CN117358179A - Liquid sample aeration strong oxidation device and use method - Google Patents

Liquid sample aeration strong oxidation device and use method Download PDF

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Publication number
CN117358179A
CN117358179A CN202311158987.5A CN202311158987A CN117358179A CN 117358179 A CN117358179 A CN 117358179A CN 202311158987 A CN202311158987 A CN 202311158987A CN 117358179 A CN117358179 A CN 117358179A
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China
Prior art keywords
aeration
oxidation
bottle
air
tube
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CN202311158987.5A
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Chinese (zh)
Inventor
李庆
陈源正
陈秀
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Fudan University
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Fudan University
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Priority to CN202311158987.5A priority Critical patent/CN117358179A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J19/088Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4044Concentrating samples by chemical techniques; Digestion; Chemical decomposition
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0894Processes carried out in the presence of a plasma

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Toxicology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Treatment Of Water By Oxidation Or Reduction (AREA)

Abstract

The invention belongs to the field of experimental sample oxidation, and particularly relates to a liquid sample aeration strong oxidation device and a use method thereof. The device of the invention comprises: the device comprises an air pump, an air purifying device, an aeration oxidation pipe, a gas cylinder, a high-voltage direct-current power supply and a reflux condensation pipe; the aeration oxidation tube is fixed in the aeration bottle, the lower part of the inner side of the aeration oxidation tube and the bottom of the outer side of the aeration bottle are respectively provided with metal electrodes, and the two metal electrodes are connected with a high-voltage direct current power supply; clean air is sent into the aeration oxidation tube through the air pump and the air purifying device, and enters the liquid sample through the through hole at the bottom of the tube; plasma discharge is formed between the two metal electrodes, oxygen in the air is oxidized, active substances such as free radicals, ozone and the like are generated in the plasma discharge process, and dissolved components and suspended matters in the solution are subjected to strong oxidation; the reflux condenser tube cools and refluxes the volatilized solvent in the sample to the vented bottle. The device has a simple structure, is convenient to operate, and can oxidize liquid samples to different degrees by changing the power-on time.

Description

Liquid sample aeration strong oxidation device and use method
Technical Field
The invention belongs to the field of experimental sample oxidation, and particularly relates to an aeration oxidation device and a use method thereof.
Background
In order to obtain samples with different oxidation degrees, the conventional chemical oxidation method such as hydrogen peroxide and other strong oxidants have limited oxidation effect on metals and introduce impurities, so that a method for efficiently oxidizing without introducing impurities is needed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a liquid sample aeration strong oxidation device capable of oxidizing a sample conveniently and efficiently without introducing impurities and a use method thereof.
The invention provides a liquid sample aeration strong oxidation device, which comprises: the air pump 1, the air purifying device 2, the aeration oxidation pipe 3, the aeration bottle 5, the high-voltage direct-current power supply 10 and the reflux condensation pipe 13; wherein:
the air pump 1 is used for providing an air source; specifically, an air compressor or a fan can be adopted;
the inlet of the air purifying device 2 is connected with the air pump 1 and is used for purifying the air provided by the air pump; including removal of organics, water vapor, particulates, and the like; specifically, the purification device takes activated carbon or molecular sieve as purification material;
the aeration oxidation tube 3 is cylindrical, the side surface of the upper part is provided with an air inlet 4, the air inlet 4 is connected with the air outlet of the air purification device 2, and purified gas is used as a gas source for aeration; the whole of the aeration oxidation tube 3 is arranged in the aeration bottle 5, and the upper part of the oxidation tube is fixed through a through hole on the aeration bottle cap 12; the bottom of the inner side of the lower part of the aeration oxidation tube 3 is provided with a metal electrode 7, the bottom of the aeration oxidation tube 3 is provided with a plurality of small through holes 8 in annular layout, so that aeration entering the aeration oxidation tube 3 uniformly enters a sample to be oxidized, oxygen is provided for ozone generated in the plasma discharge process, and meanwhile, the sample is uniformly mixed and oxidized; the inner diameter of the aeration oxidation tube is 1-3 mm, the length of the aeration oxidation tube is 120-150 mm, and the length of the aeration oxidation tube is slightly larger than the height of the ventilation bottle;
the aeration bottle 5 is used for placing a sample 6 to be oxidized; the lower end part of the aeration oxidation tube 3 is arranged in a sample 6 to be oxidized; a metal electrode 9 is arranged outside the through hole 8 at the bottom of the ventilation bottle 5;
the two poles of the high-voltage direct current power supply 10 are respectively connected with a metal electrode 7 at the bottom of the inner side of the aeration oxidation tube 3 and a metal electrode 9 at the outer side of the bottom of the aeration bottle; the high-voltage direct current power supply 10 causes ion discharge between the two metal electrodes, generates active substances such as free radicals and ozone, and performs strong oxidation on dissolved components and suspended matters in the solution.
The invention can adjust the electric field between the two metal electrodes by changing the distance between the metal electrode 7 at the lower part of the aeration oxidation tube and the metal electrode 9 at the bottom of the aeration bottle; the distance between the two is adjustable within the range of 1.5-3.5 mm;
the side of the ventilation bottle 5 is provided with a ventilation exhaust port 11, and the reflux condenser pipe 13 is connected with the ventilation exhaust port 11; the reflux condenser 13 is a serpentine, spherical or straight condenser; since a large amount of heat is also generated in the plasma discharge process, the solvent in the liquid sample volatilizes, and the reflux condenser tube 13 cools and returns the volatilized solvent in the liquid sample to the vent bottle 5, so that the volume of the oxidized sample solvent is ensured to be unchanged.
The operation flow of the liquid sample aeration strong oxidation device is as follows:
step 1: filling 10-30 ml of liquid sample 6 to be oxidized into a gas passing bottle 5;
step 2: the aeration oxidation tube 3 is fixed in the aeration bottle 5 through a cover of the aeration bottle 12, and the distance between the metal electrode 7 at the lower part of the aeration oxidation tube and the metal electrode 9 at the bottom of the aeration bottle is 1.5-3.5 mm;
step 3: opening the reflux condenser tube 13 to ensure that the temperature of the reflux condenser tube 13 is maintained below 5 ℃; then, an air pump 1 is started, the flow rate of the air pump is controlled to be 1-5L/min, and air provided by the air pump enters an aeration oxidation pipe 3 through an air purifying device 2;
step 4: the bottom metal electrode 7 at the inner side of the aeration oxidation tube 3 and the bottom metal electrode 8 at the outer side of the ventilation bottle 5 are connected with two poles of a high-voltage direct-current power supply, and the high-voltage direct-current power supply is started, and the power supply voltage is 10-30 KV;
step 5: for a certain sample, carrying out time gradient oxidation on the sample to obtain oxidation efficiency curves corresponding to different times; and then determining discharge time according to the required oxidation degree, and detecting after the liquid sample 6 reaches the expected oxidation degree, namely, turning off a high-voltage direct-current power supply, turning off an air pump and taking out the sample.
The invention has the beneficial effects that:
uniformly introducing the oxygen into a sample to be oxidized through aeration in an aeration oxidation tube, providing oxygen for ozone generated in a plasma discharge process, uniformly mixing the sample, uniformly oxidizing the oxygen in the air, generating active substances such as free radicals, ozone and the like in the plasma discharge process, and performing strong oxidation on dissolved components and suspended matters in the solution, wherein plasma discharge is formed between two metal electrodes; as a result, as shown in FIG. 5, the present invention was used to oxidize Fe ions in the sample with an oxidation efficiency of about 97%; compared with the traditional strong oxidant chemical oxidation method, the method can avoid the interference of introducing other chemical substances into the sample, and can oxidize the sample with high efficiency.
Drawings
FIG. 1 is a schematic diagram of the structure of the aeration strong oxidation device for the liquid sample.
FIG. 2 is a cross-sectional view of the structure of the aeration oxidation tube according to the present invention.
FIG. 3 is a schematic view of the small holes in the bottom cylindrical layout of the cylindrical aeration oxidation tube in the apparatus of the present invention.
Fig. 4 is a top view of the cap of the venting bottle in the device of the present invention.
FIG. 5 is a graph of experimental data for the apparatus and method of the present invention.
Reference numerals in the drawings: 1 is an air pump, 2 is an air purifying device, 3 is an aeration oxidation tube, 4 is an inlet of the aeration oxidation tube, 5 is an aeration bottle, 6 is a liquid sample to be oxidized, 7 is a metal electrode at the lower part of the aeration oxidation tube, 8 is a small through hole, 9 is a metal electrode at the bottom of the aeration bottle, 10 is a high-voltage direct current power supply, 11 is an exhaust port of the aeration bottle, 12 is a cover of the aeration bottle, and 13 is a reflux condensing tube.
Description of the embodiments
The invention will be further described with reference to the drawings and examples.
Examples: see fig. 1. Comprising the following steps: the device comprises an air pump 1, an air purifying device 2, an aeration oxidation tube 3, an aeration oxidation tube inlet 4, an aeration bottle 5, a sample 6 to be oxidized, an aeration oxidation tube lower metal electrode 7, a cylindrical hole 8, an aeration bottle bottom metal electrode 9, a high-voltage direct-current power supply 10, an aeration bottle exhaust port 11, an aeration bottle cap 12 and a reflux condenser tube 13.
In the present embodiment, the air pump 1 is used to provide an air source, specifically an air compressor, with a flow rate of 3L/min, which varies according to the size of the device and the oxidation rate.
In this embodiment, the air purifying device may remove organic matters, water vapor and particulate matters in the gas provided by the gas supply device, specifically, activated carbon or molecular sieve, and a bag-type dust collector, a cartridge dust collector or an electric dust collector.
In this embodiment, the aeration oxidation tube 3 is made of quartz, the tube wall thickness is 1.5 and mm, the internal dimension of the aeration oxidation tube 3 is 2 mm, and the diameter of the cylindrical aeration oxidation tube 3 and the diameter of the opening of the aeration bottle cap 12 are 25 mm all the time, so as to ensure stable connection and good air tightness of the device. The length of the aeration oxidation tube 3 is 140 mm, which is slightly longer than that of the aeration bottle, so that the distance between the metal electrode 7 at the lower part of the cylindrical aeration oxidation tube and the metal electrode 9 at the bottom of the aeration bottle can be changed, and the electric field between the two metal electrodes is adjusted, wherein the distance is 2 mm in this case, and the adjustment is carried out according to the high-voltage direct-current power supply voltage and the required oxidation efficiency. The bottom of the cylindrical aeration oxidation tube is provided with through holes 8, the aperture is 1 mm, and a plurality of through holes are uniformly distributed in a ring shape, so that uniform air flow distribution is ensured.
In the present embodiment, the height of the aeration bottle 5 is 60 mm, the bottle cap 12 of the aeration bottle 5 is of GL45 specification, a through hole is formed in the middle, the diameter of the through hole is 25 mm, the diameter of the through hole is the same as the outer diameter of the cylindrical aeration oxidation tube 3, the through hole is used for fixing the cylindrical aeration oxidation tube 3, the aeration bottle 5 is provided with an air outlet 11, and the diameter of the air outlet is 6 mm, and the air to be oxidized is discharged. The aeration bottle 5 is used for containing a sample 6 to be oxidized, the volume of the sample is 10-30 ml, 10 ml is added in the embodiment, and the liquid level of the sample is ensured to be higher than the cylindrical hole 8 of the cylindrical aeration oxidation tube.
In this embodiment, the dc power supply 10 is an adjustable power supply, and the voltage between the two metal electrodes can be adjusted according to the requirement, in this case, the voltage is 10 KV.
In this embodiment, the reflux condenser 13 is a serpentine condenser, which cools and returns the volatilized solvent in the sample to the aeration bottle, so as to ensure that the volume of the oxidized solvent in the sample is unchanged.
The method used in this example is:
step 1: 10 ml sample containing Fe ion is filled into a through-gas bottle 5;
step 2: the cylindrical aeration oxidation tube 3 is fixed in the aeration bottle 5 through an aeration bottle cap 12;
step 3: opening an air pump 1, wherein the flow rate of the air pump is 3L/min, and air provided by the air pump enters a cylindrical aeration oxidation tube 3 through an air purification device 2;
step 4: the metal electrodes at the lower part 7 of the cylindrical aeration oxidation tube and the bottom 8 of the aeration bottle are connected with a high-voltage direct-current power supply 10, and the high-voltage direct-current power supply 10 is started, and the power supply voltage is 10 KV;
step 5: the discharge time lasts for 30 min, and Fe in the sample is removed 2+ All oxygenated to Fe 3+ Turning off high-voltage direct current power supply, turning off air pump, taking out sample, and measuring Fe by phenanthroline molecular absorption spectrometry 2+ The content, the result of which is shown in FIG. 5, was that Fe ions in the sample were oxidized using the present example and method, and at the same time, compared with the hydrogen peroxide chemical oxidation method.
The device and the method can lead Fe of the sample to be 2+ High-efficiency oxidation; fe in the sample before oxidation as shown in the figure 2+ The content was 15. 15 mg/L, and the concentration after oxidation by the method of this example was 0.4 mg/L; and Fe after chemical oxidation with hydrogen peroxide 2+ The content of the catalyst is 3.5 mg/L which is higher than that of the oxidized catalyst obtained by the device and the method. As described above, the apparatus and method of the present invention provide improved results in the strong oxidation of dissolved components and suspended materials in solution.

Claims (8)

1. A liquid sample aeration strong oxidation device, comprising: the device comprises an air pump (1), an air purifying device (2), an aeration oxidation pipe (3), a ventilation bottle (5), a high-voltage direct-current power supply (10) and a reflux condensation pipe (13); wherein:
the air pump (1) is used for providing an air source;
the inlet of the air purifying device (2) is connected with the air pump (1) and is used for purifying the air provided by the air pump; comprises removing organic matters, water vapor and particulate matters;
the aeration oxidation tube (3) is cylindrical, an air inlet (4) is arranged on the side surface of the upper part, the air inlet (4) is connected with an air outlet of the air purifying device (2), and purified gas is used as an air source for aeration; the whole aeration oxidation tube (3) is arranged in the aeration bottle (5), and the upper part of the cylindrical tube is fixed through a through hole on the aeration bottle cap (12); the bottom of the inner side of the lower part of the aeration oxidation tube (3) is provided with a metal electrode (7), the bottom of the aeration oxidation tube (3) is provided with a plurality of small through holes (8) in annular layout, so that aeration entering the aeration oxidation tube (3) uniformly enters a sample liquid to be oxidized, oxygen is provided for ozone generated in the plasma discharge process, and meanwhile, the sample is uniformly mixed and oxidized;
the aeration bottle (5) is used for placing a sample (6) to be oxidized; the lower end part of the aeration oxidation tube (3) is arranged in a sample (6) to be oxidized; a metal electrode (9) is arranged outside the through hole (8) at the bottom of the ventilation bottle (5);
the two poles of the high-voltage direct current power supply (10) are respectively connected with a metal electrode (7) at the bottom of the inner side of the aeration oxidation tube (3) and a metal electrode (9) at the outer side of the bottom of the aeration bottle; the high-voltage direct current power supply (10) enables ionic body discharge to occur between two metal electrodes, active substances such as free radicals, ozone and the like are generated, and dissolved components and suspended matters in the solution are subjected to strong oxidation;
an air vent (11) is formed at the side of the air bottle (5), and the reflux condensation pipe (13) is connected with the air vent (11); the reflux condenser tube (13) is used for cooling and refluxing the volatilized solvent in the liquid sample into the ventilation bottle (5) so as to ensure that the volume of the oxidized sample solvent is unchanged.
2. The liquid sample aeration strong oxidation device according to claim 1, wherein the air purification device (2) is a purification device using activated carbon or molecular sieve as purification material.
3. The device for the aeration and strong oxidation of liquid samples according to claim 1, wherein the aeration bottle (5) is cylindrical in shape, has a height of 60-mm and a bottom surface diameter of 55-mm, is suitable for the treatment of 5-30 ml samples, and can be adjusted according to actual requirements.
4. The liquid sample aeration strong oxidation device according to claim 1, wherein the inner diameter of the aeration oxidation tube (3) is 1-3 mm, the length is 120-150 mm, and the length is larger than the height of the aeration bottle.
5. The liquid sample aeration strong oxidation device as claimed in claim 1, wherein the reflux condenser (13) is a serpentine, spherical or straight condenser.
6. The device for the aeration and the strong oxidation of the liquid sample according to claim 1, wherein the bottle cap (12) of the aeration bottle is matched with the aeration oxidation tube (3) in terms of GL45 specification and can be adjusted according to actual requirements.
7. The device for the aeration and strong oxidation of a liquid sample according to claim 1, wherein the electric field between the two metal electrodes is regulated by changing the distance between the metal electrode (7) at the lower part of the aeration oxidation tube and the metal electrode (9) at the bottom of the aeration bottle; the distance between the two is adjustable within the range of 1.5-3.5 mm.
8. The method for using the liquid sample aeration strong oxidation device according to any one of claims 1 to 7, wherein the specific operation flow is as follows:
step 1: filling 10-30 ml of liquid sample (6) to be oxidized into a gas passing cylinder (5);
step 2: the cylindrical aeration oxidation tube (3) is fixed in the aeration bottle (5) through a cover of the aeration bottle (12), and the distance between the metal electrode (7) at the lower part of the aeration oxidation tube and the metal electrode (9) at the bottom of the aeration bottle is 1.5-3.5 mm;
step 3: starting a reflux condensing pipe (13) and an air pump (1), controlling the flow rate of the air pump to be 1-5L/min, and enabling air provided by the air pump to enter a cylindrical aeration oxidation pipe (3) through an air purifying device (2);
step 4: the bottom metal electrode (7) at the inner side of the cylindrical aeration oxidation tube (3) and the bottom metal electrode (8) at the outer side of the ventilation bottle (5) are connected with two poles of a high-voltage direct-current power supply, and the high-voltage direct-current power supply is started, and the power supply voltage is 10-30 KV;
step 5: and determining discharge time according to the required oxidation degree, and detecting after the liquid sample (6) reaches the expected oxidation degree, namely, turning off a high-voltage direct-current power supply, turning off an air pump and taking out the sample.
CN202311158987.5A 2023-09-09 2023-09-09 Liquid sample aeration strong oxidation device and use method Pending CN117358179A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202311158987.5A CN117358179A (en) 2023-09-09 2023-09-09 Liquid sample aeration strong oxidation device and use method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202311158987.5A CN117358179A (en) 2023-09-09 2023-09-09 Liquid sample aeration strong oxidation device and use method

Publications (1)

Publication Number Publication Date
CN117358179A true CN117358179A (en) 2024-01-09

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CN202311158987.5A Pending CN117358179A (en) 2023-09-09 2023-09-09 Liquid sample aeration strong oxidation device and use method

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