Processing system and processing method for blocked microreactor

Abstract

A processing system and processing method for blocked microreactor. The processing system comprises an gas intake device, a flushing device, a microreactor to be processed and a plasma processing device. One end of the microreactor to be processed is connected with the gas intake device and the flushing device through a pipeline; the other end of the microreactor to be processed is connected with a waste liquid bottle through the pipeline; and the microreactor to be processed is arranged between electrodes of the plasma processing device. The present invention uses the effective reactivity of plasma and active free radicals in an excitation atmosphere to crack micro blockage in a micro channel in a short time. The method of the present invention has high flexibility and strong controllability, and can select plasma electrodes according to blocked regions to crack the blockage in a specific region.

Claims

1. A method for processing a blocked microreactor by using a processing system, wherein the processing system comprises a gas intake device, a flushing device, a microreactor to be processed and a plasma processing device, one end of the microreactor to be processed is connected with the gas intake device and the flushing device through a pipeline; an other end of the microreactor to be processed is connected with a waste liquid bottle through the pipeline; the microreactor to be processed is arranged between electrodes of the plasma processing device; a four-way valve is arranged between the microreactor to be processed and the gas intake device; and three valves of the four-way valve are respectively connected with an air cylinder, an oxygen cylinder and an argon cylinder; the gas intake device is also provided with a mass flow control meter for regulating a gas flow; and an opening of the mass flow control meter is 20-50 sccm; the plasma processing device comprises the electrodes, an AC power supply and an oscilloscope, wherein a first quartz sheet and a second quartz sheet are arranged between the electrodes and the microreactor to be processed; the electrodes are stainless steel, copper, zinc or iron electrodes, and have shapes of circular, square, triangular or rectangular; and each of the first quartz sheet and the second quartz sheet has an edge larger than edges of the electrodes by 1-2 cm, and a thickness of 1-3 mm; the processing system also comprises a monitoring device, and the monitoring device comprises a camera and a display; wherein the flushing device comprises an injection pump and a syringe, the syringe is respectively connected with a fourth valve of the four-way valve and the microreactor is connected to a three-way valve; wherein the method comprising the following steps: (1) placing the microreactor to be processed between the electrodes of the plasma processing device, and placing each of the first quartz sheet and the second quartz sheet on an upper side and a lower side of the microreactor to be processed; (2) opening the four-way valve, and adjusting the opening of the mass flow control meter, so that one or more mixed gases in the air cylinder, the oxygen cylinder and the argon cylinder enter the microreactor; (3) turning on the AC power supply and adjusting the oscilloscope, wherein an output power applied by the AC power supply is 1.5-5 W; (4) generating plasma to crack a blockage in the microreactor; (5) online observing the blockage in the microreactor in real time through the camera connected with the display, and turning off the AC power supply when the blockage is cracked; (6) starting the injection pump; collecting the cleaning liquid by the waste liquid bottle; closing the four-way valve and stopping the injection pump after the blockage in the pipeline is completely discharged; wherein the cleaning liquid is water, ethanol or acetone.

2. The method according to claim 1, wherein the display is a computer.

Description

DESCRIPTION OF DRAWINGS

(1) FIG. 1 is a schematic diagram of the present invention.

(2) In the figure: 1 air cylinder; 2 oxygen cylinder; 3 argon cylinder; 4 mass flow control meter; 5 injection pump; 6 syringe; four-way valve; 8 three-way valve; 9 electrode; 10 quartz sheet; 11 microreactor to be processed; 12 AC power supply; 13 oscilloscope; 14 computer; 15 camera; 16 waste liquid bottle; and 17 gas intake device.

(3) FIG. 2 is a current-voltage diagram collected by an oscilloscope in embodiment 1.

(4) FIG. 3 is a current-voltage diagram collected by an oscilloscope in embodiment 2.

(5) FIG. 4 is a current-voltage diagram collected by an oscilloscope in embodiment 3.

DETAILED DESCRIPTION

(6) The present invention will be specifically described below in combination with the drawings and the embodiments.

(7) As shown in FIG. 1, a processing system for a blocked microreactor in the present embodiment comprises a gas intake device 17, a flushing device, a microreactor to be processed and a plasma processing device. One end of the microreactor 11 to be processed is connected with the gas intake device and the flushing device through a pipeline; the other end of the microreactor 11 to be processed is connected with a waste liquid bottle 16 through the pipeline; and the microreactor 11 to be processed is arranged between electrodes 9 of the plasma processing device.

(8) The microreactor 11 to be processed is connected with the gas intake device through the pipeline; a four-way valve 7 is arranged between the microreactor to be processed and the gas intake device; and three valves of the four-way valve 7 are respectively connected with an air cylinder 1, an oxygen cylinder 2 and an argon cylinder 3.

(9) The gas intake device is also provided with a mass flow control meter 4 for regulating a gas flow; and the opening of the mass flow control meter 4 is 20-50 sccm.

(10) The flushing device comprises an injection pump 5 and a syringe 6; and the syringe 6 is respectively connected with a fourth valve of the four-way valve 7 and the microreactor 11 to be processed through a three-way valve 8.

(11) The plasma processing device comprises electrodes 9, an AC power supply 12 and an oscilloscope 13, and a quartz sheet 10 is arranged between the electrodes 9 and the microreactor 11 to be processed.

(12) The electrodes 9 are stainless steel, copper, zinc or iron electrodes, and have the shapes of circular, square, triangular, rectangular or other irregular patterns, and processing area is 1-100 cm.sup.2; and the quartz sheet 10 has an edge larger than the edges of the electrodes 9 by 1-2 cm, and a thickness of 1-3 mm.

(13) The processing system also comprises a monitoring device, and the monitoring device comprises a camera 15 and a display 14. The display 14 is a computer. The material of the microreactor 11 to be processed is glass, quartz, ceramic or borosilicate sand.

(14) A method for processing a blocked microreactor by using the processing system is provided. The method comprises the following steps: 1) placing the microreactor 11 to be processed between the electrodes 9 of the plasma processing device, and placing a quartz sheet 10 slightly larger than the electrodes 9 on an upper side and a lower side of the microreactor 11 to be processed respectively for dielectric barrier and microreactor protection; 2) opening the four-way valve 7, and adjusting the opening of the mass flow control meter 4, so that one or more mixed gases in the air cylinder 1, the oxygen cylinder 2 and the argon cylinder 3 enter the microreactor 11; 3) turning on the AC power supply 12; adjusting the oscilloscope 13; after the oscilloscope 13 shows stably, collecting the output power of the AC power supply 12, wherein the output power applied by the AC power supply 12 is 1.5-5 W and processing time is 3-10 min; 4) online observing the blockage situation in the microreactor 11 to be processed in real time through the camera 15 connected with the display 14, and turning off the AC power supply 12 when the blockage is basically cracked; 5) starting the injection pump 5; controlling the output quantity of the injection pump 5, wherein an output flow is 0.1-2 mL/min, and time of circulation is 3-15 min; introducing cleaning liquid inside the syringe 6 into the microreactor 11 to be processed; collecting the cleaning liquid by the waste liquid bottle 16; and closing the four-way valve 7 and the injection pump 5 after the blockage in the pipeline is completely discharged.

(15) The cleaning liquid is water, ethanol or acetone.

Embodiment 1

(16) A method for processing a blocked microreactor by using the processing system comprises the following steps: 1) placing the microreactor 11 to be processed between the electrodes 9 of the plasma processing device, and placing a quartz sheet 10 slightly larger than the electrodes 9 on an upper side and a lower side of the microreactor 11 to be processed respectively for dielectric barrier and microreactor protection; 2) opening the four-way valve 7, and adjusting the opening of the mass flow control meter 4 to be 30 sccm, so that oxygen in the oxygen cylinder 2 enters the microreactor 11; 3) turning on the AC power supply 12; adjusting the oscilloscope 13; after the oscilloscope 13 shows stably, collecting the output power of the AC power supply 12, wherein the output power applied by the AC power supply 12 is 2.09 W (as shown in FIG. 2. The output power can be obtained by integrating a region enclosed by the current-voltage diagram) and processing time is 8 min; 4) online observing the blockage situation in the microreactor 11 to be processed in real time through the camera 15 connected with the display 14, and turning off the AC power supply 12 when the blockage is basically cracked; 5) starting the injection pump 5; controlling the output quantity of the injection pump 5, wherein an output flow is 0.2 mL/min, and time of circulation is 10 min; introducing deionized water inside the syringe 6 into the microreactor 11 to be processed; collecting the waste deionized water by the waste liquid bottle 16; and closing the four-way valve 7 and the injection pump 5 after the blockage in the pipeline is completely discharged.

Embodiment 2

(17) A method for processing a blocked microreactor by using the processing system comprises the following steps: 1) placing the microreactor 11 to be processed between the electrodes 9 of the plasma processing device, and placing a quartz sheet 10 slightly larger than the electrodes 9 on an upper side and a lower side of the microreactor 11 to be processed respectively for dielectric barrier and microreactor protection; 2) opening the four-way valve 7, and adjusting the opening of the mass flow control meter 4 to be 25 sccm, so that oxygen in the oxygen cylinder 2 and argon in the argon cylinder 3 form mixed gas which enters the microreactor 11; 3) turning on the AC power supply 12; adjusting the oscilloscope 13; after the oscilloscope 13 shows stably, collecting the output power of the AC power supply 12, wherein the output power applied by the AC power supply 12 is 1.73 W (as shown in FIG. 3. The output power can be obtained by integrating a region enclosed by the current-voltage diagram) and processing time is 10 min; 4) online observing the blockage situation in the microreactor 11 to be processed in real time through the camera 15 connected with the display 14, and turning off the AC power supply 12 when the blockage is basically cracked; 5) starting the injection pump 5; controlling the output quantity of the injection pump 5, wherein an output flow is 0.2 mL/min, and time of circulation is 10 min; introducing deionized water inside the syringe 6 into the microreactor 11 to be processed; collecting the waste deionized water by the waste liquid bottle 16; and closing the four-way valve 7 and the injection pump 5 after the blockage in the pipeline is completely discharged.

Embodiment 3

(18) A method for processing a blocked microreactor by using the processing system comprises the following steps: 1) placing the microreactor 11 to be processed between the electrodes 9 of the plasma processing device, and placing a quartz sheet 10 slightly larger than the electrodes 9 on an upper side and a lower side of the microreactor 11 to be processed respectively for dielectric barrier and microreactor protection; 2) opening the four-way valve 7, and adjusting the opening of the mass flow control meter 4 to be 50 sccm, so that air in the air cylinder 1 enters the microreactor 11; 3) turning on the AC power supply 12; adjusting the oscilloscope 13; after the oscilloscope 13 shows stably, collecting the output power of the AC power supply 12, wherein the output power applied by the AC power supply 12 is 3.15 W (as shown in FIG. 4. The output power can be obtained by integrating a region enclosed by the current-voltage diagram) and processing time is 5 min; 4) online observing the blockage situation in the microreactor 11 to be processed in real time through the camera 15 connected with the display 14, and turning off the AC power supply 12 when the blockage is basically cracked; 5) starting the injection pump 5; controlling the output quantity of the injection pump 5, wherein an output flow is 1 mL/min, and time of circulation is 5 min; introducing deionized water inside the syringe 6 into the microreactor 11 to be processed; collecting the waste deionized water by the waste liquid bottle 16; and closing the four-way valve 7 and the injection pump 5 after the blockage in the pipeline is completely discharged.