CN114669267A - Copper-based adsorbent and preparation method and application thereof - Google Patents
Copper-based adsorbent and preparation method and application thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- 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
- B01D53/04—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 with stationary adsorbents
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Abstract
The invention belongs to the technical field of adsorption materials, and particularly relates to a copper-based adsorbent and a preparation method and application thereof. The invention provides a preparation method of a copper-based adsorbent, which comprises the following steps: and mixing and roasting a nitrogen source, a carbon source and a copper source to obtain the copper-based adsorbent. In the invention, in the roasting process, a copper source is decomposed to obtain copper oxide, and a nitrogen source and a carbon source are decomposed and doped in the copper oxide to form an adsorbing material with a porous structure; and more basic sites can be provided by carbon-nitrogen doping, so that acidic H can be adsorbed more favorably2S, increasing H2Adsorption efficiency of S.
Description
Technical Field
The invention belongs to the technical field of adsorption materials, and particularly relates to a copper-based adsorbent and a preparation method and application thereof.
Background
H2S is a colorless, corrosive and inflammable highly toxic gas, mainly generated in industries such as coal, natural gas and oil refining, and directly converts H without any treatment2S is discharged, which may have a very adverse effect on the surrounding environment and human health. It is reported that exposure to lower concentrations of H2In the S environment, eye irritation, sore throat, cough, nausea, shortness of breath and pulmonary edema can result; and high concentration of H2S can quickly weaken the smell of people and cause people to die. Thus to H2Removal of S is important and essential.
At present, both at home and abroad for H2The S is removed mainly by wet method, i.e. H is removed by alkali liquor2S is adsorbed, but the method easily generates a large amount of waste liquid, brings secondary pollution and increases the environmental burden. In contrast, adsorptive oxidation is probably the most potent H2S removal method, wherein the adsorption oxidation method mainly utilizes porous adsorption material to purify and remove H2S,H2S is adsorbed on the surface of the adsorbing material and is further oxidized into other sulfides to remove H2And (4) purpose of S. But the current adsorbents are for H2The adsorption efficiency of S is low.
Disclosure of Invention
The invention aims to provide a copper-based adsorbent, and a preparation method and application thereof2S has higher adsorption efficiency.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a preparation method of a copper-based adsorbent, which comprises the following steps:
and mixing and roasting a nitrogen source, a carbon source and a copper source to obtain the copper-based adsorbent.
Preferably, the nitrogen source comprises one or more of urea, melamine and biuret;
the carbon source comprises one or more of glucose, sucrose and starch;
the copper source comprises a copper salt.
Preferably, the mass ratio of the nitrogen source, the carbon source and the copper source is (2-10): (1-4): (1-6).
Preferably, the mixing mode is grinding; the grinding time is 10-30 min.
Preferably, the roasting temperature is 300-700 ℃, and the roasting time is 2-5 h; the heating rate of heating to the roasting temperature is 2-10 ℃/min.
The invention also provides the copper-based adsorbent prepared by the preparation method in the technical scheme, and the copper-based adsorbent is carbon-nitrogen-doped copper oxide.
The invention also provides the technical scheme that the copper-based adsorbent is used for removing H2And (5) application in S.
Preferably, the application comprises the following steps:
will contain H2And carrying out gas-solid reaction on the S gas and the copper-based adsorbent to obtain the inactivated copper-based adsorbent.
Preferably, the addition amount of the copper-based adsorbent is 0.1-0.5 g;
said compound containing H2H in S gas2The concentration of S is 400-1000 ppm; said compound containing H2The flow rate of the S gas is 80-120 mL/min.
Preferably, the gas-solid reaction temperature is 60-110 ℃.
The invention provides a preparation method of a copper-based adsorbent, which comprises the following steps: and mixing and roasting a nitrogen source, a carbon source and a copper source to obtain the copper-based adsorbent. In the invention, during the roasting process, the copper source is decomposed to obtain copper oxide, and the nitrogen source and the carbon source are decomposedDoping the copper oxide to form an adsorption material with a porous structure; and more basic sites can be provided by carbon-nitrogen doping, so that acidic H can be adsorbed more favorably2S, increasing H2Adsorption efficiency of S.
Drawings
Fig. 1 is an SEM image of the copper-based adsorbent of example 1;
fig. 2 is an XRD pattern of the deactivated copper-based adsorbent obtained in application example 2;
FIG. 3 shows the copper-based adsorbent pair H in application example 12S removing effect graph;
FIG. 4 shows the copper-based adsorbent pair H in application example 22S removing effect graph;
FIG. 5 shows the copper-based adsorbent pair H in application example 32S removing effect graph;
FIG. 6 shows the copper-based adsorbent pair H in application example 42S removing effect graph;
FIG. 7 shows the adsorbent pair H in application example 52And (5) removing effect diagram of S.
Detailed Description
The invention provides a preparation method of a copper-based adsorbent, which comprises the following steps:
and mixing and roasting a nitrogen source, a carbon source and a copper source to obtain the copper-based adsorbent.
In the present invention, all the starting materials for the preparation are commercially available products known to those skilled in the art unless otherwise specified.
In the present invention, the nitrogen source preferably includes one or more of urea, melamine and biuret. In the present invention, the carbon source preferably includes one or more of glucose, sucrose and starch. In the present invention, the copper source preferably includes a copper salt, and more preferably one or more of copper nitrate, copper sulfate, copper acetate and copper chloride.
In the invention, the mass ratio of the nitrogen source, the carbon source and the copper source is preferably (2-10): (1-4): (1-6), more preferably (3-9): (2-3): (2-5), more preferably (4-8): (2-3): (3-4).
In the present invention, the mixing is preferably performed by grinding. In the invention, the grinding time is preferably 10-30 min, more preferably 12-28 min, and still more preferably 15-25 min. The grinding process is not particularly limited in the present invention, and may be performed by a process known to those skilled in the art. In the present invention, the grinding is preferably performed in a mortar.
In the invention, the roasting temperature is preferably 300-700 ℃, more preferably 350-650 ℃, and more preferably 400-600 ℃; the time is preferably 2 to 5 hours, more preferably 2.5 to 4.5 hours, and even more preferably 3 to 4 hours; the heating rate of the temperature rise to the roasting temperature is preferably 2-10 ℃/min, more preferably 3-9 ℃/min, and even more preferably 5-8 ℃/min. In the present invention, the calcination is preferably performed in an air atmosphere.
In the present invention, the firing process is preferably: and placing the mixed material in a crucible, and then placing the crucible in a microwave muffle furnace for roasting. In the roasting process, the copper source is decomposed to generate copper oxide, and the nitrogen source and the carbon source are decomposed to realize carbon-nitrogen doping on the copper oxide, so that the carbon-nitrogen-doped copper oxide adsorbent is obtained.
After the roasting is finished, the invention also preferably comprises the steps of cooling, grinding and sieving the obtained material in sequence. The present invention does not require any particular procedure for cooling and grinding, and can be carried out by procedures well known to those skilled in the art. In the present invention, the aperture of the screen used for the screening treatment is preferably 40 to 60 mesh, and more preferably 50 mesh.
The preparation method provided by the invention is simple, needs less equipment, has short preparation period, needs cheap and easily-obtained materials, and greatly reduces the preparation cost of the adsorbent.
The invention also provides the copper-based adsorbent prepared by the preparation method in the technical scheme, and the copper-based adsorbent is carbon-nitrogen-doped copper oxide.
The invention also provides the technical scheme that the copper-based adsorbent is used for removing H2And (S).
In the present invention, the application preferably comprises the steps of:
will contain H2And carrying out gas-solid reaction on the S gas and the copper-based adsorbent to obtain the inactivated copper-based adsorbent.
In the present invention, the amount of the copper-based adsorbent added is preferably 0.1 to 0.5g, more preferably 0.2 to 0.4g, and still more preferably 0.2 to 0.3 g.
The invention is directed to said compound containing H2The source of the S gas is not particularly limited as long as it contains H2And (4) S gas. In the present invention, the compound containing H2The gas of S preferably comprises H2S, oxygen and nitrogen. In the present invention, the compound containing H2H in S gas2The concentration of S is preferably 400 to 1000ppm, more preferably 500 to 900ppm, and still more preferably 600 to 800 ppm. In the present invention, the volume concentration of the oxygen gas is preferably 0.5% to 2%, more preferably 0.8% to 1.8%, even more preferably 0.9% to 1.5%, and most preferably 1.0% to 1.2%. In the invention, the oxygen can further activate the adsorbent, and active sites on the adsorbent are improved. In the present invention, the nitrogen gas is used to control H2The flow rate of S. In the present invention, the compound containing H2The flow rate of the S gas is preferably 80 to 120mL/min, more preferably 85 to 115mL/min, and still more preferably 90 to 110 mL/min.
In the present invention, the process of the gas-solid reaction is preferably: placing the copper-based adsorbent in a quartz glass tube, plugging two ends of the quartz glass tube by quartz wool, and then placing the quartz glass tube in a tube furnace for preheating;
said catalyst contains H2S gas is passed through a tube furnace, and H is controlled by nitrogen2And (3) carrying out gas-solid reaction on the flow velocity of the S and the copper-based adsorbent to obtain the inactivated copper-based adsorbent.
In the invention, the preheating temperature is preferably 60-110 ℃, further preferably 70-100 ℃, and more preferably 80-90 ℃; the time is preferably 20 to 40min, more preferably 25 to 35min, and still more preferably 28 to 30 min. In the present invention, moisture and impurities in the copper-based adsorbent can be removed by preheating.
In the invention, the gas-solid reaction temperature is preferably 60-110 ℃, more preferably 70-100 ℃, and even more preferably 80-90 ℃. The time of the gas-solid reaction is not specially limited, and a gas chromatograph is preferably adopted for H at the inlet and the outlet of the tubular furnace in the gas-solid reaction process2S concentration is detected as H at the inlet and outlet of the tube furnace2When the concentration of S is equal, the gas-solid reaction is stopped. The invention is directed to said H2The detection process of the S concentration is not particularly limited, and a detection process known to those skilled in the art may be employed.
After the gas-solid reaction is finished, the invention also preferably comprises the steps of cleaning and drying the obtained material.
In the invention, the cleaning liquid used for cleaning is preferably deionized water; the number of times of cleaning is preferably 3-5 times, and more preferably 3-4 times; the drying temperature is preferably 80-120 ℃, more preferably 90-110 ℃, and more preferably 95-100 ℃; the time is preferably 12-15 h, and more preferably 13-14 h; the drying is preferably carried out in an oven.
In the invention, the inactivated copper-based adsorbent comprises CuS which is a P-type semiconductor material with high light-heat conversion rate, and can be widely applied to the fields of solar batteries, nonlinear optical materials, high-capacity lithium ion battery cathode materials, nano switches, biosensors and the like. The invention adsorbs, purifies and removes H2S at the same time realize H2The CuS is synthesized by resource conversion of S, so that the method has high recycling value, the aim of synchronously removing toxic and harmful waste gas and recycling the waste gas is fulfilled, and the waste gas purification cost is reduced.
In order to further illustrate the present invention, the following detailed description of a copper-based adsorbent, its preparation method and application are provided in conjunction with the accompanying drawings and examples, which should not be construed as limiting the scope of the present invention.
Example 1
2g of urea, 1g of glucose and 4g of copper nitrate are put into a mortar for grinding for 10min, the ground mixture is put into a crucible, then the crucible is put into a microwave muffle furnace, and the temperature is raised to 500 ℃ at the heating rate of 10 ℃/min for roasting for 3 h; and cooling and grinding the roasted material, and sieving the material by using a 40-60-mesh sieve to obtain the copper-based adsorbent.
Example 2
Putting 6g of urea, 1g of glucose and 2g of copper nitrate into a mortar for grinding for 30min, putting the ground mixture into a crucible, then putting the crucible into a microwave muffle furnace, heating to 550 ℃ at the heating rate of 5 ℃/min, and roasting for 3 h; and cooling and grinding the roasted material, and sieving the material by using a 40-60-mesh sieve to obtain the copper-based adsorbent.
Example 3
Putting 7g of urea, 2g of glucose and 3g of copper nitrate into a mortar for grinding for 10min, putting the ground mixture into a crucible, then putting the crucible into a microwave muffle furnace, and heating to 500 ℃ at the heating rate of 3 ℃/min for roasting for 3 h; and cooling and grinding the roasted material, and sieving the material by using a 40-60-mesh sieve to obtain the copper-based adsorbent.
Example 4
Putting 5g of urea, 1g of glucose and 2g of copper nitrate into a mortar for grinding for 10min, putting the ground mixture into a crucible, then putting the crucible into a microwave muffle furnace, heating to 550 ℃ at the heating rate of 3 ℃/min, and roasting for 3 h; and cooling and grinding the roasted material, and sieving the material by using a 40-60-mesh sieve to obtain the copper-based adsorbent.
Application example 1
Placing 0.3g of the copper-based adsorbent obtained in example 1 in a quartz glass tube, plugging both ends of the quartz glass tube with quartz wool, placing the quartz glass tube in a tube furnace, and preheating at 90 ℃ for 20 min;
then 100mL/min of the mixed gas was passed into the reactor (wherein nitrogen was used to control the flow rate of the gas, H)2The concentration of S is 600ppm, the concentration of oxygen is 0.5 percent, the rest is nitrogen), the reaction temperature is 90 ℃, gas-solid reaction is carried out, and then gas-phase color is carried outSpectrometer for detecting H in inlet and outlet gases2Concentration of S when H2When the inlet concentration and the outlet concentration of the S are consistent, the adsorption is finished; and taking out the adsorbed copper-based adsorbent, washing the copper-based adsorbent for 3 times by using deionized water, and drying the copper-based adsorbent in an oven at 100 ℃ for 14h to obtain the inactivated copper-based adsorbent.
Application example 2
Placing 0.3g of the copper-based adsorbent obtained in example 2 in a quartz glass tube, plugging both ends of the quartz glass tube with quartz wool, placing the quartz glass tube in a tube furnace, and preheating at 90 ℃ for 20 min;
then 100mL/min of the mixed gas was passed into the reactor (wherein nitrogen was used to control the flow rate of the gas, H)2The concentration of S is 600ppm, the concentration of oxygen is 1 percent, the rest is nitrogen), the reaction temperature is 90 ℃, gas-solid reaction is carried out, and then a gas chromatograph is used for detecting H in inlet and outlet gas2Concentration of S when H2When the inlet concentration and the outlet concentration of the S are consistent, the adsorption is finished; and taking out the adsorbed copper-based adsorbent, washing the copper-based adsorbent for 3 times by using deionized water, and drying the copper-based adsorbent in an oven at 100 ℃ for 14h to obtain the inactivated copper-based adsorbent.
Application example 3
Placing 0.3g of the copper-based adsorbent obtained in example 3 in a quartz glass tube, plugging both ends of the quartz glass tube with quartz wool, placing the quartz glass tube in a tube furnace, and preheating at 100 ℃ for 20 min;
then 100mL/min of the mixed gas was passed into the reactor (wherein nitrogen was used to control the flow rate of the gas, H)2The concentration of S is 600ppm, the concentration of oxygen is 0.8 percent, the rest is nitrogen), the reaction temperature is 100 ℃, gas-solid reaction is carried out, and then a gas chromatograph is used for detecting H in inlet and outlet gas2Concentration of S when H2When the inlet concentration and the outlet concentration of the S are consistent, the adsorption is finished; and taking out the adsorbed copper-based adsorbent, washing the copper-based adsorbent for 3 times by using deionized water, and drying the copper-based adsorbent in an oven at 100 ℃ for 14h to obtain the inactivated copper-based adsorbent.
Application example 4
Placing 0.3g of the copper-based adsorbent obtained in example 4 in a quartz glass tube, plugging both ends of the quartz glass tube with quartz wool, placing the quartz glass tube in a tube furnace, and preheating at 100 ℃ for 20 min;
then 100mL/min of the mixed gas was passed into the reactor (wherein nitrogen was used to control the flow rate of the gas, H)2The concentration of S is 600ppm, the concentration of oxygen is 1 percent, the rest is nitrogen), the reaction temperature is 100 ℃, gas-solid reaction is carried out, and then a gas chromatograph is used for detecting H in inlet and outlet gas2Concentration of S when H2When the inlet concentration and the outlet concentration of the S are consistent, the adsorption is finished; and taking out the adsorbed copper-based adsorbent, washing the copper-based adsorbent for 3 times by using deionized water, and drying the copper-based adsorbent in an oven at 100 ℃ for 14h to obtain the inactivated copper-based adsorbent.
Comparative example 1
Putting 3g of urea and 2g of copper nitrate into a mortar for grinding for 30min, putting the ground mixture into a crucible, then putting the crucible into a microwave muffle furnace, heating to 550 ℃ at the heating rate of 10 ℃/min, and roasting for 3 h; and cooling and grinding the roasted material, and sieving the material by using a 40-60-mesh sieve to obtain the adsorbent.
Application example 5
Placing 0.3g of the adsorbent obtained in comparative example 1 in a quartz glass tube, plugging both ends of the quartz glass tube with quartz wool, placing the quartz glass tube in a tube furnace, and preheating at 90 ℃ for 20 min;
then 100mL/min of the mixed gas was passed into the reactor (wherein nitrogen was used to control the flow rate of the gas, H)2The concentration of S is 600ppm, the concentration of oxygen is 1 percent, the rest is nitrogen), the reaction temperature is 90 ℃, gas-solid reaction is carried out, and then a gas chromatograph is used for detecting H in inlet and outlet gas2Concentration of S when H2And when the inlet concentration and the outlet concentration of the S are consistent, finishing the adsorption.
Performance testing
Test example 1
The scanning electron microscope test is performed on the copper-based adsorbent obtained in example 1, the test result is shown in fig. 1, and it can be seen from fig. 1 that the copper-based adsorbent obtained in this example has a porous structure, tableThe face is similar to coral and is more beneficial to H2And (4) adsorbing S.
Test example 2
The deactivated copper-based adsorbent obtained in application example 2 was tested by a D/MAX-2200 type X-ray diffractometer under the test conditions of CuKa radiation (λ: 0.15406nm), voltage 36kV, current 30mA, scanning range of 10-80 °, scanning speed of 5 °/min, and the test result is shown in fig. 2, and it can be seen from fig. 2 that many diffraction peaks of CuS appear on the surface of the deactivated copper-based adsorbent, which illustrates that the copper-based adsorbent and H of the present invention are combined with each other, and thus the present invention is applicable to the deactivated copper-based adsorbent obtained in application example 22S reacts and the main product is CuS. From the XRD results, no other substances were detected on the deactivated copper-based adsorbent, indicating that the purity of the produced CuS was high.
Test example 3
Application example 1 copper-based adsorbent to H2The S removal effect is shown in FIG. 3. from FIG. 3, it can be seen that the copper-based adsorbent is responsible for H2The time for maintaining the removal efficiency of S to be more than 90% is 480min, and the sulfur capacity in each gram of copper-based adsorbent is 144.8 mg;
application example 2 copper-based adsorbent to H2The removal effect of S is shown in FIG. 4. from FIG. 4, it can be seen that the copper-based adsorbent is on H2The time for maintaining the removal efficiency of the S to be more than 90% is 900min, and the sulfur capacity in each gram of the copper-based adsorbent is 273.2 mg;
application example 3 copper-based adsorbent pair H2The S removal effect is shown in FIG. 5. from FIG. 5, it can be seen that the copper-based adsorbent is responsible for H2The time for maintaining the removal efficiency of the S to be more than 90% is 630min, and the sulfur capacity in each gram of copper-based adsorbent is 190.3 mg;
application example 4 copper-based adsorbent pair H2The S removal effect is shown in FIG. 6. from FIG. 6, it can be seen that the copper-based adsorbent is responsible for H2The time for maintaining the removal efficiency of the S to be more than 90% is 780min, and the sulfur capacity in each gram of copper-based adsorbent is 235.2 mg;
adsorbent Pair H in application example 52The S removal effect is shown in FIG. 7. from FIG. 7, it can be seen that the adsorbent is coupled to H2The time for maintaining the removal efficiency of S over 90 percent is 420min, and the sulfur capacity in each gram of the copper-based adsorbent is 126.4 mg.
Although the above embodiments have been described in detail, they are only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and all of the embodiments belong to the protection scope of the present invention.
Claims (10)
1. The preparation method of the copper-based adsorbent is characterized by comprising the following steps:
and mixing and roasting a nitrogen source, a carbon source and a copper source to obtain the copper-based adsorbent.
2. The method of claim 1, wherein the nitrogen source comprises one or more of urea, melamine, and biuret;
the carbon source comprises one or more of glucose, sucrose and starch;
the copper source comprises a copper salt.
3. The preparation method according to claim 2, wherein the mass ratio of the nitrogen source, the carbon source and the copper source is (2-10): (1-4): (1-6).
4. The method according to claim 1, wherein the mixing is carried out by grinding; the grinding time is 10-30 min.
5. The preparation method according to claim 1, wherein the roasting temperature is 300-700 ℃ and the roasting time is 2-5 h; the heating rate of heating to the roasting temperature is 2-10 ℃/min.
6. The copper-based adsorbent prepared by the preparation method of any one of claims 1 to 5, wherein the copper-based adsorbent is carbon-nitrogen-doped copper oxide.
7. Use of the copper-based adsorbent of claim 6 in removing H2In SApplication is carried out.
8. The application according to claim 7, characterized in that it comprises the following steps:
will contain H2And carrying out gas-solid reaction on the S gas and the copper-based adsorbent to obtain the inactivated copper-based adsorbent.
9. The use according to claim 8, wherein the copper-based adsorbent is added in an amount of 0.1 to 0.5 g;
said compound containing H2H in S gas2The concentration of S is 400-1000 ppm; said compound containing H2The flow rate of the S gas is 80-120 mL/min.
10. The use according to claim 8, wherein the gas-solid reaction temperature is 60-110 ℃.
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