proof centrifugal pump 6 adopts a BAW-80-30 high-power centrifugal pump with the power of 100KW, has the characteristics of high flow and high lift, and provides continuous power for mixing various ionic liquid raw materials and mixing the ionic liquid and water.
In this embodiment, the pressure sensor and the temperature sensor in the reaction furnace 8 use the GT25XX explosion-proof stage pressure sensor and the MFS10 pipe clamp NTC temperature sensor, and can accurately measure the pressure and the temperature in the reaction furnace when the raw materials react.
In this embodiment, the time controller on the reaction furnace uses an Enlaields type industrial timer, and has multiple output control functions of intelligent timing, timing and alarming.
In the embodiment, the audible and visual alarm on the reaction furnace uses the Hangya YS-BBJ type explosion-proof audible and visual alarm, and the high boron silicon steel glass lampshade with special process treatment has good explosion-proof performance and is suitable for mines.
In the embodiment, a water inlet switch of the water flow cleaning device on the reaction furnace uses a BZA1-5 mining flameproof control button, and can be used in an environment with methane and coal dust explosive gas mixture.
In the embodiment, the liquid level sensor on the reaction furnace uses a mining GUY10 liquid level sensor, and is matched with the warning device to send out a warning signal when the liquid level exceeds or falls below a designated position.
In this embodiment, the constant-speed stirrer is a blade type corrosion-resistant constant-speed stirrer.
The embodiment also provides the preparation of [ BMIM ] by using the preparation device][BF 4 ]A method of ionic liquid stopping agents, the method comprising the steps of:
firstly, respectively storing N-methylimidazole, bromo-N-butane, ethyl acetate and sodium fluoroborate solution in four raw material storage tanks 1, injecting two raw materials of the two ionic liquid inhibitor into a reaction furnace 8 along a mining PE pipeline 7 under the action of an explosion-proof centrifugal pump 6, and accurately controlling the proportion of the two raw materials through an explosion-proof turbine flowmeter 5 in the process to ensure that the two raw materials are mixed according to the proportion of 1:1.1 in the reaction furnace 8;
secondly, enabling high-temperature water to flow out of a hot water container 28 of the water circulation heating and cooling device 22, enabling the high-temperature water to enter an interlayer cavity of the reaction furnace 8 through a high-temperature water pipeline 21, raising the reaction temperature to 80 ℃, starting timing by a time controller, finishing the reaction after 0.5h (in the process, the movable filter plate 10 is in a closed state, monitoring the reaction temperature at all times through a temperature sensor, and sending a command signal to an audible and visual alarm by the controller 27 once the temperature is abnormal), after finishing the reaction, controlling the water circulation heating and cooling device 22 to convert heating into cooling by the controller 27, enabling low-temperature water to flow out of the cold water container 22 into the interlayer cavity of the reaction furnace 8, enabling a product after the reaction to be cooled, continuously monitoring the temperature sensor, and strictly controlling the temperature in the reaction furnace 8;
thirdly, after the reaction furnace 8 is cooled to room temperature, ethyl acetate is added into the reaction furnace 8 for a plurality of times, the reaction product in the second step is washed for a plurality of times, repeated washing is carried out for a plurality of times, after standing for half an hour, an intermediate product [ BMIM ] Br which is positioned on the movable filter plate 10 and is obtained after the reaction of N-methylimidazole and bromo-N-butane and residual ethyl acetate at the bottom of the reaction furnace 8 are obtained, the residual ethyl acetate also contains impurities and byproducts generated in the second step of reaction, then the movable filter plate 10 is closed again, an emptying valve 20 is opened to discharge unreacted ethyl acetate through the emptying valve 20, and then an electromagnetic valve is opened to start a movable water flow cleaning device 11 to clean the residual impurities;
fourthly, adding sodium fluoborate solution, adding the sodium fluoborate solution and [ BMIM ] in the reaction furnace]Br in a mass ratio of 1:1.2, then reacting at 45 ℃ for 0.5h, standing for 0.5h, observing the layered liquid level of the reactant through a visual window 9, moving to a proper position through a moving rocker 14, opening the movable filter plate 10, closing the movable filter plate 10 after separation, and obtaining a target product [ BMIM ] on the movable filter plate 10][BF 4 ]The ionic liquid and the byproduct sodium bromide at the bottom of the reaction furnace 8 are discharged by opening the vent valve 20, and the target product is producedObject [ BMIM ]][BF 4 ]The ionic liquid is sucked into a finished product storage tank 23 for standby through an explosion-proof centrifugal pump 6.
Fifth step, [ BMIM ]][BF 4 ]The ionic liquid and the water tank 24 respectively enter the proportioning tank 26 through the explosion-proof centrifugal pump C37 and the explosion-proof centrifugal pump D40, are uniformly mixed after being stirred by the constant-speed stirrer 25, and the flow rates of the water and the ionic liquid can be regulated through the explosion-proof turbine flowmeter C35 and the explosion-proof turbine flowmeter D39 in the process, so that the proportioning work of the ionic liquid stopping agents with different concentrations is realized.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (7)
1. The preparation device of the mining ionic liquid inhibitor is characterized by comprising a raw material storage tank (1), a reaction furnace (8), a finished product storage tank (23) and a proportioning tank (26) which are sequentially communicated through a PE mining pipeline (7), wherein the reaction furnace (8) is connected with a water circulation heating and cooling device (19) through the PE mining pipeline (7), the proportioning tank (26) is connected with a water tank (24) through the PE mining pipeline (7), a movable filter plate (10) and a movable water flow cleaning device (11) are arranged in the reaction furnace (8), constant-speed stirrers (25) are arranged on the proportioning tank (26), the raw material storage tanks (1) are multiple, and the raw material storage tanks (1) are connected with the reaction furnace (8) in parallel; the furnace wall of the reaction furnace (8) consists of two layers of steel plates, an interlayer cavity is formed between the two layers of steel plates of the furnace wall, and the interlayer cavity is connected with a water circulation heating and cooling device (19) through a high-temperature water pipe (21);
the movable filter plates (10) are horizontally arranged in the reaction furnace (8), a plurality of rows of filter holes are uniformly formed in the movable filter plates (10), fixed blades (45) and movable blades (12) which are mutually spliced and used for blocking the filter holes are arranged on the filter holes, the fixed blades (45) are fixed on the filter holes, the movable blades (12) which are positioned on the same row of filter holes are fixedly connected with the thin dowel bars (13), one ends of all the thin dowel bars (13) are gathered together and are fixedly connected with the thick dowel bars (17) which are horizontally arranged, the thick dowel bars (17) are connected with the switch rods (15) through telescopic rods (18) which are vertically arranged, one ends of the switch rods (15) penetrate out of the furnace wall of the reaction furnace (8), inverted T-shaped sliding grooves are formed in the upper surfaces of the movable filter plates (10), connecting rods (44) which are in sliding fit with the sliding grooves are arranged in the sliding grooves, and the connecting rods (44) are fixedly connected with the thick dowel bars (17); a plurality of movable pulleys (31) are arranged on the periphery of the movable filter plate (10), and a track which is matched with the movable pulleys (31) in an up-down sliding way is vertically arranged on the inner wall of the reaction furnace (8) at the position corresponding to the movable pulleys (31);
the movable water flow cleaning device (11) comprises a plurality of water inlets formed in the bottom end of the inner wall of the reaction furnace (8), each water inlet is connected with a flushing nozzle (34) through a water hose, the interlayer cavity is communicated with the flushing nozzle (34), an electromagnetic valve for controlling the flushing nozzle (34) to open and close is arranged on each water inlet, the electromagnetic valve is electrically connected with a control switch (16) arranged on the outer wall of the reaction furnace, a booster for increasing water pressure is arranged in the flushing nozzle (34), one end of a steel cable (43) is fixedly connected with the flushing nozzle (34), the other end of the steel cable (43) sequentially penetrates through a movable pulley (31) and a fixed pulley (36) to be fixedly connected with one end of a rocking handle (14), and the fixed pulley (36) is fixedly arranged at the inner top of the reaction furnace (8) and the rocking handle (14) is fixedly arranged on the outer wall of the reaction furnace (8);
the water circulation heating and cooling device (19) comprises a hot water container (28) and a cold water container (22), a heat exchanger is arranged between the hot water container (28) and the cold water container (22), the hot water container (28) and the cold water container (22) are respectively connected to an interlayer cavity of the reaction furnace (8) through a high-temperature water pipe (21), and automatic control valves are arranged at water outlets of the hot water container (28) and the cold water container (22).
2. The mining ionic liquid inhibitor preparation device according to claim 1, wherein the furnace wall of the reaction furnace (8) is composed of two layers of steel plates, a feed inlet and a discharge outlet which penetrate through a PE mining pipeline (7) are formed in the furnace wall of the reaction furnace (8), an interlayer cavity is formed between the two layers of steel plates of the furnace wall, the interlayer cavity is connected with a water circulation heating and cooling device (19) through a high-temperature water pipe (21), a temperature sensor and a liquid level sensor are arranged on the inner wall of the reaction furnace (8), and a visual window (9), a time controller, an audible-visual alarm and an emptying valve (20) are sequentially arranged on the outer wall of the reaction furnace (8).
3. The mining ionic liquid inhibitor preparation device according to claim 2, wherein the temperature sensor, the liquid level sensor, the time control instrument, the audible and visual alarm and the automatic control valve on the water circulation heating and cooling device (19) are electrically connected with the controller (27).
4. The mining ionic liquid inhibitor preparation device according to claim 1, wherein the side walls of the raw material storage tank (1), the finished product storage tank (23), the water tank (24) and the proportioning tank (26) are respectively provided with a liquid level meter (2), the bottoms of the raw material storage tank (1), the finished product storage tank (23) and the water tank (24) are respectively provided with a rubber sliding small wheel (3), an electric flange type fluorine lining ball valve A (4), an explosion-proof turbine flowmeter A (5) and an explosion-proof centrifugal pump A (6) are sequentially arranged between the raw material storage tank (1) and the reaction furnace (8), an electric flange type fluorine lining ball valve B (29), an explosion-proof turbine flowmeter B (30) and an explosion-proof centrifugal pump B (32) are sequentially arranged between the reaction furnace (8) and the finished product storage tank (23), an electric flange type fluorine lining ball valve C (33), an explosion-proof turbine flowmeter C (35) and an explosion-proof centrifugal pump C (37) are sequentially arranged between the finished product storage tank (23) and the proportioning tank (26), an electric flange type fluorine lining ball valve C (38), an explosion-proof turbine flowmeter D (39) and an explosion-proof centrifugal pump D (40) are sequentially arranged between the water tank (24) and the proportioning tank (26), an electric flange type fluorine lining ball valve E (41) and an explosion-proof turbine flowmeter E (42) are arranged on the outlet of the proportioning tank.
5. The mining ionic liquid inhibitor preparation device according to claim 1, wherein the raw material storage tank (1) is a steel lining plastic storage tank, and the reaction furnace (8) is made of NS333 type corrosion-resistant alloy steel.
6. The mining ionic liquid inhibitor preparation device according to claim 1, wherein a sealing ring is arranged at the position of the reaction furnace (8) where the switch rod (15) is arranged.
7. Preparation [ BMIM ]][BF 4 ]The method for preparing the ionic liquid inhibitor is characterized by adopting the mining ionic liquid inhibitor preparation device as claimed in claim 4, and comprises the following steps:
firstly, respectively storing N-methylimidazole, bromo-N-butane, ethyl acetate and sodium fluoroborate solution in four raw material storage tanks (1), injecting two raw materials of the two ionic liquid inhibitor into a reaction furnace (8) along a mining PE pipeline (7) under the action of an explosion-proof centrifugal pump A (6), and accurately controlling the proportion of the two raw materials through an explosion-proof turbine flowmeter A (5) in the process to ensure that the two raw materials are mixed according to the proportion of 1:1.1 mass ratio is added into a reaction furnace (8);
secondly, enabling high temperature water to flow out of a hot water container (28) of the water circulation heating and cooling device (19), enabling the high temperature water to enter an interlayer cavity of the reaction furnace (8) through a high temperature water pipe (21), raising the reaction temperature to 80 ℃, starting timing by a time controller, and finishing the reaction after 0.5 h; the movable filter plate (10) is in a closed state in the reaction process, meanwhile, the temperature of the reaction is monitored at any time through a temperature sensor, once the temperature is abnormal, a controller (27) can send a command signal to an audible and visual alarm, after the reaction is finished, the controller (27) controls a water circulation heating and cooling device (19) to convert heating into cooling, low-temperature water flows out of a cold water container (22) and enters an interlayer cavity of the reaction furnace (8), so that a product after the reaction is cooled, and the temperature sensor is continuously monitored at the moment, so that the temperature in the reaction furnace (8) is strictly controlled;
thirdly, after the reaction furnace (8) is cooled to room temperature, ethyl acetate is added into the reaction furnace (8) for a plurality of times, the reaction product in the second step is washed for a plurality of times, repeated washing is carried out for a plurality of times, after standing for half an hour, an intermediate product [ BMIM ] Br which is positioned on the movable filter plate (10) and is obtained after N-methylimidazole and bromo-N-butane react and residual ethyl acetate at the bottom of the reaction furnace (8) are obtained, the residual ethyl acetate also contains impurities and byproducts generated in the second step, then the movable filter plate (10) is closed, an emptying valve (20) is opened to discharge unreacted ethyl acetate through the emptying valve (20), and then an electromagnetic valve is opened to start a movable water flow cleaning device (11) to clean the residual impurities;
fourth, adding sodium fluoborate solution and [ BMIM ] in the reaction furnace]Br in a mass ratio of 1:1.2, then reacting for 0.5h at 45 ℃ and standing for 0.5h, observing the layering liquid level of the reactant through a visual window (9), moving to a proper position through a moving rocker (14), opening a movable filter plate (10), closing the movable filter plate (10) after separation is completed, and obtaining a target product [ BMIM ] on the movable filter plate (10)][BF 4 ]The ionic liquid and the byproduct sodium bromide at the bottom of the reaction furnace (8) are discharged by opening the vent valve (20), and the target product [ BMIM ]][BF 4 ]The ionic liquid is sucked into a finished product storage tank (23) for standby through an explosion-proof centrifugal pump B (32);
fifth step, [ BMIM ]][BF 4 ]The ionic liquid and the water in the water tank (24) respectively enter the proportioning tank (26) through the explosion-proof centrifugal pump C (37) and the explosion-proof centrifugal pump D (40), are uniformly mixed after being stirred by the constant-speed stirrer (25), and the flow rates of the water and the ionic liquid can be regulated through the explosion-proof turbine flowmeter C (35) and the explosion-proof turbine flowmeter D (39) in the process so as toThis achieves different concentrations [ BMIM ]][BF 4 ]The ionic liquid inhibitor is proportioned.
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| CN1857767A (en) * | 2005-11-02 | 2006-11-08 | 中国科学院过程工程研究所 | Multifunctional reactor for preparing ionic liquid |
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| CN209438577U (en) * | 2018-11-30 | 2019-09-27 | 西安科技大学 | A kind of mining ionic liquid retardant preparation facilities |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| FR2994430B1 (en) * | 2012-08-10 | 2014-12-19 | Arkema France | PROCESS FOR PRODUCING DIFLUOROMETHANE |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1857767A (en) * | 2005-11-02 | 2006-11-08 | 中国科学院过程工程研究所 | Multifunctional reactor for preparing ionic liquid |
| CN1939953A (en) * | 2006-09-26 | 2007-04-04 | 天津大学 | Microwave synthesis for producing polyketone ionic liquid |
| CN107376808A (en) * | 2017-08-17 | 2017-11-24 | 东莞市盛奇智能设备科技有限公司 | A kind of reactor of recirculated water cleaning |
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