CN115739018A - Preparation method and application of molten salt method sulfur modified porous material - Google Patents
Preparation method and application of molten salt method sulfur modified porous material Download PDFInfo
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- CN115739018A CN115739018A CN202211423446.6A CN202211423446A CN115739018A CN 115739018 A CN115739018 A CN 115739018A CN 202211423446 A CN202211423446 A CN 202211423446A CN 115739018 A CN115739018 A CN 115739018A
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 150000003839 salts Chemical class 0.000 title claims abstract description 38
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 29
- 239000011593 sulfur Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000011148 porous material Substances 0.000 title abstract description 7
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 64
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001179 sorption measurement Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims description 26
- 239000007787 solid Substances 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 12
- 238000000967 suction filtration Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 230000005496 eutectics Effects 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000003546 flue gas Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 235000011164 potassium chloride Nutrition 0.000 claims description 5
- 239000001103 potassium chloride Substances 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 229910052753 mercury Inorganic materials 0.000 abstract description 21
- 238000001354 calcination Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 2
- 238000002159 adsorption--desorption isotherm Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002715 modification method Methods 0.000 description 2
- 239000012429 reaction media Substances 0.000 description 2
- 125000004434 sulfur atom Chemical group 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- -1 i.e. Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012806 monitoring device Methods 0.000 description 1
- 238000000696 nitrogen adsorption--desorption isotherm Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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Abstract
The invention relates to a preparation method and application of a sulfur modified porous material by a molten salt method, wherein the sulfur modified porous material comprises 85-95% of activated carbon by mass and 5-15% of total sulfur by mass. The sulfur modified porous carbon material is obtained at a lower calcination temperature by a molten salt method, and the material prepared by the method has the advantages that the molecular weight of the loaded elemental sulfur is small, the elemental sulfur is combined with unsaturated active sites on the surface of the material, the elemental sulfur is not easy to lose, and the mercury modified porous carbon material has excellent mercury elemental adsorption capacity.
Description
Technical Field
The invention relates to the technical field of porous carbon material modification and coal-fired flue gas demercuration, in particular to a preparation method and application of a molten salt method sulfur-modified porous carbon material.
Background
Mercury is one of the main harmful pollutants in air, and the mercury can continuously diffuse to the surroundings along with air in the atmosphere, and once being released into the atmosphere, the mercury simple substance is difficult to capture. Mercury is highly toxic to human health and the environment, and therefore, it is imperative to control mercury emissions.
The adsorbent currently used most in the industry is a porous carbon material, i.e., activated carbon. However, the untreated activated carbon only has physical adsorption with mercury, and the adsorption capacity of the untreated activated carbon to mercury is weak. In order to improve the mercury adsorption capacity of the porous carbon material, the porous carbon material needs to be modified. At present, other elements such as halogen, metal oxide and sulfur are mainly added into the carbon material by modification methods, and the modification methods comprise solution impregnation, gas deposition, mixed heating and the like. Among them, after the sulfur-doped porous carbon material adsorbs mercury, mercury elements can be stably stored in the adsorbent in the form of HgS, which is beneficial to the post-treatment and long-term stable burying of mercury, so the research on the sulfur-doped porous carbon material is the most extensive.
However, sulfur-doped porous carbons require heating of sulfur powder to generate small molecular elemental sulfur, such as S 2 So that the preparation temperature is higher, generally about 600 ℃. And the loaded elemental sulfur is mainly subjected to physical adsorption, the elemental sulfur is easy to cover the surface of the carbon material in a large area, pore channels of the material are blocked, and the elemental sulfur is easy to fall off at a later stage, so that the mercury adsorption performance of the material is influenced.
Therefore, a new technology is developed, the modification temperature of the porous carbon material can be reduced, the binding force between the elemental sulfur and the material can be increased, and the adsorption capacity of the porous carbon material to the elemental mercury can be effectively improved.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: in order to overcome the defects in the prior art, the invention provides a preparation method of a sulfur modified porous carbon material by a molten salt method and application thereof. The modified porous carbon material prepared by the method has the characteristics of large specific surface area, uniform sulfur loading and strong mercury simple substance adsorption capacity.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a sulfur modified porous carbon material by a molten salt method comprises the following steps:
step 1: mixing and grinding sodium chloride, potassium chloride and aluminum chloride according to a proportion to prepare molten salt with a eutectic point;
step 2: mixing the molten salt, the porous carbon material and the sulfur powder into solid powder according to a mass ratio of 80-100;
and 3, step 3: pouring the solid powder obtained in the step (2) into a crucible with a screw cap, tightly covering the crucible, placing the crucible into a heating furnace, heating to 250-350 ℃ at the speed of 5-10 ℃/min, and then heating at the constant temperature of 250-350 ℃ for 4-6 h;
and 4, step 4: after heating, filtering with a metal mesh screen while the material is hot, and collecting carbon materials;
and 5: washing the carbon material with deionized water, and performing suction filtration and washing for three times to obtain a solid;
and 6: and (3) placing the solid obtained by suction filtration in an oven at the temperature of 60-80 ℃ for drying for 4-8 h, and drying to obtain the sulfur modified porous carbon material.
Preferably, the composition of the molten salt obtained in the step 1 is 15-30 wt% NaCl, 15-25 wt% KCl and 55-75 wt% AlCl 3 。
Further, the molten salt is eutectic salt, the melting point of the eutectic salt is 130-140 ℃, and the decomposition temperature is more than or equal to 600 ℃.
Preferably, the specific surface area of the porous carbon material adopted in the step 2 is 800-2000 m 2 The grain diameter is 80-200 meshes.
Preferably, the steps 1 to 4 are all completed in a glove box, and the protective gas used by the glove box is high-purity nitrogen or argon.
The sulfur content of the sulfur-modified porous carbon material obtained in the step 6 is 5-15 wt%, and the mass fraction of the activated carbon is 85-95%.
The application of the sulfur-modified porous carbon material prepared by the preparation method is to apply the sulfur-modified porous carbon material to the adsorption of elemental mercury in flue gas.
The invention has the beneficial effects that: the invention selects low-melting-point molten salt as a reaction medium, can dissolve sulfur molecules at a lower temperature, reduces the reaction temperature and avoids collapse of porous carbon material pore passages at a high temperature. Under the liquid environment, the carbon material and the sulfur molecules are mixed more uniformly. In addition, the polarity of the chlorinated molten salt is strong, so that a C-S bond can be promoted to form, a short chain is constructed, and sulfur is doped in the activated carbon more uniformly and is not easy to run off. And the S atom bonded on the carbon material has stronger mercury simple substance attraction capacity than the sulfur simple substance, thereby improving the demercuration performance of the material.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 shows NaCl-KCl-AlCl 3 DSC profile of eutectic salt.
FIG. 2 shows NaCl-KCl-AlCl 3 Graph of thermal stability of eutectic salts.
Fig. 3 is a sample view of a modified activated carbon product.
FIG. 4 is N of modified activated carbon support of example 2 Adsorption-desorption isotherm diagram.
Detailed Description
Molten salt method sulfur modified multiThe preparation method of the porous carbon material uses NaCl-KCl-AlCl according to the mass ratio 3 (0.2169.
The low-melting-point chloride molten salt prepared by the method is subjected to melting point and thermal stability tests, and the obtained curves are shown in figures 1 and 2, wherein the melting point is 125.1 ℃, and the decomposition temperature is 620 ℃.
The present invention will be described in detail with reference to the following specific examples:
example 1:
step 1: the method comprises the following steps of (1) weighing 21.69g of sodium chloride, 10.48g of potassium chloride and 67.83g of aluminum chloride according to a mass ratio (0.2169;
and 2, step: respectively weighing 100g, 6.25g and 1.25g of the molten salt, the porous carbon material and the sulfur powder obtained in the step 1 according to a mass ratio of 80;
and 3, step 3: pouring the solid powder obtained in the step (2) into a crucible with a screw cap, tightly covering the crucible, placing the crucible into a heating furnace, heating to 250 ℃ at the speed of 5 ℃/min, and then heating at the constant temperature of 250 ℃ for 5 hours;
and 4, step 4: after heating, the mixture is filtered by a metal mesh screen while the mixture is hot, and the carbon material is collected.
And 5: and washing the carbon material with deionized water, and performing suction filtration and washing for three times to obtain a solid.
Step 6: and (3) placing the solid obtained by suction filtration in an oven at 80 ℃ for drying for 6h, and drying to obtain the sulfur modified porous carbon material.
Example 2:
step 1: a eutectic molten salt was prepared according to step 1 of example 1;
step 2: the method comprises the following steps of (1) respectively weighing 100g, 5.88g and 1.18g of molten salt, a porous carbon material and sulfur powder according to a mass ratio of 85;
and step 3: pouring the solid powder obtained in the step 2 into a crucible with a screw cap, tightly covering the crucible, placing the crucible into a heating furnace, heating to 250 ℃ at the speed of 5 ℃/min, and then heating at the constant temperature of 250 ℃ for 5 hours;
and 4, step 4: after heating, filtering with a metal mesh screen while the material is hot, and collecting carbon materials;
and 5: washing the carbon material with deionized water, and performing suction filtration and washing for three times to obtain a solid;
and 6: and (3) placing the solid obtained by suction filtration in an oven at 80 ℃ for drying for 6h, and drying to obtain the sulfur modified porous carbon material.
Example 3:
step 1: a eutectic point molten salt was prepared according to step 1 of example 1;
step 2: the method comprises the following steps of (1) respectively weighing 100g, 11.76g and 1.18g of molten salt, a porous carbon material and sulfur powder according to a mass ratio of 85;
and 3, step 3: pouring the solid powder obtained in the step 2 into a crucible with a screw cap, tightly covering the crucible, placing the crucible into a heating furnace, heating to 350 ℃ at the speed of 5 ℃/min, and then heating at the constant temperature of 350 ℃ for 5 hours;
and 4, step 4: after heating, filtering with a metal mesh screen while the material is hot, and collecting carbon materials;
and 5: washing the carbon material with deionized water, and performing suction filtration and washing for three times to obtain a solid;
step 6: and (3) placing the solid obtained by suction filtration in an oven at 80 ℃ for drying for 6h, and drying to obtain the sulfur modified porous carbon material.
Example 4:
step 1: a eutectic point molten salt was prepared according to step 1 of example 1;
and 2, step: respectively weighing 100g, 11.11g and 1.11g of molten salt, a porous carbon material and sulfur powder according to a mass ratio of 90;
and 3, step 3: pouring the solid powder obtained in the step (2) into a crucible with a screw cap, tightly covering the crucible, placing the crucible into a heating furnace, heating to 350 ℃ at the speed of 5 ℃/min, and then heating at the constant temperature of 350 ℃ for 5 hours;
and 4, step 4: after heating, filtering with a metal mesh screen while the material is hot, and collecting carbon materials;
and 5: washing the carbon material with deionized water, and performing suction filtration and washing for three times to obtain a solid;
and 6: and (3) placing the solid obtained by suction filtration in an oven at 80 ℃ for drying for 6h, and drying to obtain the sulfur modified porous carbon material.
FIG. 3 shows modified activated carbons obtained in examples 1 to 4.
The modified porous carbon materials obtained in examples 1 to 4 were measured for specific surface area using an ASAP-2020 physical adsorption apparatus with an N adsorbate 2 And performing nitrogen adsorption-desorption isotherm test in a liquid nitrogen environment (-196 ℃), and calculating and measuring by using a BET method. The mercury removal amount is tested by using a fixed bed simulation experiment platform, the platform mainly comprises a gas distribution and flow control device, a mercury vapor generation device, a flue gas preheating and mixing system, a fixed bed adsorption reaction device, a mercury concentration online monitoring device and a tail gas treatment device, mercury vapor in simulated flue gas is generated by a mercury permeation tube, and CO is generated by a CO (carbon monoxide) gas 2 As a carrier gas through the mercury permeation tube, the other gas components were metered by a mass flow controller. The measured parameters are shown in Table 1, and N of the activated carbon obtained in different examples 2 The adsorption-desorption isotherms are shown in figure 4:
TABLE 1 basic parameters of modified porous carbon materials
The invention selects the low-melting-point molten salt as a reaction medium, can dissolve sulfur molecules at a lower temperature, reduces the reaction temperature, and avoids the collapse of porous carbon material pore canals at a high temperature. Under the liquid state environment, the carbon material and the sulfur molecules are mixed more uniformly. In addition, the polarity of the chlorinated molten salt is strong, so that a C-S bond can be promoted to form, a short chain is constructed, and sulfur is doped in the activated carbon more uniformly and is not easy to run off.
The sulfur modified porous carbon material obtained by the preparation method is applied to the adsorption of elemental mercury in flue gas, and the S atom bonded on the carbon material has stronger mercury elemental attraction capacity than the sulfur elemental, so that the demercuration performance of the material is improved.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (7)
1. A preparation method of a molten salt sulfur modified porous carbon material is characterized by comprising the following steps: comprises the following steps:
step 1: mixing and grinding sodium chloride, potassium chloride and aluminum chloride according to a proportion to prepare molten salt with a eutectic point;
step 2: mixing the molten salt, the porous carbon material and the sulfur powder into solid powder according to a mass ratio of 80-100;
and 3, step 3: pouring the solid powder obtained in the step (2) into a crucible with a screw cap, tightly covering the crucible, placing the crucible into a heating furnace, heating to 250-350 ℃ at the speed of 5-10 ℃/min, and then heating at the constant temperature of 250-350 ℃ for 4-6 hours;
and 4, step 4: after heating, filtering with a metal mesh screen while the material is hot, and collecting carbon materials;
and 5: washing the carbon material with deionized water, and performing suction filtration and washing for three times to obtain a solid;
step 6: and (3) placing the solid obtained by suction filtration in an oven at the temperature of 60-80 ℃ for drying for 4-8 h, and drying to obtain the sulfur modified porous carbon material.
2. The method for preparing a sulfur-modified porous carbon material by a molten salt method according to claim 1, which is characterized by comprising the following steps: the molten salt obtained in the step 1 comprises 15-30 wt% of NaCl, 15-25 wt% of KCl and 55-75 wt% of AlCl 3 。
3. The method for preparing a sulfur-modified porous carbon material by a molten salt method according to claim 2, which is characterized by comprising the following steps: the molten salt is eutectic salt, the melting point is 130-140 ℃, and the decomposition temperature is more than or equal to 600 ℃.
4. The method for preparing a sulfur-modified porous carbon material by a molten salt method according to claim 1, which is characterized by comprising the following steps: the specific surface area of the porous carbon material adopted in the step 2 is 800-2000 m 2 The grain diameter is 80-200 meshes.
5. The method for preparing a sulfur-modified porous carbon material by a molten salt method according to claim 1, which is characterized by comprising the following steps: the steps 1-4 are all completed in a glove box, and the protective gas used by the glove box is high-purity nitrogen or argon.
6. The method for preparing a sulfur-modified porous carbon material by a molten salt method according to claim 1, which is characterized by comprising the following steps: the sulfur content of the sulfur-modified porous carbon material obtained in the step 6 is 5-15 wt%, and the mass fraction of the activated carbon is 85-95%.
7. Use of a sulfur-modified porous carbon material prepared according to any one of claims 1 to 6, characterized in that: the obtained sulfur modified porous carbon material is applied to the adsorption of elemental mercury in flue gas.
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