CN111330533A - Preparation method of phosphorus-doped porous boron nitride adsorbent and application of phosphorus-doped porous boron nitride adsorbent in adsorption of heavy metal zinc in flue gas - Google Patents
Preparation method of phosphorus-doped porous boron nitride adsorbent and application of phosphorus-doped porous boron nitride adsorbent in adsorption of heavy metal zinc in flue gas Download PDFInfo
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- CN111330533A CN111330533A CN202010180806.9A CN202010180806A CN111330533A CN 111330533 A CN111330533 A CN 111330533A CN 202010180806 A CN202010180806 A CN 202010180806A CN 111330533 A CN111330533 A CN 111330533A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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Abstract
The invention discloses a preparation method of a phosphorus-doped porous boron nitride adsorbent and application of the phosphorus-doped porous boron nitride adsorbent in adsorption of heavy metal zinc in flue gas, and belongs to the field of preparation of non-metal porous materials and flue gas treatment. Adding boric acid, melamine, red phosphorus and deionized water into a container, and stirring to obtain a jelly; sealing the container, placing in a constant temperature shaking table, shaking, and cooling to obtain floccule; carrying out suction filtration on the obtained floccule, washing with deionized water, and drying in an oven to obtain a precursor; after nitrogen is introduced into the atmosphere furnace, the precursor which is paved in the corundum crucible is placed in the atmosphere furnace, and the opening of the atmosphere furnace is sealed; introducing nitrogen into the atmosphere furnace 5min before the temperature of the atmosphere furnace is increased, then starting to increase the temperature of the atmosphere furnace, and keeping the temperature of 1250-. The phosphorus-doped porous boron nitride prepared by the method has the advantages of large specific surface area and high purity, and can efficiently absorb heavy metal zinc in flue gas.
Description
Technical Field
The invention relates to the field of preparation of non-metallic porous materials and flue gas treatment, in particular to a preparation method of a phosphorus-doped porous boron nitride adsorbent and application of the phosphorus-doped porous boron nitride adsorbent in adsorption of heavy metal zinc in flue gas.
Background
The porous material is a material with a network structure formed by interconnected or closed pores, the boundaries or surfaces of the pores are formed by pillars or flat plates, and according to the definition of International Union of Pure and Applied Chemistry (IUPAC), the porous material can be divided into three categories, namely micropores (the pore diameter is less than 2nm), mesopores (the pore diameter is 2-50 nm) and macropores (the pore diameter is more than 50 nm). Porous materials generally have the advantages of low relative density, high specific surface area, light weight, and the like. The porous boron nitride is a novel non-oxide porous material, the interior of the porous boron nitride is formed by mutually communicated or closed pores, the porous boron nitride has a high specific surface area and a rich pore structure, the pore size can be regulated and controlled according to practical application, and meanwhile, the porous boron nitride is stable in chemical performance, high in heat conductivity, good in insulating property and has the hydrophobic characteristic. Compared with the traditional oxide carrier and the porous carbon carrier, the porous boron nitride material has good high-temperature stability and acid-base corrosion resistance, has small change of chemical property and thermal property even at higher temperature, and can be used as a catalyst carrier under severe conditions of high temperature, oxygen, strong corrosion and the like. In addition, the porous boron nitride material has special hydrogenation property and selective adsorption performance, and has great application potential in the fields of hydrogen storage, gas adsorption and separation.
The doping activation mode can further improve the heavy metal adsorption capacity of the porous boron nitride on the premise of not influencing the specific surface area, thereby improving the adsorption effect and efficiency of the porous boron nitride.
Disclosure of Invention
One of the objectives of the present invention is to provide a method for preparing a phosphorus-doped porous boron nitride adsorbent, which uses red phosphorus as a doping material to improve the adsorption efficiency of porous boron nitride.
The invention also aims to provide the application of the phosphorus-doped porous boron nitride as an adsorbent in adsorbing heavy metal zinc in flue gas.
The technical scheme adopted by the invention is as follows: a preparation method of a phosphorus-doped porous boron nitride adsorbent comprises the following steps:
1) adding boric acid, melamine, red phosphorus and deionized water into a container, and stirring to obtain a jelly; sealing the container, and placing the container in a constant-temperature shaking table for shaking; cooling to obtain floccule; carrying out suction filtration on the obtained floccule, washing with deionized water, and drying in an oven to obtain a precursor;
2) after nitrogen is introduced into the atmosphere furnace, the precursor which is paved in the corundum crucible is placed in the atmosphere furnace, and the opening of the atmosphere furnace is sealed; introducing nitrogen into the atmosphere furnace 5min before the temperature of the atmosphere furnace is raised, then raising the temperature of the atmosphere furnace, and keeping the temperature of 1250-.
Further, in the above preparation method, step 1), the molar ratio of boric acid to melamine to red phosphorus is 2:1: 0.5.
Further, in the above preparation method, in step 1), the shaking condition in the constant temperature shaking table is as follows: the oscillation frequency is 150r/min, the temperature is 85 ℃, and the oscillation time is 2 h.
Further, in the above preparation method, in step 1), the drying conditions in the oven are as follows: the oven temperature was 85 ℃ and the drying time was 12 h.
Further, in the preparation method, step 2), the flow rate of the introduced nitrogen is 400 ml/min.
The application of the phosphorus-doped porous boron nitride adsorbent in adsorbing heavy metals in flue gas.
Further, the heavy metal is zinc.
Further, the method is as follows: introducing flue gas containing heavy metal zinc into a container containing a phosphorus-doped porous boron nitride adsorbent, controlling the temperature of the container to be 50-250 ℃, and adsorbing.
The invention has the beneficial effects that:
(1) the phosphorus-doped porous boron nitride adsorbent prepared by the invention has stable chemical properties, good heat resistance and strong mechanical properties.
(2) The phosphorus-doped porous boron nitride adsorbent prepared by the invention has high efficiency and good effect of adsorbing heavy metal zinc in flue gas.
(3) The phosphorus-doped porous boron nitride adsorbent prepared by the invention has the advantages of rich main raw material sources, low price and low preparation cost.
(4) The phosphorus-doped porous boron nitride adsorbent prepared by the invention can also adsorb heavy metals of copper and chromium in flue gas.
(5) The doping substance adopted by the invention is red phosphorus, and the red phosphorus is doped in the porous boron nitride to form phosphate, so that on one hand, the phosphorus-doped porous boron nitride can physically adsorb heavy metals in the flue gas, and on the other hand, the phosphorus-doped porous boron nitride can also utilize phosphate radicals therein to adsorb heavy metals through chemical reaction, thereby greatly improving the effect of adsorbing the heavy metals in the flue gas.
Drawings
FIG. 1 is a schematic diagram of a device for generating simulated high-temperature flue gas in embodiment 2 of the invention.
Fig. 2 shows the selective effect of the phosphorus-doped porous boron nitride adsorbent prepared in the present invention on the adsorption of different heavy metals in flue gas containing 3 heavy metals of zinc, copper and cadmium.
Fig. 3 is a comparison graph of adsorption characteristics of the phosphorus-doped porous boron nitride adsorbent and the phosphorus-free porous boron nitride adsorbent prepared by the invention on heavy metal Zn in flue gas containing 3 heavy metals of zinc, copper and cadmium.
Fig. 4 is a graph comparing the adsorption characteristics of the phosphorus-doped porous boron nitride adsorbent and activated carbon prepared by the present invention on heavy metal Zn in flue gas containing only heavy metal zinc.
Detailed Description
Example 1
A preparation method of a phosphorus-doped porous boron nitride adsorbent comprises the following steps:
1) adding boric acid, melamine and red phosphorus into a conical flask according to the mol ratio of 2:1:0.5, adding deionized water, and stirring for 30min by using a glass rod to obtain pink jelly. Sealing the conical bottle with a sealing film, placing the conical bottle into a constant temperature shaking table, and shaking for 2 hours at a shaking frequency of 150r/min and a temperature of 85 ℃ to obtain pink transparent liquid. Stopping shaking, and cooling to room temperature to obtain pink floccule. And (3) carrying out suction filtration on the obtained pink floccule, repeatedly washing the pink floccule by using deionized water, putting the pink floccule into an oven, and drying the pink floccule for 12 hours at 85 ℃ to obtain a precursor.
2) The opening of the atmosphere furnace was sealed with a raw material tape (white opaque film-shaped polytetrafluoroethylene product), and nitrogen gas was introduced into the furnace at a flow rate of 400 ml/min. And (3) putting the precursor into a corundum crucible, uniformly spreading the precursor, putting the corundum crucible into a heating area in an atmosphere furnace, and sealing the opening of the atmosphere furnace by using the raw material belt again. And introducing nitrogen into the atmosphere furnace at the flow rate of 400ml/min 5min before the temperature of the atmosphere furnace is raised, then raising the temperature of the atmosphere furnace, keeping the temperature at 1300 ℃ for 4h, finally cooling to room temperature, and closing the atmosphere furnace and then closing the nitrogen to obtain the red fibrous phosphorus-doped porous boron nitride adsorbent.
Example 2
Adsorption of phosphorus-doped porous boron nitride adsorbent to heavy metals in flue gas
As shown in figure 1, heavy metal salt (zinc chloride and/or copper chloride and/or cadmium chloride) is placed in a heating zone of a tubular resistance furnace 2, the temperature of the tubular resistance furnace is adjusted, the temperature is kept at 950 ℃, the heavy metal salt is taken out after the temperature is kept for 20min, high-temperature flue gas containing heavy metals is obtained in the tubular resistance furnace 2, and the flue gas is cooled to room temperature. Adsorbent 5 (phosphorus-doped porous boron nitride adsorbent prepared in example 1 or other comparative adsorbent) was placed inside U-tube 3. An electric jacket is sleeved on the U-shaped pipe 3 to heat the U-shaped pipe, and the temperature is adjusted to be 50-250 ℃. Through air system 1, let in air to tubular resistance furnace in, take out the flue gas that contains the heavy metal, let in U type pipe 3 in through the pipeline, behind the absorbent 5 of U type pipe 3 bottom of flowing through, tail gas channels into in the tail gas processing apparatus 4. And detecting the adsorbent adsorbing the heavy metal.
1. Selective adsorption of phosphorus-doped porous boron nitride adsorbent on different heavy metals
The method comprises the following steps: the phosphorus-doped porous boron nitride adsorbent prepared in example 1 was placed inside the U-shaped tube 3. The temperature of the tubular resistance furnace 2 was adjusted to 950 ℃. Weighing 3g of zinc chloride, copper chloride and cadmium chloride in a crucible, quickly placing the crucible into a heating area of a tubular resistance furnace which is arranged well, and keeping the temperature for 20min to obtain simulated high-temperature flue gas containing heavy metal mixed with zinc, copper and cadmium. And after the constant temperature is finished, taking the crucible out of the tubular resistance furnace, and cooling on a refractory brick platform. And adjusting the adjustable electric heating sleeve on the U-shaped pipe to enable the U-shaped pipe to be at different temperatures, taking out flue gas containing mixed heavy metal of zinc, copper and cadmium in the tubular resistance furnace through the air system 1, introducing the flue gas into the U-shaped pipe through a pipeline, and introducing the tail gas into the tail gas treatment device 4 after the flue gas flows through the adsorbent at the bottom of the U-shaped pipe. And after adsorption, taking out the adsorbent which is placed in the U-shaped pipe and adsorbs the heavy metal, and putting the adsorbent into a self-sealing bag for detection.
Placing the adsorbent adsorbing heavy metals in a polytetrafluoroethylene crucible, adding a few drops of water for wetting, sequentially adding nitric acid, hydrofluoric acid and perchloric acid, placing on a 280 ℃ temperature-control electric hot plate, exhausting perchloric acid white smoke, adding aqua regia, standing for 2 minutes, and cooling. Transferring the solution into a plastic colorimetric tube, diluting with ultrapure water, shaking up, and clarifying. And (4) transferring the clear solution into a plastic colorimetric tube, diluting with nitric acid, and shaking up to obtain a digestion solution. And finally, measuring the heavy metal content of the digested solution by using an inductively coupled plasma emission spectrometer (ICP-OES).
As shown in FIG. 2, the phosphorus-doped porous boron nitride prepared in example 1 has a certain adsorption capacity for heavy metals, wherein the adsorption capacity for Zn is high and can reach 32.74mg/g at 50 ℃. The total adsorption amount of the porous boron nitride doped with phosphorus to the three heavy metals is reduced along with the increase of the temperature. The maximum value is 38.179mg/g at 100 ℃, and the total adsorption amount is about 41.7% of that at 100 ℃ when the temperature reaches 250 ℃. When the temperature is 100 ℃, the adsorption capacity of the phosphorus-doped porous boron nitride to Zn is 2.29 times and 5.19 times of that of Cu and Cd respectively, which shows that the phosphorus-doped porous boron nitride adsorbent has stronger adsorption selectivity to Zn.
2. The adsorption characteristics of the phosphorus-doped porous boron nitride adsorbent and the phosphorus-free porous boron nitride adsorbent on heavy metal zinc in smoke containing different heavy metals are compared.
Comparative example: the preparation method of the phosphorus-free porous boron nitride adsorbent is the same as that of example 1, except that red phosphorus is not added.
The method comprises the following steps: the phosphorus-doped porous boron nitride adsorbent and the phosphorus-free porous boron nitride adsorbent prepared in example 1 were placed in U-shaped tubes, respectively. The temperature of the tubular resistance furnace 2 was adjusted to 950 ℃. Weighing 3g of zinc chloride, copper chloride and cadmium chloride in a crucible, quickly placing the crucible into a heating area of a tubular resistance furnace which is arranged well, and keeping the temperature for 20min to obtain simulated high-temperature flue gas containing heavy metal mixed with zinc, copper and cadmium. And after the constant temperature is finished, taking the crucible out of the tubular resistance furnace, and cooling on a refractory brick platform. And adjusting the adjustable electric heating sleeve on the U-shaped pipe to enable the U-shaped pipe to be at different temperatures, taking out flue gas containing mixed heavy metal of zinc, copper and cadmium in the tubular resistance furnace through an air system, introducing the flue gas into the U-shaped pipe through a pipeline, and introducing the tail gas into a tail gas treatment device after the flue gas flows through the adsorbent at the bottom of the U-shaped pipe. And after adsorption, taking out the heavy metal-adsorbed adsorbent placed in the U-shaped pipe, and respectively placing the heavy metal-adsorbed adsorbent into the self-sealing bags.
Respectively placing the adsorbent adsorbing heavy metals in a polytetrafluoroethylene crucible, adding a few drops of water for wetting, sequentially adding nitric acid, hydrofluoric acid and perchloric acid, placing on a 280 ℃ temperature-control electric hot plate, exhausting perchloric acid white smoke, adding aqua regia, standing for 2 minutes, and cooling. Transferring the solution into a plastic colorimetric tube, diluting with ultrapure water, shaking up, and clarifying. And (4) transferring the clear solution into a plastic colorimetric tube, diluting with nitric acid, and shaking up to obtain a digestion solution. And finally, respectively measuring the heavy metal content of the digested solution by using an inductively coupled plasma emission spectrometer (ICP-OES).
As a result, as shown in FIG. 3, when comparing the adsorption amount of Zn in the simulated flue gas by the phosphorus-doped porous boron nitride and the phosphorus-free porous boron nitride, the adsorption amounts of Zn in both the adsorbents are gradually reduced along with the increase of the temperature. The adsorption capacity of the phosphorus-doped porous boron nitride to Zn is always higher than that of a phosphorus-free porous boron nitride adsorbent to Zn, the difference value reaches the maximum value of 1.98mg/g at 50 ℃, the minimum value reaches 0.51mg/g at 200 ℃, and the difference value is gradually reduced along with the rise of temperature, which shows that the adsorption effect of the phosphorus-doped porous boron nitride to Zn in simulated high-temperature flue gas is better than that of the phosphorus-free porous boron nitride adsorbent.
3. And comparing the adsorption characteristics of the phosphorus-doped porous boron nitride adsorbent and the activated carbon on Zn in the smoke only containing Zn.
The method comprises the following steps: the phosphorus-doped porous boron nitride adsorbent prepared in example 1 and activated carbon were placed in U-shaped tubes, respectively. The temperature of the tubular resistance furnace 2 was adjusted to 950 ℃. Weighing 10g of zinc chloride in a crucible, quickly placing the crucible into a heating area of a tubular resistance furnace which is arranged, and keeping the temperature for 20min to obtain simulated high-temperature flue gas only containing heavy metal zinc. And after the constant temperature is finished, taking the crucible out of the tubular resistance furnace, and cooling on a refractory brick platform. And adjusting the adjustable electric heating sleeve on the U-shaped pipe to enable the U-shaped pipe to be at different temperatures, taking out the smoke containing heavy metal zinc in the tubular resistance furnace through an air system, introducing the smoke into the U-shaped pipe through a pipeline, and introducing the tail gas into a tail gas treatment device after the smoke flows through the adsorbent at the bottom of the U-shaped pipe. After adsorption, the adsorbent which is placed in the U-shaped pipe and adsorbs heavy metal zinc is taken out and respectively placed in the self-sealing bags.
Placing the adsorbent adsorbing heavy metals in a polytetrafluoroethylene crucible, adding a few drops of water for wetting, sequentially adding nitric acid, hydrofluoric acid and perchloric acid, placing on a 280 ℃ temperature-control electric hot plate, exhausting perchloric acid white smoke, adding aqua regia, standing for 2 minutes, and cooling. Transferring the solution into a plastic colorimetric tube, diluting with ultrapure water, shaking up, and clarifying. And (4) transferring the clear solution into a plastic colorimetric tube, diluting with nitric acid, and shaking up to obtain a digestion solution. And finally, measuring the heavy metal content of the digested solution by using an inductively coupled plasma emission spectrometer (ICP-OES).
As a result, as shown in FIG. 4, the Zn adsorption amount of the activated carbon reached a maximum of 47.375mg/g at 150 ℃ and a minimum of 5.26mg/g at 50 ℃. The adsorption capacity of the porous boron nitride doped with phosphorus for Zn also reaches a maximum of 54.45mg/g at 150 ℃ and a minimum of 39.425mg/g at 50 ℃. The adsorption capacity of the porous boron nitride to Zn is kept above 40mg/g in each temperature range, the adsorption capacity is still as high as 40.425mg/g even if the temperature is 250 ℃, and the adsorption capacity of the activated carbon is only 18.125mg/g at 250 ℃. The adsorption capacity of the two adsorbents is gradually increased along with the increase of the temperature before 150 ℃, and the adsorption capacity of the phosphorus-doped porous boron nitride and the activated carbon to Zn is gradually reduced along with the continuous increase of the temperature after the temperature is higher than 150 ℃, which shows that the adsorption effect of the phosphorus-doped porous boron nitride to Zn in the simulated high-temperature flue gas only containing Zn is better than that of the activated carbon.
Claims (8)
1. A preparation method of a phosphorus-doped porous boron nitride adsorbent is characterized by comprising the following steps:
1) adding boric acid, melamine, red phosphorus and deionized water into a container, and stirring to obtain a jelly; sealing the container, and placing the container in a constant-temperature shaking table for shaking; cooling to obtain floccule; carrying out suction filtration on the obtained floccule, washing with deionized water, and drying in an oven to obtain a precursor;
2) after nitrogen is introduced into the atmosphere furnace, the precursor which is paved in the corundum crucible is placed in the atmosphere furnace, and the opening of the atmosphere furnace is sealed; introducing nitrogen into the atmosphere furnace 5min before the temperature of the atmosphere furnace is raised, then raising the temperature of the atmosphere furnace, and keeping the temperature of 1250-.
2. The method according to claim 1, wherein in step 1), the molar ratio of boric acid to melamine to red phosphorus is 2:1: 0.5.
3. The method according to claim 1, wherein in step 1), the shaking conditions in the constant temperature shaking table are as follows: the oscillation frequency is 150r/min, the temperature is 85 ℃, and the oscillation time is 2 h.
4. The preparation method according to claim 1, wherein in the step 1), the drying conditions in the oven are as follows: the oven temperature was 85 ℃ and the drying time was 12 h.
5. The method according to claim 1, wherein in the step 2), the flow rate of the nitrogen gas is 400 ml/min.
6. Use of a phosphorus-doped porous boron nitride adsorbent prepared according to the method of any one of claims 1-5 for adsorbing heavy metals in flue gas.
7. The use according to claim 6, wherein the heavy metal is zinc.
8. Use according to claim 7, characterized in that the method is as follows: introducing flue gas containing heavy metal zinc into a container containing the phosphorus-doped porous boron nitride adsorbent disclosed by any one of claims 1 to 5, and controlling the temperature of the container to be 50-250 ℃ for adsorption.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107126816A (en) * | 2017-05-16 | 2017-09-05 | 沈阳航空航天大学 | The method that heavy metal in high-temperature flue gas is removed using active boron nitride |
| CN110201628A (en) * | 2019-05-29 | 2019-09-06 | 沈阳航空航天大学 | A kind of doping boron nitride and preparation method thereof removing heavy metal in high-temperature flue gas |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107126816A (en) * | 2017-05-16 | 2017-09-05 | 沈阳航空航天大学 | The method that heavy metal in high-temperature flue gas is removed using active boron nitride |
| CN110201628A (en) * | 2019-05-29 | 2019-09-06 | 沈阳航空航天大学 | A kind of doping boron nitride and preparation method thereof removing heavy metal in high-temperature flue gas |
Non-Patent Citations (2)
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| JING ZHANG ET AL: "Regulating the electronic and optic properties of hexagonal boron nitride nanosheets via phosphorus doping", 《EPL》 * |
| 翟振宇: "多孔氮化硼的制备、活化及其重金属高温吸附特性研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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Application publication date: 20200626 |