CN117205883A - Method for preparing layered water treatment functional material from alkali-melting acid-leaching molybdenum tailing fine mud - Google Patents
Method for preparing layered water treatment functional material from alkali-melting acid-leaching molybdenum tailing fine mud Download PDFInfo
- Publication number
- CN117205883A CN117205883A CN202311260409.2A CN202311260409A CN117205883A CN 117205883 A CN117205883 A CN 117205883A CN 202311260409 A CN202311260409 A CN 202311260409A CN 117205883 A CN117205883 A CN 117205883A
- Authority
- CN
- China
- Prior art keywords
- fine mud
- water treatment
- functional material
- tailing fine
- molybdenum tailing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 55
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 49
- 239000011733 molybdenum Substances 0.000 title claims abstract description 49
- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000002386 leaching Methods 0.000 title claims abstract description 20
- 238000002844 melting Methods 0.000 title claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 13
- 239000000292 calcium oxide Substances 0.000 claims abstract description 12
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000002105 nanoparticle Substances 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 5
- 238000007873 sieving Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000005543 nano-size silicon particle Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 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
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 3
- 239000011707 mineral Substances 0.000 claims description 3
- 235000010755 mineral Nutrition 0.000 claims description 3
- 239000011259 mixed solution Substances 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
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000003513 alkali Substances 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 229910021645 metal ion Inorganic materials 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 230000004927 fusion Effects 0.000 abstract description 2
- 239000000378 calcium silicate Substances 0.000 description 18
- 229910052918 calcium silicate Inorganic materials 0.000 description 18
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 18
- 238000001179 sorption measurement Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 239000010949 copper Substances 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 229910001385 heavy metal Inorganic materials 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 3
- 239000000920 calcium hydroxide Substances 0.000 description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 3
- 239000004568 cement Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000008569 process Effects 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
- 239000003463 adsorbent Substances 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- -1 firstly Substances 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000004537 pulping Methods 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 238000010306 acid treatment Methods 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
- 239000011449 brick Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 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
- 230000008859 change Effects 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
- 229910001431 copper ion Inorganic materials 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000010436 fluorite 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
- 238000000227 grinding Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000464 low-speed centrifugation Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 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
- 239000010453 quartz Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000013501 sustainable material Substances 0.000 description 1
- 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
- 238000003911 water pollution Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Abstract
The invention relates to a method for preparing a layered water treatment functional material by alkali-melting acid leaching of molybdenum tailing fine mud at low cost. The method adopts a method of alkali fusion and acid leaching to treat molybdenum tailing fine mud, firstly ball-milling, crushing and sieving the molybdenum tailing fine mud, then mixing and roasting molybdenum tailing fine mud powder and sodium hydroxide, then adding a roasting product into hydrochloric acid heated by a water bath, selectively dissolving metal ions by acid leaching to form a rich porous structure, generating silicon dioxide nano particles with interparticle mesopores under the condition of no template agent, and then placing the silicon dioxide nano particles and calcium oxide in a reaction kettle together for hydrothermal reaction to obtain the lamellar water treatment functional material with good dispersibility. The invention uses the molybdenum 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 molybdenum tailing fine mud into mesoporous silica 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 layered water treatment functional material from alkali-leaching molybdenum tailing fine mud.
Background
With the rapid development of modern industry, the water pollution phenomenon is increasingly serious, and the pollution of heavy metal ions in water forms a great threat to the life health of people. The common treatment mode is an adsorption method, and the hydrated calcium silicate is used as a common water treatment functional material, has the characteristics of larger specific surface area, uniform granularity and no secondary pollution, 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. CN107721228A relates to a method for preparing hydrated calcium silicate, firstly, acid leaching the recycled aggregate for 12-48 h to obtain recycled aggregate waste liquid,then gradually adding the calcium silicate into the sodium silicate solution at the rate of 500mL/min, stirring, and carrying out suction filtration and washing to obtain the calcium silicate hydrate. However, this method has a limitation in that the acid leaching time is long and the dropping rate needs to be controlled. 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, and accumulated tailings occupy valuable storage land and 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 molybdenum tailings, fluorite tailings, vanadium titano-magnetite tailings, single magnetite tailings, gold tailings and the like. The molybdenum tailing fine mud is widely distributed in China, and has large reserves and low price. In general, molybdenum tailings fines are composed primarily of quartz and small amounts of metal oxides, where SiO 2 The content can reach more than 70 percent. The chemical composition and mineralogy of the molybdenum tailing fine mud are similar to those of clay, and are formed by [ SiO 4 ]Silicate formed by tetrahedrally formed silica framework. This indicates that the molybdenum tailing fine mud has a structure which is formed by adjusting the frameworkPotential for structuring as sustainable materials.
Disclosure of Invention
The invention provides a method for preparing a layered water treatment functional material by alkali-melting acid leaching of molybdenum tailing fine mud at low cost, which aims to solve the defects of the prior art. The method adopts a method of alkali fusion and acid leaching to treat molybdenum tailing fine mud, firstly ball-milling, crushing and sieving the molybdenum tailing fine mud, then mixing and roasting molybdenum tailing fine mud powder and sodium hydroxide, then adding a roasting product into hydrochloric acid heated by a water bath, selectively dissolving metal ions by acid leaching to form a rich porous structure, generating silicon dioxide nano particles with interparticle mesopores under the condition of no template agent, and then placing the silicon dioxide nano particles and calcium oxide in a reaction kettle together for hydrothermal reaction to obtain the lamellar water treatment functional material with good dispersibility. The invention uses the molybdenum 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 molybdenum 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:
the method for preparing the layered water treatment functional material by alkali-melting acid leaching of the molybdenum tailing fine mud at low cost comprises the following steps:
(1) The molybdenum tailing fine mud is prepared according to the mass ratio of ball ore of 3:1 to 5:1 are put into a ball mill to be ball-milled for 30 to 60 minutes at the speed of 1200 to 1800r/min; sieving the obtained tailings with a 250-2000 mesh sieve to obtain molybdenum tailings fine mud powder;
(2) Mixing the molybdenum tailing fine mud powder obtained in the step (1) with sodium hydroxide, roasting for 1-3 hours at 600-800 ℃, then adding the roasted powder into hydrochloric acid solution at one time, placing the suspension into a water bath kettle, stirring, and reacting for 1-4 hours at 60-80 ℃; cooling to room temperature after the reaction is finished; centrifuging, washing and drying the product to obtain silica nanoparticles;
wherein, the mass ratio of the molybdenum tailing fine mud powder to the sodium hydroxide is 0.8-1.5: 1, a step of; adding 5-18 g of roasted product into every 100mL of hydrochloric acid solution;
(3) Adding the obtained nano silicon dioxide particles and calcium oxide into 60-80 mL of deionized water, and then carrying out ultrasonic treatment on the mixture for 15-30 min;
wherein, the molar ratio of the calcium oxide to the nano silicon dioxide is 0.8-2;
(4) Transferring the mixed solution obtained in the step (3) into a reaction kettle, and performing hydrothermal reaction for 4-8 h at 140-180 ℃; and cooling to room temperature after the reaction is finished, and carrying out suction filtration, washing and drying on the product to obtain the layered water treatment functional material (hydrated calcium silicate).
The concentration of the hydrochloric acid solution in the step (2) is 2-4 mol/L.
The main components of the molybdenum tailing fine mud comprise: 40% -80% of SiO 2 10 to 20 percent of Al 2 O 3 2 to 8 percent of CaO and 3 to 10 percent of Fe 2 O 3 。
Application of layered water treatment functional material prepared by the method to adsorption of Cu 2+ 。
According to the method for preparing the layered water treatment functional material by the alkali-melting acid leaching of the molybdenum tailing fine mud, other raw materials, reagents and equipment except the molybdenum 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-melting acid leaching method to treat molybdenum tailing fine mud, firstly ball milling treatment is carried out to turn the molybdenum tailing fine mud into powder, then the molybdenum tailing fine mud is mixed with sodium hydroxide for roasting, the roasted product is added into hydrochloric acid heated by water bath, the acid leaching treatment selectively dissolves metal ions to form abundant porous structures, silicon dioxide nano particles with interparticle mesopores are generated, and then the silicon dioxide nano particles and calcium oxide are placed in a reaction kettle together for hydrothermal reaction, so that the lamellar water treatment functional material with good dispersibility is obtained.
Compared with the prior art, the invention has the following outstanding substantive characteristics and obvious progress:
(1) Compared with a water treatment functional material (hydrated calcium silicate) prepared by adopting a chemical reagent as a silicon source, the molybdenum tailing fine mud is used as the silicon source, so that the production cost is effectively reduced, the dispersibility of the water treatment functional material (hydrated calcium silicate) is improved, and the adsorption performance of the water treatment functional material 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 shorter production time, only needs 6-12 h, and does not need to control the dripping rate.
(4) Compared with CN108584969A, the purity of the sample prepared by the method is higher and can reach 99.5%, and no excitant is needed, so that the excessive excitant is not needed to be removed.
(5) The molybdenum 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 molybdenum 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 lamellar water treatment functional material prepared in example 1;
FIG. 2 is a TEM image of the lamellar 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 well known materials, and are particularly molybdenum tailings fine mud in the northwest of China, and the main components are shown in table 1. But is not limited thereto.
TABLE 1 Main chemical Components (wt%) of molybdenum tailings fine mud
Example 1
Weighing 10g of molybdenum tailing fine mud and 30g of grinding balls with the diameter of 3mm, adding into a ball mill, ball milling for 30min at the speed of 1800r/min, sieving with a 250-mesh sieve, mixing 10g of sieved powder with 10g of sodium hydroxide, and baking at 800 DEG CAnd (3) burning for 3 hours, adding 10g of the roasted product into 100mL of 2mol/L hydrochloric acid solution at one time, transferring the mixed solution into a water bath kettle, heating in the water bath at 75 ℃ for two hours, cooling to room temperature after heating is finished, and centrifuging, flushing and drying to obtain mesoporous nano silicon dioxide particles. Adding 0.3g (0.005 mol) of nano silicon dioxide particles and 0.42g (0.0075 mol) of calcium oxide into 70mL of deionized water, carrying out ultrasonic treatment for 15min, transferring the mixture into a reaction kettle, carrying out hydrothermal reaction for 8h at 180 ℃, cooling to room temperature, and carrying out suction filtration, flushing and drying to obtain the layered water treatment functional material. The prepared 0.05g of water treatment functional material was added to 100mL of Cu 2+ And (3) placing the copper chloride solution with the concentration of 300mg/L on a magnetic stirrer for stirring for 4 hours, and taking 10mL of the solution after stirring is finished, and placing the solution in a GNST-900 water quality tester for measuring the concentration of copper ions in the solution.
Fig. 1 is a TEM image of the lamellar water treatment function material prepared in example 1, and it can be seen that the prepared water treatment function material is lamellar.
TABLE 2 Table 2 major chemical Components of lamellar Water treatment function Material prepared in example 1
Example 2
The other steps are the same as in example 1 except that "0.3g (0.005 mol) of nano-silica particles and 0.42g (0.0075 mol) of calcium oxide were added to 70mL of deionized water" 0.3g (0.005 mol) of nano-silica particles and 0.56g (0.010 mol) of calcium oxide were replaced by "adding to 70mL of deionized water".
Fig. 2 is a TEM image of the lamellar water treatment functional material prepared in example 2, and it can be seen that although the lamellar distribution is worse than that in example 1, the lamellar distribution is uneven, the growth is irregular, and excessive calcium hydroxide and calcium carbonate are also present, the prepared water treatment functional material is still obviously lamellar. It is explained that proper change of the calcium-silicon ratio in the parameter range of the technical proposal of the invention does not affect the synthesis of the layered water treatment functional material.
Comparative example 1
The other steps differ from example 1 in that the "hydrothermal reaction at 180℃for 8h" is replaced by "hydrothermal reaction at 80℃for 8h".
In comparative example 1, the resulting product contains a large amount of calcium hydroxide, calcium carbonate and unreacted nanosilica, which may be caused by the low reaction temperature.
Comparative example 2
The other steps are different from example 1 in that "hydrothermal reaction at 180℃for 8 hours" is replaced with "hydrothermal reaction at 180℃for 1 hour".
In comparative example 2, the resulting product contained a portion of calcium hydroxide and mesoporous silica, and the reaction was not complete, which may be due to insufficient reaction time, and a portion of the raw materials were in the future and reacted.
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 589.36mg/g, example 2 was conducted on Cu 2+ The adsorption capacity of (C) is 524.36mg/g, comparative example 1 for Cu 2+ Has an adsorption capacity of 180.67mg/g, comparative example 2 was conducted on Cu 2+ The adsorption capacity of (C) was 200.76mg/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 layered water treatment functional material by a simple hydrothermal method on the basis of alkali-leaching acid treatment of the molybdenum tailings fine mud, and improves the dispersibility thereof. The preparation process is simple, the molybdenum tailing fine mud with rich reserves is used as a silicon source, the cost is low, and the molybdenum tailing fine mud 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. The method for preparing the layered water treatment functional material by alkali-melting acid leaching of the molybdenum tailing fine mud at low cost is characterized by comprising the following steps of:
(1) Placing the molybdenum tailing fine mud into a ball mill for ball milling for 30-60 min; sieving the obtained tailings with a 250-2000 mesh sieve to obtain molybdenum tailings fine mud powder;
(2) Mixing the molybdenum tailing fine mud powder obtained in the step (1) with sodium hydroxide, roasting for 1-3 hours at 600-800 ℃, adding the roasted powder into hydrochloric acid solution for one time for immersing, placing the suspension into a water bath kettle, stirring, and reacting for 1-4 hours at 60-80 ℃; cooling to room temperature after the reaction is finished; centrifuging, washing and drying the product to obtain silica nanoparticles;
wherein, the mass ratio of the molybdenum tailing fine mud powder to the sodium hydroxide is 0.8-1.5: 1, a step of; adding 5-18 g of roasted product into every 100mL of hydrochloric acid solution;
(3) Adding the obtained nano silicon dioxide particles and calcium oxide into 60-80 mL of deionized water, and then carrying out ultrasonic treatment on the mixture for 15-30 min;
wherein, the molar ratio of the calcium oxide to the nano silicon dioxide is 0.8-2;
(4) Transferring the mixed solution obtained in the step (3) into a reaction kettle, and performing hydrothermal reaction for 4-8 h at 140-180 ℃; and cooling to room temperature after the reaction is finished, and carrying out suction filtration, washing and drying on the product to obtain the layered water treatment functional material.
2. The method for preparing the layered water treatment functional material by using the alkali-melting acid-leaching molybdenum tailing fine mud, which is disclosed in claim 1, is characterized in that the concentration of the hydrochloric acid solution in the step (2) is 2-4 mol/L.
3. The method for preparing the layered water treatment functional material by the alkali-melting acid leaching molybdenum tailing fine mud, which is disclosed in claim 1, is characterized in that the rotating speed of the ball mill in the step (1) is 1200-1800 r/min; ball mineral mass ratio 3:1 to 5:1.
4. the method for preparing the layered water treatment functional material by alkali-melting acid leaching of the molybdenum tailing fine mud, which is disclosed in claim 1, is characterized in that the components of the molybdenum tailing fine mud comprise: 40% -80% of SiO 2 10 to 20 percent of Al 2 O 3 2 to 8 percent of CaO and 3 to 10 percent of Fe 2 O 3 。
5. The use of the layered water treatment functional material prepared by the method of claim 1, characterized by being used for adsorbing Cu 2+ 。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311260409.2A CN117205883A (en) | 2023-09-27 | 2023-09-27 | Method for preparing layered water treatment functional material from alkali-melting acid-leaching molybdenum tailing fine mud |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311260409.2A CN117205883A (en) | 2023-09-27 | 2023-09-27 | Method for preparing layered water treatment functional material from alkali-melting acid-leaching molybdenum tailing fine mud |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117205883A true CN117205883A (en) | 2023-12-12 |
Family
ID=89035172
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311260409.2A Pending CN117205883A (en) | 2023-09-27 | 2023-09-27 | Method for preparing layered water treatment functional material from alkali-melting acid-leaching molybdenum tailing fine mud |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117205883A (en) |
-
2023
- 2023-09-27 CN CN202311260409.2A patent/CN117205883A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101683979B (en) | New process for purifying and manufacturing microcrystalline graphite product | |
| CN107954623B (en) | Preparation method for in-situ growth of nano particles on surface of solid waste | |
| CN111874914B (en) | Method for preparing 4N high-purity quartz sand by taking pegmatite quartz as raw material | |
| CN102234116A (en) | Method for preparing nano white carbon black by utilizing iron tailings | |
| CN106315605B (en) | The method that 1.1nm tobermorites are prepared using low-grade attapulgite clay | |
| CN110284004A (en) | A kind of method that copper ashes cooperates with recycling with sodium sulphate waste residue | |
| CN101306819B (en) | Process for abstracting white carbon black from fly ash or slag | |
| CN105540623A (en) | Method for preparing nanometer magnesia | |
| CN114212799B (en) | Fly ash pretreatment method for molecular sieve preparation | |
| CN106865565A (en) | A kind of flyash synthesizes the method for X-type zeolite | |
| CN113387394A (en) | Preparation method of layered double-metal hydroxide material based on biobased calcium carbonate | |
| Li et al. | Progress in comprehensive utilization of electrolytic manganese residue: a review | |
| RU2394764C1 (en) | Method of producing silicon dioxide | |
| CN112607785A (en) | MnFe2O4/C nano composite microsphere and preparation method thereof | |
| CN101700903A (en) | Process for preparing nanometer ZnO | |
| CN102676826A (en) | Method for extracting lead from waste CRT (Cathode Ray Tube) cone glass | |
| CN117205883A (en) | Method for preparing layered water treatment functional material from alkali-melting acid-leaching molybdenum tailing fine mud | |
| CN103599765A (en) | Method for synthesizing surfactant-modified goethite | |
| CN107349900B (en) | A kind of heavy metal absorbent and its preparation | |
| CN116003050A (en) | Mortar capable of solidifying heavy metal ions in tungsten tailings and preparation method thereof | |
| CN117205882A (en) | Method for preparing two-dimensional water treatment functional material from acidified fluorite tailing fine mud | |
| CN110257851B (en) | Special electrolytic manganese dioxide for lithium manganate battery and preparation method thereof | |
| CN107352554A (en) | A kind of preparation method and application of magnetic X-type molecular sieve | |
| CN117258748A (en) | Method for preparing two-dimensional water treatment functional material from single magnetite tailing fine mud | |
| CN117299075A (en) | Method for preparing lamellar water treatment functional material from vanadium titano-magnetite tailing fine mud |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |