CN117258748A - Method for preparing two-dimensional water treatment functional material from single magnetite tailing fine mud - Google Patents
Method for preparing two-dimensional water treatment functional material from single magnetite tailing fine mud Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000000463 material Substances 0.000 title claims abstract description 45
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 29
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000010703 silicon Substances 0.000 claims abstract description 42
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 17
- 239000000047 product Substances 0.000 claims abstract description 16
- 239000000292 calcium oxide Substances 0.000 claims abstract description 14
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 11
- 230000008025 crystallization Effects 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 7
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 7
- 239000006228 supernatant Substances 0.000 claims abstract description 7
- 230000001105 regulatory effect Effects 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 239000003463 adsorbent Substances 0.000 abstract description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 abstract description 3
- 239000004115 Sodium Silicate Substances 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 229910052911 sodium silicate Inorganic materials 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 abstract 2
- 239000000378 calcium silicate Substances 0.000 description 16
- 229910052918 calcium silicate Inorganic materials 0.000 description 16
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 238000001179 sorption measurement Methods 0.000 description 9
- 239000010949 copper Substances 0.000 description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
- 239000003513 alkali Substances 0.000 description 6
- 229910001385 heavy metal Inorganic materials 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 238000003917 TEM image Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 4
- 239000000920 calcium hydroxide Substances 0.000 description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 239000004568 cement Substances 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
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- 239000011707 mineral Substances 0.000 description 2
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- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- OSMSIOKMMFKNIL-UHFFFAOYSA-N calcium;silicon Chemical compound [Ca]=[Si] OSMSIOKMMFKNIL-UHFFFAOYSA-N 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
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- 239000010881 fly ash Substances 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000000464 low-speed centrifugation Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Abstract
The invention relates to a method for preparing a two-dimensional water treatment functional material from single magnetite tailing fine mud. The method adopts single magnetite tailing fine mud as a silicon source, then the single magnetite tailing fine mud is mixed with sodium hydroxide for roasting, then a roasting product is placed in deionized water heated in a water bath, sodium silicate in the roasting product is leached out, then supernatant fluid is centrifugally reserved, template agent CTAB is added into the supernatant fluid, the pH value is regulated, mesoporous silicon is obtained through crystallization after the reaction is finished, and finally the obtained mesoporous silicon and calcium oxide are placed in a reaction kettle together for carrying out microwave hydrothermal reaction, so that the water treatment functional material adsorbent with good dispersibility is obtained. The invention uses the single magnetic tailing fine mud with low cost as the main raw material, and realizes the low-cost preparation of the high-performance water treatment functional material by converting the single magnetic tailing fine mud into mesoporous silicon and then preparing the high-dispersion two-dimensional water treatment functional material.
Description
Technical Field
The technical scheme of the invention relates to the field of adsorbent synthesis, in particular to a method for preparing a two-dimensional water treatment functional material from single magnetite tailing fine mud.
Background
Along with the development of industrialization, a large amount of heavy metal ions are discharged into water, and the removal of the heavy metal ions in the water by utilizing a water treatment functional material becomes an important technology. As a common water treatment functional material, the calcium silicate hydrate has relatively excellent adsorption performance and is widely used in the fields of heavy metal ion wastewater treatment and the like.
The hydrated calcium silicate has excellent application prospect in the field of heavy metal ion wastewater treatment, but the high synthesis cost and the characteristic of spontaneous agglomeration limit the application of the hydrated calcium silicate in industry. The high-performance water treatment functional material (hydrated calcium silicate) prepared by taking the tailing fine mud as a silicon source can not only effectively reduce the synthesis cost, but also reduce the environmental risk by absorbing and stacking the tailings. Therefore, the method for preparing the proper high-performance water treatment functional material has important significance.
CN112661164a discloses a method for preparing hydrated calcium silicate by using waste cement-based material and non-wood pulping black liquor as raw materials, firstly, acid treating the waste cement-based material, then mixing the waste cement-based material with the non-wood pulping black liquor with impurities filtered, and performing coprecipitation reaction for 2 hours to obtain the hydrated calcium silicate. However, the hydrated calcium silicate prepared by the method is granular, has smaller particle size and poor dispersibility. CN114275790A relates to a method for preparing hydrated calcium silicate, which comprises leaching fly ash with alkaline agent to obtain silicate leaching solution, dripping the silicate leaching solution into calcium hydroxide suspension at a constant speed of 15-35 mL/h, stirring and heating to obtain hydrated calcium silicate gel, and adding hydrated siliconThe calcium acid gel is mixed with an organic alcohol solvent and then subjected to azeotropic distillation, and then is subjected to separation, drying and roasting for reaming. However, this method has a limitation in preparation time due to the necessity of controlling the dropping rate and performing the reaming process. CN108584969a provides a method for preparing hydrated calcium silicate by using industrial steel slag, firstly, mixing sodium hydroxide solution and water glass to prepare strong alkali excitant, then adding industrial steel slag into the excitant solution, stirring and heating to obtain suspension; centrifuging the obtained suspension, removing excessive strong alkali excitant, and performing ultrasonic treatment to obtain particle suspension; then mixing with unreacted steel slag particles, and obtaining the nano calcium silicate hydrate nano-sheet after low-speed centrifugation. However, this method has a limitation in that the operation is complicated due to the requirement of an excessive amount of the activator. Eisinas team (Ceramics International,2023, 49 (9): 14886-14894) provides a one-step hydrothermal synthesis of calcium silicate hydrate using commercial calcium and silica with oxygen, but the process is costly and the calcium silicate hydrate is poorly dispersible in Cu 2+ The maximum adsorption amount of (C) was only 142mg/g.
Tailings are main industrial solid wastes generated in the processing process of metal minerals and nonmetallic minerals, the cumulative amount of the tailings in China reaches 195 hundred million tons at present, and the comprehensive rate of the tailings is only 10%. The piled tailings not only occupy valuable storage land, but also cause environmental pollution and hidden troubles of dam break, landslide and collapse. Therefore, comprehensive utilization of tailings has attracted a great deal of attention. For example, recovery of valuable metal elements, production of building materials (i.e., concrete, burned brick, glass ceramic, wall materials, etc.), manufacture of functional ceramics, and use as soil conditioners and trace element fertilizers. The common tailings mainly comprise fluorite tailings, molybdenum tailings, vanadium titano-magnetite tailings, single magnetite tailings, gold tailings and the like. And single magnetite tailings are widely distributed in China and have large reserves. In general, single magnetite tailings consist mainly of quartz and small amounts of metallic elements, where SiO 2 The content can reach more than 40 percent. The chemical composition and mineralogy of the single magnetite tailings are similar to those of clay and are formed by [ SiO 4 ]Silicate formed by tetrahedrally formed silicon dioxide framework. This suggests that single magnetite tailings have the potential to act as sustainable materials by modulating the framework structure. However, the industrial utilization is low due to the fact that impurities are difficult to completely remove, and the current research on the application is little.
Disclosure of Invention
The invention provides a method for preparing a high-dispersity two-dimensional water treatment functional material by using single magnetite tailing fine mud, which aims to solve the defects of the prior art. The method adopts single magnetite tailing fine mud after alkali fusion treatment as a silicon source, namely, firstly, the single magnetite tailing fine mud is mixed with sodium hydroxide for roasting, then, a roasting product is placed in deionized water heated by water bath, sodium silicate in the roasting product is leached out, then, supernatant liquor is centrifugally reserved, template agent CTAB is added into the supernatant liquor, pH value is regulated, crystallization is carried out after reaction is finished, mesoporous silicon is obtained, and finally, the obtained mesoporous silicon and calcium oxide are jointly placed in a reaction kettle for microwave hydrothermal reaction, so that a water treatment functional material with good dispersibility is obtained. The invention uses the single magnetic tailing fine mud with low cost as the main raw material, and realizes the low-cost preparation of the high-performance water treatment functional material by converting the single magnetic tailing fine mud into mesoporous silicon and then preparing the high-dispersion two-dimensional water treatment functional material.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for preparing a two-dimensional water treatment functional material from single magnetite tailing fine mud comprises the following steps:
(1) Mixing single magnetite tailing fine mud with sodium hydroxide according to the mass ratio of 0.8: 1-2: 1 is put in a muffle furnace for roasting for 1-4 hours at 400-800 ℃, and is cooled to room temperature after roasting is finished to obtain a roasting product;
(2) Placing the roasting product obtained in the step (1) into deionized water, placing the suspension into a water bath, heating and stirring, and cooling to room temperature after the reaction is finished; centrifuging the product, and reserving supernatant to obtain crude silicon solution;
wherein 8-20 g of roasting product is added into every 100mL of deionized water;
(3) Adding a template agent CTAB into the crude silicon solution, regulating pH, reacting for 1-4 h, then placing the crude silicon solution into a baking oven for crystallization, centrifuging and drying after the crystallization is finished to obtain mesoporous silicon;
(4) Adding the mesoporous silicon and calcium oxide obtained in the step (3) into deionized water, and then carrying out ultrasonic treatment on the mixture for 15-30 min;
wherein, every 70mL deionized water is added with 0.1-0.5 g mesoporous silicon;
(5) Transferring the mixed solution obtained in the step (3) into a reaction kettle, then placing the reaction kettle in a microwave hydrothermal synthesizer for microwave hydrothermal reaction, cooling to room temperature after the reaction is finished, and carrying out suction filtration, washing and drying on the product to obtain the two-dimensional water treatment functional material.
The heating temperature of the water bath kettle in the step (2) is 60-80 ℃, and the water bath heating time is 0.5-2 h.
The addition amount of the template agent CTAB of each 100mL of crude silicon solution in the step (3) is 0.5-2 g, the pH value is 8-12, the crystallization time is 4-24 h, and the crystallization temperature is 40-100 ℃.
The mass ratio of mesoporous silicon to calcium oxide in the step (4) is 0.5-2.
In the step (5), the microwave hydrothermal reaction temperature is 100-210 ℃ and the hydrothermal reaction time is 1-4 h.
The single magnetite tailing fine mud comprises the following components in percentage by weight: 40% -70% of SiO 2 5 to 20 percent of Al 2 O 3 5 to 25 percent of CaO and 5 to 30 percent of Fe 2 O 3 5% -15% MgO and 2% -10% other trace components.
Application of the two-dimensional water treatment functional material prepared by the method to Cu adsorption 2+ 。
The method for preparing the two-dimensional water treatment functional material by the single magnetite tailing fine mud is characterized in that other raw materials, reagents and equipment except the single magnetite tailing fine mud are obtained through known ways, and the operation process can be mastered by a person skilled in the art.
The invention has the substantial characteristics that:
the invention adopts an alkali fusion method to treat single magnetite tailing fine mud, and adds a template agent into the single magnetite tailing fine mud to enable alkali fusion activated crude silicon to generate mesoporous silicon, firstly, the single magnetite tailing fine mud and sodium hydroxide are mixed and roasted, then the crude silicon is leached out under the condition of water bath heating, then the template agent is added into the crude silicon solution to prepare mesoporous silicon, and the obtained mesoporous silicon and calcium oxide are mixed and added into a reaction kettle to carry out microwave hydrothermal reaction, thus obtaining the water treatment functional material with good dispersibility.
The beneficial effects of the invention are as follows:
(1) Compared with a water treatment functional material (hydrated calcium silicate) prepared by adopting a chemical reagent as a silicon source, the single magnetite tailing fine mud is used as the silicon source, so that the production cost is effectively reduced, and meanwhile, the process disclosed by the invention obviously improves the dispersibility of the water treatment functional material (hydrated calcium silicate) and ensures that the adsorption performance is more excellent.
(2) Compared with CN112661164A, the water treatment functional material (hydrated calcium silicate) prepared by the invention is lamellar and has better dispersibility.
(3) Compared with CN107721228A, the invention has simple production process, no need of reaming and no need of controlling the dripping rate.
(4) Compared with CN108584969A, the purity of the sample prepared by the method is higher and can reach 98.6%, and no excitant is needed, so that the excessive excitant is not needed to be removed.
(5) The single magnetite tailing fine mud has the characteristics of low price, large storage quantity, high environmental risk in storage areas and the like, and the preparation of the high-performance water treatment functional material by taking the single magnetite tailing fine mud as a main raw material accords with the development concept of changing waste into valuable.
Drawings
FIG. 1 is a TEM image of a two-dimensional water treatment functional material prepared in example 1;
FIG. 2 is a TEM image of the two-dimensional water treatment functional material prepared in example 2;
FIG. 3 is a graph of the adsorption performance of different prepared samples.
Detailed Description
The present invention will be described with reference to specific examples, but the scope of the present invention is not limited to these examples.
The tailings are known materials, specifically single magnetite tailings fine mud (particle size is smaller than 0.075 mm) in the northwest Maillard region, and the main components are shown in table 1. But is not limited thereto.
TABLE 1 Main chemical Components (wt%) of Single magnetite tailing Fine mud
Example 1
Weighing 10g of single magnetite tailing fine mud and 8g of sodium hydroxide, mixing, placing in a muffle furnace, roasting at 600 ℃ for 3 hours, and cooling to room temperature to obtain 16.2g of roasting product; then adding the mixture into 100mL of deionized water, transferring the mixture into a water bath kettle, heating in the water bath at 75 ℃ and stirring for 2 hours, cooling to room temperature after heating is completed, centrifuging, and reserving supernatant to prepare 92mL of crude silicon solution. Adding 1g of template agent CTAB into the crude silicon solution, adjusting the pH value to 10 by using 0.1M dilute hydrochloric acid to react for 2 hours, then crystallizing for 8 hours at 60 ℃, and carrying out suction filtration and washing by using alcohol after crystallization to obtain the mesoporous silicon. Adding 0.3g of mesoporous silicon and 0.42g of calcium oxide into 70mL of deionized water, carrying out ultrasonic treatment for 15min, transferring the mixture into a reaction kettle, placing the reaction kettle in a microwave hydrothermal synthesizer for carrying out microwave hydrothermal reaction for 1h at 180 ℃, cooling to room temperature, and carrying out suction filtration, flushing and drying to obtain the water treatment functional material. The prepared 0.05g of water treatment functional material was added to 100mL of Cu 2+ Placing in copper chloride solution with concentration of 400mg/L, stirring on magnetic stirrer for 4 hr, taking 10mL of the above solution after stirring, placing in GNST-900 water quality tester, and measuring Cu therein 2+ Concentration.
Fig. 1 is a TEM image of a water treatment functional material with good dispersibility prepared in example 1, and its microstructure is lamellar and uniformly distributed.
TABLE 2 Main chemical composition Table (wt%) of two-dimensional Water treatment functional Material prepared in example 1
Example 2
The other steps are the same as in example 1 except that "0.3g of mesoporous silica and 0.42g of calcium oxide are added to 70mL of deionized water" instead of "0.3g of mesoporous silica and 0.56g of calcium oxide are added to 70mL of deionized water".
TEM FIG. 2 is a TEM image of the two-dimensional water treatment functional material prepared in example 2, and it can be seen that although the ply distribution is worse than that in example 1, the ply distribution is uneven, the growth is irregular and the skeleton is loose, excessive calcium hydroxide and calcium carbonate are also present, but the prepared water treatment functional material is still obviously in a ply shape. The method shows that the synthesis of the two-dimensional water treatment functional material is not influenced by properly changing the calcium-silicon ratio in the parameter range of the technical scheme of the invention.
Comparative example 1
The other steps are different from example 1 in that "microwave hydrothermal reaction at 180℃for 1h" is replaced with "microwave hydrothermal reaction at 80℃for 1h".
In comparative example 1, the resulting products were calcium hydroxide, calcium carbonate and unreacted mesoporous silicon, indicating that the lower reaction temperature did not allow the mesoporous silicon and calcium oxide to react completely.
Comparative example 2
The other steps are different from example 1 in that "microwave hydrothermal reaction at 180℃for 1h" is replaced by "hydrothermal reaction at 180℃for 1h".
In comparative example 2, calcium hydroxide, calcium carbonate and unreacted mesoporous silicon were obtained, indicating that the mesoporous silicon and calcium oxide could not be completely reacted within 1 hour of ordinary hydrothermal reaction.
FIG. 3 is a graph of the adsorption performance of example 1, example 2, comparative example 1 and comparative example 2, wherein example 1 vs. Cu 2+ The adsorption capacity of (C) was 696.52mg/g, example 2 was conducted on Cu 2+ The adsorption capacity of (C) is 652.38mg/g, comparative example 1 for Cu 2+ Is 128.56mg/g, comparative example 2 was conducted on Cu 2+ The adsorption capacity of (C) was 110.23mg/g. It is evident that example 1 and example 2 perform better than the other samples.
As can be seen from the above examples and comparative examples, the present invention prepares a two-dimensional water treatment functional material by a simple hydrothermal method on the basis of alkali fusion treatment of single magnetite tailing fine mud, and improves the dispersibility thereof. The preparation process is simple, the tailings with rich reserves are used as a silicon source, the cost is low, and the tailings can be used as a high-quality heavy metal ion adsorbent.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
The invention is not a matter of the known technology.
Claims (5)
1. A method for preparing a two-dimensional water treatment functional material by single magnetite tailing fine mud is characterized by comprising the following steps:
(1) Mixing single magnetite tailing fine mud with sodium hydroxide according to the mass ratio of 0.8: 1-2: 1 is put in a muffle furnace for roasting for 1-4 hours at 400-800 ℃, and is cooled to room temperature after roasting is finished to obtain a roasting product;
(2) Placing the roasting product obtained in the step (1) into deionized water, placing the suspension into a water bath kettle, heating the suspension in the water bath under stirring at 60-80 ℃ for reaction for 0.5-2 h, and cooling to room temperature after the reaction is finished; centrifuging the product, and reserving supernatant to obtain crude silicon solution;
wherein 8-20 g of roasting product is added into every 100mL of deionized water;
(3) Adding a template agent CTAB into the crude silicon solution, regulating pH, reacting for 1-4 h, then placing the crude silicon solution into a baking oven for crystallization, centrifuging and drying after the crystallization is finished to obtain mesoporous silicon;
wherein, 0.5-2 g of template agent CTAB is added into each 100mL of crude silicon solution, and the pH value is 8-12;
(4) Adding the mesoporous silicon and calcium oxide obtained in the step (3) into deionized water, and then carrying out ultrasonic treatment on the mixture for 15-30 min;
wherein, every 70mL deionized water is added with 0.1-0.5 g mesoporous silicon; the mass ratio of the mesoporous silicon to the calcium oxide is 0.5-2;
(5) Transferring the mixed solution obtained in the step (3) into a reaction kettle, performing microwave hydrothermal reaction, cooling to room temperature after the reaction is finished, and performing suction filtration, washing and drying on the product to obtain the two-dimensional water treatment functional material.
2. The method for preparing the two-dimensional water treatment functional material by using the single magnetite tailing fine mud according to claim 1, wherein in the step (3), the crystallization time is 4-24 hours, and the crystallization temperature is 40-100 ℃.
3. The method for preparing the two-dimensional water treatment functional material by using the single magnetite tailing fine mud according to claim 1, wherein the microwave hydrothermal reaction temperature in the step (5) is 100-210 ℃, and the hydrothermal reaction time is 1-4 h.
4. The method for preparing the two-dimensional water treatment functional material by using the single magnetite tailing fine mud as claimed in claim 1, wherein the components and the content range of the single magnetite tailing fine mud comprise: 40% -70% of SiO 2 5 to 20 percent of Al 2 O 3 5 to 25 percent of CaO and 5 to 30 percent of Fe 2 O 3 5% -15% MgO and 2% -10% other trace components.
5. The use of the two-dimensional water treatment functional material prepared by the method as claimed in claim 1, which is characterized by being used for adsorbing Cu 2+ 。
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