CN115196614B - Preparation and detection method of porous material loaded with nano oxygen - Google Patents
Preparation and detection method of porous material loaded with nano oxygen Download PDFInfo
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- CN115196614B CN115196614B CN202210707715.5A CN202210707715A CN115196614B CN 115196614 B CN115196614 B CN 115196614B CN 202210707715 A CN202210707715 A CN 202210707715A CN 115196614 B CN115196614 B CN 115196614B
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- 239000001301 oxygen Substances 0.000 title claims abstract description 297
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 297
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 255
- 239000011148 porous material Substances 0.000 title claims abstract description 86
- 238000001514 detection method Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 31
- 230000000087 stabilizing effect Effects 0.000 claims abstract description 26
- 239000002105 nanoparticle Substances 0.000 claims abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 10
- 238000011068 loading method Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 84
- 239000000243 solution Substances 0.000 claims description 42
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 40
- 238000007789 sealing Methods 0.000 claims description 38
- 238000006243 chemical reaction Methods 0.000 claims description 35
- 238000011282 treatment Methods 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 28
- 239000002245 particle Substances 0.000 claims description 28
- 239000012286 potassium permanganate Substances 0.000 claims description 20
- 235000010265 sodium sulphite Nutrition 0.000 claims description 20
- 238000004448 titration Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000009826 distribution Methods 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 9
- 241001411320 Eriogonum inflatum Species 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 7
- 239000002028 Biomass Substances 0.000 claims description 6
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 4
- 239000011707 mineral Substances 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 239000012621 metal-organic framework Substances 0.000 claims description 3
- 229920000620 organic polymer Polymers 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000013268 sustained release Methods 0.000 abstract description 2
- 239000012730 sustained-release form Substances 0.000 abstract description 2
- 238000010792 warming Methods 0.000 abstract 1
- 239000003610 charcoal Substances 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000002689 soil Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 235000015097 nutrients Nutrition 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229960000892 attapulgite Drugs 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000009499 grossing Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052901 montmorillonite Inorganic materials 0.000 description 2
- 229910052625 palygorskite Inorganic materials 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229910052902 vermiculite Inorganic materials 0.000 description 2
- 239000010455 vermiculite Substances 0.000 description 2
- 235000019354 vermiculite Nutrition 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 238000000540 analysis of variance Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 239000003621 irrigation water Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 230000000696 methanogenic effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006213 oxygenation reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
Abstract
The invention relates to a preparation and detection method of a porous material loaded with nano oxygen, which comprises the following steps of S1: loading nano oxygen for the porous material by utilizing a negative pressure vacuum device and a high pressure oxygen carrier; s2: measuring the nano-oxygen content carried by the porous material by using a closed continuous flow system comprising a nitrogen providing device, a gas flow stabilizing device, an oxygen releasing device and an oxygen reacting device; s3: and detecting the form and the characteristics of the nano oxygen carried by the porous material by adopting a nano particle tracking analyzer. Compared with the prior art, the nano-oxygen-loaded porous material has higher nano-oxygen content, slow and sustained release capacity and better performance, and the nano-oxygen detection method is more convenient and accurate, so that the nano-oxygen-loaded porous material prepared by the invention has great significance in ensuring grain safety and alleviating global warming if being applied in paddy fields, and is beneficial to agricultural yield increase and emission reduction.
Description
Technical Field
The invention belongs to the technical field of novel material preparation and performance detection, and particularly relates to a preparation and detection method of a porous material loaded with nano oxygen.
Background
The aeration condition of farmland soil is a key factor affecting nutrient element absorption and growth and development of crops, and the root system of the crops needs to consume enough oxygen to perform respiration in the growth and development process, so that the absorption of the crops to the nutrients and moisture in the soil is promoted. Thus, adequate oxygen supply is a key factor in promoting crop improvement in nutrient utilization efficiency. The paddy field is easy to enrich methanogenic bacteria due to the dry-wet alternation characteristic, and becomes a main source of methane emission in the atmosphere, and if the oxygen content is increased in the paddy field, the soil redox condition is improved, the growth and propagation of methane-oxidizing bacteria are facilitated, and the methane emission in the paddy field is greatly reduced.
In recent years, nanometer oxygen bubbles are receiving more and more attention due to the characteristics of long service life, negative charge on the surface and high oxygen mass transfer efficiency. The common oxygen bubbles with non-nanometer size have large buoyancy and are easy to burst, and on the contrary, the nanometer oxygen bubbles have small volume, can slowly diffuse oxygen into surrounding liquid phase, and can exist for more than 70 days when the diameter is smaller than 200 nm. The nanometer oxygen bubbles can be divided into liquid-phase nanometer oxygen bubbles and interface nanometer oxygen bubbles, and the application of the nanometer oxygen bubbles in the agricultural field is focused on adding the liquid-phase nanometer oxygen bubbles into irrigation water at present, so that the dissolution of fertilizer is promoted, the concentration of dissolved oxygen in water is increased, and the yield and quality of crops are improved, for example, chinese patent application CN212876707U discloses a micro-nanometer bubble oxygenation irrigation system which can be applied to agricultural crop cultivation.
Compared with liquid phase nano oxygen bubbles, the interface nano oxygen bubbles have greater advantages in manufacturing cost, existence time and transportation portability. Chinese patent application CN101503238B discloses a method for repairing lake and anaerobic sediment by utilizing nano oxygen bubbles, which effectively improves the dissolved oxygen level of water body by spraying or jetting composite material loaded with nano oxygen bubbles to the surface of the lake. On one hand, the material loaded with nano oxygen bubbles carries nano oxygen through a complex pore structure and a huge specific surface area, and on the other hand, the nano oxygen is slowly released in the environment, and meanwhile, the oxygen carrying material can be used for soil improvement.
However, to date, the methods for preparing the porous material carrying nano oxygen and detecting the oxygen carrying amount are still imperfect, most of the prior art emphasizes the performance of the porous material, but ignores oxygen, and does not pay attention to whether the carried oxygen is nano oxygen bubbles, for example, chinese patent application CN111097374B discloses a preparation method of the composite functional material carrying oxygen and adsorption and application thereof in water body restoration, and although the preparation method and application condition of the oxygen carrying material are described in detail, the measurement of the oxygen carrying amount of the oxygen carrying material and the detection of the oxygen carrying form are lacking. In the preparation method of the oxygen-carrying porous material, the problems of overlarge energy consumption, higher cost, long time consumption, complex device, difficult transportation and the like exist, for example, chinese patent application CN215234150U discloses a preparation system of the oxygen-carrying porous material, and successfully prepares an environment-friendly oxygen-carrying porous material which has a high molecular compound coating layer and can overcome the defect of overlarge oxygen release rate. Therefore, a technology for preparing and detecting a porous material with complete interface nano oxygen bubbles is found, the operation difficulty and the commercial cost in the technical operation are reduced, and the technology is very important for achieving the purposes of increasing the yield and reducing the emission of agriculture when applied to a paddy field ecological system.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation and detection method of a porous material loaded with nano oxygen.
The aim of the invention can be achieved by the following technical scheme:
a preparation and detection method of a porous material loaded with nano oxygen comprises the following steps:
s1: loading nano oxygen into a porous material by utilizing a negative pressure vacuum device and a high-pressure oxygen-bearing device:
vacuumizing the porous material by using a negative pressure vacuum device, transferring the vacuumized porous material into a high-pressure oxygen-bearing device, adjusting the pressure of the high-pressure oxygen-bearing device to 0.2MPa, and then filling pure oxygen to load nano oxygen into the porous material;
s2: measuring the nano oxygen content carried by the porous material by using a closed continuous flow system comprising a nitrogen providing device, a gas flow stabilizing device, an oxygen releasing device and an oxygen reacting device, and ensuring that the nano oxygen content carried by the porous material is 12-16mg/g;
s3: detecting the form and the characteristic of the nano oxygen carried by the porous material by adopting a nano particle tracking analyzer, and ensuring the average particle size of the nano oxygen bubbles to be 110-120nm;
wherein the porous material is selected from biomass, minerals, organic polymers or metal-organic frameworks.
In one embodiment of the present invention, in step S1:
the negative pressure vacuum device is formed by connecting a circulating water type vacuum pump and a suction bottle, wherein an air outlet of the suction bottle is communicated with an air inlet of the circulating water type vacuum pump through a rubber tube, and a sample inlet of the suction bottle is closed by a movable sealing plug;
the high-pressure oxygen-carrying device is formed by connecting an oxygen supply device and a high-pressure sealing device, wherein the oxygen supply device can be communicated with an air inlet of the high-pressure sealing device through an air outlet by using a rubber tube, the high-pressure sealing device can control air inlet through a valve switch, and sample injection is performed through a handle opening device.
In one embodiment of the invention:
the operation flow of the negative pressure vacuum device is that a proper amount of porous material is weighed, the sample is added into a suction filtration bottle, a sealing plug is used for sealing a sample inlet, and the vacuum is pumped for 2 hours under the condition that the pressure is minus 0.1 MPa;
the operation flow of the high-pressure oxygen-bearing device is that the porous material after the vacuum pumping is transferred into the high-pressure oxygen-bearing device, the sealing device is used for adjusting the pressure of the oxygen supply device to 0.2MPa, 99.99% pure oxygen is filled after the pressure in the high-pressure sealing device is increased to 0.2MPa, the operation flow is maintained for 30min, then the oxygen supply device is closed, and the pressure in the high-pressure sealing device is reduced to atmospheric pressure.
In one embodiment of the invention, the negative pressure vacuum device and the high pressure oxygen carrier device are operated for 3 times in sequence, wherein in the operation of the negative pressure vacuum device for the last 2 times, the vacuumizing time is changed to 45 minutes, and the rest operation parameters are the same.
In one embodiment of the present invention, in step S2:
the nitrogen supply device consists of a nitrogen cylinder and a pressure valve and is connected with an air inlet of the air flow stabilizing device through a rubber pipe;
the air flow stabilizing device is a wide-mouth bottle filled with anaerobic water, and the air outlet is connected with the oxygen releasing device through a rubber tube;
the oxygen release device comprises a three-neck flask, wherein a left neck is an air inlet, a right neck is an air outlet, a dissolved oxygen measuring instrument is inserted into a middle neck, the air outlet is connected with the air inlet of the oxygen reaction device through a rubber tube, a sample to be measured and oxygen-free water are contained in the three-neck flask, the three-neck flask is placed in a water bath heater, and the water bath heater is placed on a magnetic stirrer;
the oxygen reaction device main part is three-necked flask, and the left neck includes intake pipe and outlet duct simultaneously, and the right neck is sealed through airtight stopper, and the buret that holds potassium permanganate solution is inserted to the middle neck, holds sodium sulfite solution in the three-necked flask, and the three-necked flask holds in water bath heater, and water bath heater holds on magnetic stirrer.
In one embodiment of the invention:
the anaerobic water in the air flow stabilizing device and the oxygen releasing device is obtained by filling pure water with nitrogen with the air outlet pressure of 0.1MPa for 20 min;
the potassium permanganate solution in the burette in the oxygen reaction device is prepared by dissolving potassium permanganate solid in sulfuric acid solution with the concentration of 1mol/L, wherein the concentration is 0.02mol/L;
the sodium sulfite solution in the three-necked flask in the oxygen reaction device was obtained by dissolving sodium sulfite solid in deionized water at a concentration of 0.01mol/L.
In one embodiment of the present invention, in step S2:
the pretreatment of the closed continuous flow system comprises the steps of adding 0.02mol/L potassium permanganate solution into a burette in an oxygen reaction device, adding 150ml of anaerobic water into an air flow stabilizing device, closing a bottle stopper, adding 200ml of anaerobic water into a three-neck flask in an oxygen release device, closing the bottle stopper, opening an air valve of a nitrogen supply device, adjusting the air outlet pressure to be 0.1MPa, and inputting continuous nitrogen flow into the oxygen release device through the air flow stabilizing device until the dissolved oxygen content measured by a dissolved oxygen measuring instrument is 0 and is unchanged for 60 seconds.
In one embodiment of the present invention, in step S2:
the operation flow of the closed continuous flow system is that 200ml of sodium sulfite solution with the concentration of 0.01mol/L and a magnetic stirrer are added into an oxygen reaction device under the condition that nitrogen is kept flowing in the whole system, 0.5g of nano-oxygen porous material to be detected and the magnetic stirrer are added into an oxygen release device, two water bath heaters in the oxygen reaction device and the oxygen release device are turned on, the temperature is adjusted to 45 ℃, the two magnetic stirrers are turned on, and the rotating speed is adjusted to 1500rpm.
In one embodiment of the present invention, in step S2:
the method for detecting the closed continuous flow system comprises the steps of closing a water bath heater and a magnetic stirrer in an oxygen release device and an oxygen reaction device after the content of dissolved oxygen detected by a dissolved oxygen detector in the oxygen release device is changed to 0 again and is unchanged for 30 seconds, titrating in the oxygen reaction device, reading a titration starting point until the solution in a three-necked flask is changed from colorless to light red, and reading a titration end point;
the nano oxygen content of the nano oxygen carrying porous material is calculated according to the following formula:
wherein M is the nano oxygen content carried by the porous material per unit mass, and the unit is mg/g, c (Na 2 SO 3 ) For the concentration of sodium sulfite solution, c (KMnO 4 ) Is the concentration of potassium permanganate solution, V end For the value converted to L for the titration endpoint reading, V ini For the value converted into L of the titration starting point reading, m (material) is the mass of the nano-oxygen carrying porous material to be tested.
In one embodiment of the present invention, in step S3:
the method for detecting the nano-oxygen morphology comprises the steps of setting porous material treatment and nano-oxygen carrying porous material treatment, respectively adding the porous material and the nano-oxygen carrying porous material into deionized water with the concentration of 0.1g/ml, fully mixing, then passing through a 0.3 mu m filter membrane, diluting 50 times by each treatment, and detecting the morphology and particle size distribution of nano-particles in liquid by using a nano-particle tracking analyzer;
the method for detecting the nano oxygen characteristic comprises the steps of additionally setting a treatment of retaining the nano oxygen carrying porous material in ionized water for 1 week, wherein the concentration is 0.1g/ml, fully mixing, sealing and preserving for 1 week at the room temperature of 24+/-1 ℃, then passing through a 0.3 mu m filter membrane, diluting for 50 times, and detecting the form and particle size distribution of nano particles in the liquid by using a nano particle tracking analyzer.
In one embodiment of the invention, the biomass char comprises biochar, hydrothermal char, and modified biochar; the mineral comprises zeolite, vermiculite, montmorillonite, attapulgite, etc.; .
In one embodiment of the present invention, the porous material is preferably biomass charcoal which has been widely used in paddy fields.
The porous material loaded with nano oxygen can be applied to a paddy field ecological system.
Compared with the prior art, the invention has the following beneficial effects:
(1) The equipment and the container used by the negative pressure vacuum device and the high pressure oxygen carrier are common, the combination is simple, the total consumption of the oxygen carrier flow is 5.75 hours, the process time is greatly shortened, the operation is convenient, the safety guarantee is provided, and the advantages are provided on the cost and the fabrication cost.
(2) Besides the oxygen carrying technology, the oxygen carrying method is also included, the stable and continuous unidirectional flow of nitrogen in the system is ensured through the air flow stabilizing device, the oxygen carrying amount is ensured not to be interfered by external oxygen, the oxygen release of the oxygen carrying material is quickened through the modes of magnetic stirring and water bath heating, the oxygen carrying material is released as completely as possible, the accuracy of the oxygen carrying amount is improved, the system can be ensured to operate in sequence only by utilizing the dissolved oxygen detector, the detection is visual, and the oxygen carrying material is convenient to adjust at any time.
(3) Besides the oxygen carrying amount measuring method, the method also comprises nano oxygen form and characteristic detection, so that the prepared oxygen carrying material is ensured to carry nano oxygen in multiple dimensions, has the characteristic of slow release, and provides theoretical basis for application of the oxygen carrying material in a paddy field system.
Drawings
FIG. 1 is a schematic diagram of a negative pressure vacuum apparatus;
FIG. 2 is a schematic diagram of a high pressure oxygen ballast device;
FIG. 3 is a schematic diagram of a closed continuous flow system comprising a nitrogen providing means, a gas flow smoothing means, an oxygen releasing means, an oxygen reacting means;
FIG. 4 is the presence of nanooxygen bubbles in BC process;
FIG. 5 is the presence of nano-oxygen bubbles in a BOC process;
FIG. 6 shows the presence of nano-oxygen bubbles in a BOC-NW process.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following examples.
The preparation and detection method of the porous material loaded with nano oxygen applied to the paddy field ecological system comprises the following steps:
s1: and loading nano oxygen into the porous material by utilizing a negative pressure vacuum device and a high-pressure oxygen-loading device.
The negative pressure vacuum device is formed by connecting a circulating water type vacuum pump and a suction bottle, wherein an air outlet of the suction bottle is communicated with an air inlet of the circulating water type vacuum pump through a rubber tube, and a sample inlet of the suction bottle is closed by a movable sealing plug.
The high-pressure oxygen-carrying device is formed by connecting an oxygen supply device and a high-pressure sealing device, wherein the oxygen supply device can be communicated with an air inlet of the high-pressure sealing device through an air outlet by using a rubber tube, the high-pressure sealing device can control air inlet through a valve switch, and sample injection is performed through a handle opening device.
The operation flow of the negative pressure vacuum device is that a proper amount of porous material is weighed, the sample is added into a suction filtration bottle, a sample inlet is closed by a sealing plug, and the vacuum is pumped for 2 hours under the condition that the pressure is minus 0.1 MPa.
The operation flow of the high-pressure oxygen-bearing device is that the porous material after the vacuum pumping is transferred into the high-pressure oxygen-bearing device, the sealing device is used for adjusting the pressure of the oxygen supply device to 0.2MPa, 99.99% pure oxygen is filled after the pressure in the high-pressure sealing device is increased to 0.2MPa, the operation flow is maintained for 30min, then the oxygen supply device is closed, and the pressure in the high-pressure sealing device is reduced to atmospheric pressure.
The negative pressure vacuum device and the high pressure oxygen-bearing device are operated for 3 times in sequence, wherein in the operation of the negative pressure vacuum device for the last 2 times, the vacuumizing time is modified to 45 minutes, and the rest operation parameters are the same.
S2: the nano-oxygen content carried by the porous material was measured using a closed continuous flow system comprising a nitrogen providing device, a gas flow smoothing device, an oxygen releasing device, an oxygen reacting device.
The nitrogen supply device consists of a nitrogen cylinder and a pressure valve, and is connected with an air inlet of the air flow stabilizing device through a rubber pipe. The air flow stabilizing device is a wide-mouth bottle filled with oxygen-free water, and the air outlet is connected with the oxygen releasing device through a rubber tube. The oxygen release device main body is a three-necked flask, the left neck is an air inlet, the right neck is an air outlet, the middle neck is inserted into the dissolved oxygen measuring instrument, the air outlet is connected with the air inlet of the oxygen reaction device through a rubber tube, the three-necked flask is filled with a sample to be measured and oxygen-free water, the three-necked flask is placed in a water bath heater, and the water bath heater is placed on the magnetic stirrer. The oxygen reaction device main body is a three-necked flask, the left neck simultaneously comprises an air inlet pipe and an air outlet pipe, the right neck is closed by a closed plug, the middle neck is inserted into a burette filled with potassium permanganate solution, sodium sulfite solution is filled in the three-necked flask, the three-necked flask is placed in a water bath heater, and the water bath heater is placed on a magnetic stirrer.
The oxygen-free water in the air flow stabilizing device and the oxygen releasing device is obtained by charging pure water with nitrogen gas with the air outlet pressure of 0.1MPa for 20 min. The potassium permanganate solution in the burette in the oxygen reaction device is prepared by dissolving potassium permanganate solid in sulfuric acid solution with the concentration of 1mol/L, and the concentration is 0.02mol/L. The sodium sulfite solution in the three-necked flask in the oxygen reaction apparatus was obtained by dissolving sodium sulfite solid in deionized water at a concentration of 0.01mol/L.
The pretreatment of the closed continuous flow system comprises the steps of adding 0.02mol/L potassium permanganate solution into a burette in an oxygen reaction device, adding 150ml of anaerobic water into an air flow stabilizing device, closing a bottle stopper, adding 200ml of anaerobic water into a three-neck flask in an oxygen release device, closing the bottle stopper, opening an air valve of a nitrogen supply device, adjusting the air outlet pressure to be 0.1MPa, and inputting continuous nitrogen flow into the oxygen release device through the air flow stabilizing device until the dissolved oxygen content measured by a dissolved oxygen measuring instrument is 0 and is unchanged for 60 seconds.
The operation flow of the closed continuous flow system is that 200ml of sodium sulfite solution with the concentration of 0.01mol/L and a magnetic stirrer are added into an oxygen reaction device under the condition of keeping nitrogen flowing in the whole system, 0.5g of nano-oxygen porous material to be detected and the magnetic stirrer are added into an oxygen release device, two water bath heaters in the oxygen reaction device and the oxygen release device are turned on, the temperature is adjusted to 45 ℃, the two magnetic stirrers are turned on, and the rotating speed is adjusted to 1500rpm.
The method for detecting the closed continuous flow system comprises the steps of closing a water bath heater and a magnetic stirrer in the oxygen release device and the oxygen reaction device after the content of the dissolved oxygen detected by a dissolved oxygen detector in the oxygen release device is changed to 0 again and is unchanged for 30 seconds, titrating in the oxygen reaction device, reading a titration starting point until the solution in the three-necked flask is changed from colorless to light red, and reading a titration end point. The nano oxygen content of the nano oxygen carrying porous material is calculated according to the following formula:
wherein M is the nano oxygen content carried by the porous material in mg/g, and c (Na 2 SO 3 ) For the concentration of sodium sulfite solution, c (KMnO 4 ) Is the concentration of potassium permanganate solution, V end For the value converted to L for the titration endpoint reading, V ini For the value converted into L of the titration starting point reading, m (material) is the mass of the nano-oxygen carrying porous material to be tested.
S3: and detecting the form and the characteristic of the nano oxygen carried by the porous material by adopting a nano particle tracking analyzer, and ensuring the average particle size of the nano oxygen bubbles to be 110-120nm.
The method for detecting the nano-oxygen morphology comprises the steps of setting deionized water treatment, porous material treatment and nano-oxygen carrying porous material treatment, adding the porous material and the nano-oxygen carrying porous material into deionized water respectively, wherein the concentration is 0.1g/ml, fully and uniformly mixing, then, passing through a 0.3 mu m filter membrane, diluting the treatments for 50 times, and detecting the morphology of nano-particles and the particle size distribution of the particles in the liquid by using a nano-particle tracking analyzer.
The method for detecting the nano oxygen characteristic comprises the steps of additionally setting the treatment of retaining the nano oxygen-carrying porous material in the ionized water for 1 week, wherein the concentration is 0.1g/ml, fully and uniformly mixing, sealing and preserving for 1 week at the room temperature of 24+/-1 ℃, then passing through a 0.3 mu m filter membrane, diluting for 50 times, and detecting the form and particle size distribution of nano particles in the liquid by using a nano particle tracking analyzer.
Porous materials include biomass charcoal (biochar, hydrothermal charcoal and modified biochar), minerals (zeolite, vermiculite, montmorillonite, attapulgite, etc.), organic polymers, metal-organic frameworks, etc., and preferably biomass charcoal which has been widely used in paddy fields.
Examples
The embodiment provides a preparation and detection method of a nano-oxygen-loaded porous material applied to a paddy field ecological system. The nano-oxygen-carrying porous material is selected from biochar which is widely applied in paddy fields, the raw material is rice straw, three treatments shown in table 1 are respectively deionized and anaerobic water blank treatment CK, deionized and anaerobic water and biochar contrast treatment BC and deionized and anaerobic water and nano-oxygen-carrying biochar treatment BOC, and three repetitions are respectively arranged in experiments for measuring the nano-oxygen content of the nano-oxygen-carrying biochar.
TABLE 1 oxygen carrying amount measurement test treatment set-up details
The embodiment comprises the following steps:
s1: and loading nano oxygen into the biochar in BOC treatment by using a negative pressure vacuum device and a high pressure oxygen carrier.
The negative pressure vacuum device used in the embodiment is shown in fig. 1, and is formed by connecting a circulating water type vacuum pump and a suction filtration bottle, wherein an air outlet of the suction filtration bottle is communicated with an air inlet of the circulating water type vacuum pump through a rubber tube, and an injection port of the suction filtration bottle is closed by a movable sealing plug.
The high-pressure oxygen-carrying device used in the embodiment is shown in fig. 2 and is formed by connecting an oxygen supply device and a high-pressure sealing device, wherein the oxygen supply device can be communicated with an air inlet of the high-pressure sealing device through an air outlet by a rubber tube, the high-pressure sealing device can control air inlet through a valve switch, and the handle is used for opening the device for sample injection.
In a negative pressure vacuum device, weighing 0.5g of biochar, adding the biochar into a suction filtration bottle, sealing a sample inlet by using a sealing plug, filling water into a water tank of a circulating water type vacuum pump, turning on a motor switch, vacuumizing under the pressure condition that the pressure representation number shows that the pressure is minus 0.1MPa for 2 hours, then pulling out a communicating pipe at an air outlet of the suction filtration bottle, and turning off a motor.
In the high-pressure oxygen-bearing device, a handle switch is turned on, biochar in the suction filtration bottle is transferred to the high-pressure device, the handle is screwed, and the device is sealed. Opening an oxygen supply device, regulating the indication number of a pressure valve to 0.2MPa, charging 99.99% pure oxygen after the pressure in the high-pressure sealing device is increased to 0.2MPa, maintaining for 30min, then closing a switch of the oxygen supply device, and taking out biochar after the pressure in the high-pressure sealing device is naturally reduced until the internal pressure is equal to the external atmospheric pressure of the device.
And (3) putting the biochar material into a negative pressure vacuum device again, and repeating the operation flow in the two devices for 2 times in sequence, wherein the operation parameters are kept consistent except that the vacuumizing time is modified to 45 min. Finally obtaining the nano-oxygen-carrying biochar in BOC treatment.
S2: the nano-oxygen content carried by the biochar is measured by using a closed continuous flow system comprising a nitrogen providing device, a gas flow stabilizing device, an oxygen releasing device and an oxygen reacting device, and the nano-oxygen content carried by the porous material is ensured to be 12-16mg/g.
The closed continuous flow system used in this embodiment is shown in fig. 3, and is a nitrogen supply device, a gas flow stabilizing device, an oxygen release device and an oxygen reaction device in this order from left to right.
The nitrogen supply device consists of a nitrogen cylinder and a pressure valve, and is connected with an air inlet of the air flow stabilizing device through a rubber pipe.
The air flow stabilizing device is a wide-mouth bottle filled with oxygen-free water, and the air outlet is connected with the oxygen releasing device through a rubber tube.
The oxygen release device main body is a three-necked flask, the left neck is an air inlet, the right neck is an air outlet, the middle neck is inserted into the dissolved oxygen measuring instrument, the air outlet is connected with the air inlet of the oxygen reaction device through a rubber tube, the three-necked flask is filled with a sample to be measured and oxygen-free water, the three-necked flask is placed in a water bath heater, and the water bath heater is placed on the magnetic stirrer.
The oxygen reaction device main body is a three-necked flask, the left neck simultaneously comprises an air inlet pipe and an air outlet pipe, the right neck is closed by a closed plug, the middle neck is inserted into a burette filled with potassium permanganate solution, sodium sulfite solution is filled in the three-necked flask, the three-necked flask is placed in a water bath heater, and the water bath heater is placed on a magnetic stirrer.
The preparation method of the solution used in this example is as follows: the anaerobic water in the air flow stabilizing device and the oxygen releasing device is obtained by filling pure water with nitrogen with the air outlet pressure of 0.1MPa for 20 min; the potassium permanganate solution in the burette in the oxygen reaction device is prepared by dissolving potassium permanganate solid in sulfuric acid solution with the concentration of 1mol/L, wherein the concentration is 0.02mol/L; the sodium sulfite solution in the three-necked flask in the oxygen reaction apparatus was obtained by dissolving sodium sulfite solid in deionized water at a concentration of 0.01mol/L.
In a closed continuous flow system, a pretreatment operation is first performed. To a 50mL burette in an oxygen reactor, 0.02mol/L of an acidic potassium permanganate solution was added to remove air bubbles. 150ml of anaerobic water is added into the air flow stabilizing device, and the bottle stopper is closed. 200ml of oxygen-free water was added to a three-necked flask in an oxygen releasing device, and the bottle stopper was closed. Opening a gas valve of the nitrogen supply device, adjusting the gas outlet pressure to be 0.1MPa, and inputting continuous nitrogen flow into the oxygen release device through the gas flow stabilizing device until the dissolved oxygen content measured by a dissolved oxygen measuring instrument in the oxygen release device is 0 and is unchanged for 60 seconds.
In a closed continuous flow system, formal operation is then initiated. 200ml of a 0.01mol/L sodium sulfite solution and a magnetic stirrer were added to the oxygen reactor while maintaining the flow of nitrogen through the system. To the oxygen releasing device, 0.5g of nano-oxygen-carrying Biochar (BOC)/Biochar (BC)/none (CK) to be tested and a magnetic stirrer were added. Two water bath heaters in the oxygen release device and the oxygen reaction device are turned on, the temperature is adjusted to 45 ℃, two magnetic stirrers are turned on, and the rotating speed is adjusted to 1500rpm.
And finally detecting the nano oxygen content in a closed continuous flow system. When the dissolved oxygen content measured by the dissolved oxygen detector in the oxygen releasing device is changed to 0 again and is unchanged for 30 seconds, the water bath heater and the magnetic stirrer in the oxygen releasing device and the oxygen reacting device are turned off. Titration was performed in an oxygen reaction apparatus, and the titration start point was read until the solution in the three-necked flask was changed from colorless to pale red, and the titration end point was read. The nano oxygen content of the nano oxygen-carrying biochar is calculated according to the following formula:
wherein M is the nano oxygen content carried by the porous material per unit mass, and the unit is mg/g, c (Na 2 SO 3 ) The concentration of the sodium sulfite solution is 0.01mol/L, c (KMnO 4 ) The concentration of the potassium permanganate solution is 0.02mol/L, V end For the value converted to L for the titration endpoint reading, V ini For the value converted to L of the titration start reading, m (material) is the mass of the nano-oxygen porous material to be tested, and is 0.5g.
The nano-oxygen content of each treatment is shown in Table 2, wherein the nano-oxygen content of the nano-oxygen-loaded biochar reaches 14mg/g, which is far greater than that of the non-oxygen-loaded biochar and blank treatment (p <0.001, ANOVA), indicating that the oxygen loading was successful.
TABLE 2 oxygen carrying amount detection results
S3: and detecting the form and the characteristics of the nano oxygen carried by the porous material by adopting a nano particle tracking analyzer.
1g of nano-oxygen-loaded Biochar (BOC)/Biochar (BC) was placed in a 50ml plastic centrifuge tube, 10ml of deionized water was added, thoroughly mixed, then filtered through a 0.3 μm filter, and 50-fold dilution was performed with deionized water, and the nanoparticle size distribution in each treated sample was detected using a nanoparticle tracking analyzer (Zeta view 8.04.02Particle Metrix Inc.).
In order to detect the time-varying characteristics of the nano oxygen bubbles, a treatment (BOC-NW) of retaining the nano oxygen-carrying biochar in ionized water for 1 week was additionally provided, 1g of the nano oxygen-carrying biochar was placed in a 50ml plastic centrifuge tube, 10ml of deionized water was added, thoroughly mixed, sealed and stored at room temperature of 24+ -1deg.C for 1 week, then filtered through a 0.3 μm filter membrane, and 50-fold diluted with deionized water, and the particle size distribution of the nano particles in the sample was detected by a nanoparticle tracking analyzer (Zeta view 8.04.02Particle Metrix Inc.).
The presence of nano-oxygen bubbles in BC processing is shown in fig. 4, the presence of nano-oxygen bubbles in BOC processing is shown in fig. 5, and the presence of nano-oxygen bubbles in BOC-NW processing is shown in fig. 6. As can be seen from the three figures, the content of nano oxygen bubbles in BOC treatment is high, the particle size is small, the content of nano oxygen bubbles in BOC-NW treatment is second, the particle size is medium, and the content of nano oxygen bubbles in BC treatment is low, the particle size is medium.
The nanoparticle concentration and particle size distribution in each treatment are shown in table 3, where X10 is the largest particle size of the 10% particles with the smallest particle size, X50 is the largest particle size of the 50% particles with the smallest particle size, and X90 is the largest particle size of the 90% particles with the smallest particle size.
The results show that the average particle size of the nano oxygen bubbles in the nano oxygen-carrying biochar treatment (BOC) is about 118nm, the nano oxygen concentration is higher by one order of magnitude than that in the BC treatment, the nano oxygen concentration is obviously higher (p <0.001, turkey), the oxygen carrying effect is good, the values of X50 and X90 are obviously smaller than that in the BC treatment (p=0.032, turkey; p=0.040, turkey) in mutual evidence with the oxygen carrying amount detection result, and the ratio of the nano oxygen bubbles with smaller particle size in the BOC treatment is larger.
In the treatment (BOC-NW) where the nano-oxygen-carrying biochar was left in ionized water for 1 week, the mean particle size of the nano-oxygen bubbles was not much different from that of the BOC treatment (p=0.170, turkey), the nano-oxygen concentration was an order of magnitude higher than that of the BC treatment, the values of X50 and X90 were significantly greater (p=0.016, turkey), and there was no significant difference from that of the BOC treatment (p=0.172, turkey; p=0.211, turkey), and these results indicated that the nano-oxygen of the nano-oxygen-carrying biochar was not released rapidly even when left in water for one week, with the potential of slow sustained release.
TABLE 3 nanoparticle concentration and particle size distribution
The foregoing describes in detail preferred embodiments of the present invention. It should be understood that numerous modifications and variations can be made in accordance with the concepts of the invention by one of ordinary skill in the art without undue burden. Therefore, all technical solutions which can be obtained by logic analysis, reasoning or limited experiments based on the prior art by the person skilled in the art according to the inventive concept shall be within the scope of protection defined by the claims.
Claims (7)
1. The preparation and detection method of the nano-oxygen loaded porous material is characterized by comprising the following steps of:
s1: loading nano oxygen into a porous material by utilizing a negative pressure vacuum device and a high-pressure oxygen-bearing device:
vacuumizing the porous material by using a negative pressure vacuum device, transferring the vacuumized porous material into a high-pressure oxygen-bearing device, adjusting the pressure of the high-pressure oxygen-bearing device to 0.2MPa, and then filling pure oxygen to load nano oxygen into the porous material;
s2: measuring the nano oxygen content carried by the porous material by using a closed continuous flow system comprising a nitrogen providing device, a gas flow stabilizing device, an oxygen releasing device and an oxygen reacting device, and ensuring that the nano oxygen content carried by the porous material is 12-16mg/g;
s3: detecting the form and the characteristic of the nano oxygen carried by the porous material by adopting a nano particle tracking analyzer, and ensuring the average particle size of the nano oxygen bubbles to be 110-120nm;
wherein the porous material is selected from biomass, minerals, organic polymers or metal-organic frameworks;
in step S1:
the negative pressure vacuum device is formed by connecting a circulating water type vacuum pump and a suction bottle, wherein an air outlet of the suction bottle is communicated with an air inlet of the circulating water type vacuum pump through a rubber tube, and a sample inlet of the suction bottle is closed by a movable sealing plug;
the high-pressure oxygen-carrying device is formed by connecting an oxygen supply device and a high-pressure sealing device, wherein the oxygen supply device can be communicated with an air inlet of the high-pressure sealing device through an air outlet by using a rubber tube, the high-pressure sealing device can control air inlet through a valve switch, and sample injection is performed through a handle opening device;
in step S2:
the nitrogen supply device consists of a nitrogen cylinder and a pressure valve and is connected with an air inlet of the air flow stabilizing device through a rubber pipe;
the air flow stabilizing device is a wide-mouth bottle filled with anaerobic water, and the air outlet is connected with the oxygen releasing device through a rubber tube;
the oxygen release device comprises a three-neck flask, wherein a left neck is an air inlet, a right neck is an air outlet, a dissolved oxygen measuring instrument is inserted into a middle neck, the air outlet is connected with the air inlet of the oxygen reaction device through a rubber tube, a sample to be measured and oxygen-free water are contained in the three-neck flask, the three-neck flask is placed in a water bath heater, and the water bath heater is placed on a magnetic stirrer;
the oxygen reaction device is characterized in that the main body of the oxygen reaction device is a three-necked flask, the left neck simultaneously comprises an air inlet pipe and an air outlet pipe, the right neck is sealed by a sealing plug, a burette filled with potassium permanganate solution is inserted into the middle neck, sodium sulfite solution is filled in the three-necked flask, the three-necked flask is placed in a water bath heater, and the water bath heater is placed on a magnetic stirrer;
in step S3:
the method for detecting the nano-oxygen morphology comprises the steps of setting porous material treatment and nano-oxygen carrying porous material treatment, respectively adding the porous material and the nano-oxygen carrying porous material into deionized water with the concentration of 0.1g/ml, fully mixing, then passing through a 0.3 mu m filter membrane, diluting 50 times by each treatment, and detecting the morphology and particle size distribution of nano-particles in liquid by using a nano-particle tracking analyzer;
the method for detecting the nano oxygen characteristics comprises the steps of additionally setting a treatment of retaining the nano oxygen carrying porous material in the ionized water for 1 week, wherein the concentration is 0.1g/ml, fully mixing, sealing and preserving for 1 week at the room temperature of 24+/-1 ℃, then passing through a 0.3 mu m filter membrane, diluting for 50 times, and detecting the form and particle size distribution of nano particles in the liquid by using a nano particle tracking analyzer.
2. The method for preparing and detecting the nano-oxygen supported porous material according to claim 1, wherein the method comprises the following steps:
the operation flow of the negative pressure vacuum device is that the porous material is weighed, the sample is added into a suction filtration bottle, a sealing plug is used for sealing a sample inlet, and the vacuum is pumped for 2 hours under the condition that the pressure is minus 0.1 MPa;
the operation flow of the high-pressure oxygen-bearing device is that the porous material after the vacuum pumping is transferred into the high-pressure oxygen-bearing device, the sealing device is used for adjusting the pressure of the oxygen supply device to 0.2MPa, 99.99% pure oxygen is filled after the pressure in the high-pressure sealing device is increased to 0.2MPa, the operation flow is maintained for 30min, then the oxygen supply device is closed, and the pressure in the high-pressure sealing device is reduced to atmospheric pressure.
3. The method for preparing and detecting the nano-oxygen loaded porous material according to claim 2, wherein the negative pressure vacuum device and the high pressure oxygen loading device are operated for 3 times in sequence, wherein in the operation of the negative pressure vacuum device for the last 2 times, the vacuumizing time is changed to 45min, and the rest operation parameters are the same.
4. The method for preparing and detecting the nano-oxygen supported porous material according to claim 1, wherein the method comprises the following steps:
the anaerobic water in the air flow stabilizing device and the oxygen releasing device is obtained by filling pure water with nitrogen with the air outlet pressure of 0.1MPa for 20 min;
the potassium permanganate solution in the burette in the oxygen reaction device is prepared by dissolving potassium permanganate solid in sulfuric acid solution with the concentration of 1mol/L, wherein the concentration is 0.02mol/L;
the sodium sulfite solution in the three-necked flask in the oxygen reaction device was obtained by dissolving sodium sulfite solid in deionized water at a concentration of 0.01mol/L.
5. The method for preparing and detecting nano-oxygen applied to paddy field ecosystem according to claim 1, wherein in step S2:
the pretreatment of the closed continuous flow system comprises the steps of adding 0.02mol/L potassium permanganate solution into a burette in an oxygen reaction device, adding 150ml of anaerobic water into an air flow stabilizing device, closing a bottle stopper, adding 200ml of anaerobic water into a three-neck flask in an oxygen release device, closing the bottle stopper, opening an air valve of a nitrogen supply device, adjusting the air outlet pressure to be 0.1MPa, and inputting continuous nitrogen flow into the oxygen release device through the air flow stabilizing device until the dissolved oxygen content measured by a dissolved oxygen measuring instrument is 0 and is unchanged for 60 seconds.
6. The method for preparing and detecting a porous material loaded with nano oxygen according to claim 1, wherein in step S2:
the operation flow of the closed continuous flow system is that 200ml of sodium sulfite solution with the concentration of 0.01mol/L and a magnetic stirrer are added into an oxygen reaction device under the condition that nitrogen is kept flowing in the whole system, 0.5g of nano-oxygen porous material to be detected and the magnetic stirrer are added into an oxygen release device, two water bath heaters in the oxygen reaction device and the oxygen release device are turned on, the temperature is adjusted to 45 ℃, the two magnetic stirrers are turned on, and the rotating speed is adjusted to 1500rpm.
7. The method for preparing and detecting a porous material loaded with nano oxygen according to claim 1, wherein in step S2:
the method for detecting the closed continuous flow system comprises the steps of closing a water bath heater and a magnetic stirrer in an oxygen release device and an oxygen reaction device after the content of dissolved oxygen detected by a dissolved oxygen detector in the oxygen release device is changed to 0 again and is unchanged for 30 seconds, titrating in the oxygen reaction device, reading a titration starting point until the solution in a three-necked flask is changed from colorless to light red, and reading a titration end point;
the nano oxygen content of the nano oxygen carrying porous material is calculated according to the following formula:
wherein M is the nano oxygen content carried by the porous material per unit mass, and the unit is mg/g, c (Na 2 SO 3 ) For the concentration of sodium sulfite solution, c (KMnO 4 ) Is the concentration of potassium permanganate solution, V end For the value converted to L for the titration endpoint reading, V ini For the value converted into L of the titration starting point reading, m (material) is the mass of the nano-oxygen carrying porous material to be tested.
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