CN109485101B - Method for preparing nanoscale carbon-coated magnetic ferroferric oxide by taking backwashing iron mud as raw material - Google Patents
Method for preparing nanoscale carbon-coated magnetic ferroferric oxide by taking backwashing iron mud as raw material Download PDFInfo
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- CN109485101B CN109485101B CN201811476793.9A CN201811476793A CN109485101B CN 109485101 B CN109485101 B CN 109485101B CN 201811476793 A CN201811476793 A CN 201811476793A CN 109485101 B CN109485101 B CN 109485101B
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 49
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000011001 backwashing Methods 0.000 title claims abstract description 11
- 239000002994 raw material Substances 0.000 title claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000010802 sludge Substances 0.000 claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 16
- -1 iron ions Chemical class 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 239000008103 glucose Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000011572 manganese Substances 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 239000002699 waste material Substances 0.000 abstract description 9
- 238000011282 treatment Methods 0.000 abstract description 8
- 238000004064 recycling Methods 0.000 abstract description 3
- 239000012847 fine chemical Substances 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 7
- 235000013980 iron oxide Nutrition 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910006540 α-FeOOH Inorganic materials 0.000 description 1
- 229910006299 γ-FeOOH Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Compounds Of Iron (AREA)
Abstract
A method for preparing nano-scale carbon-coated magnetic ferroferric oxide by taking backwashing iron mud as a raw material belongs to the field of water treatment waste recycling and inorganic fine chemical and engineering application. Aiming at the problem that a large amount of waste iron sludge generated by a water treatment plant taking underground water rich in iron elements as a water source cannot be recycled, a novel method for preparing nano-scale carbon-coated magnetic ferroferric oxide from waste iron sludge is provided. According to the method, waste iron mud is used for providing an iron source, and the nano-scale carbon-coated magnetic ferroferric oxide is prepared by a hydrothermal method.
Description
The technical field is as follows:
the invention belongs to the field of water treatment waste recycling and inorganic fine chemical industry.
Background art:
in recent years, magnetic ferroferric oxide materials have been widely used in the fields of water treatment, catalysis, dyeing, high magnetic recording, biosensing and the like due to their special physicochemical properties such as electrical and magnetic properties. The nanometer-level ferroferric oxide has larger specific surface area, stronger catalytic activity and the like due to the fact that the particle size of the nanometer-level ferroferric oxide is in the nanometer level, so that the nanometer-level ferroferric oxide draws the attention of a plurality of researchers, and explores a plurality of methods for preparing the nanometer-level magnetic ferroferric oxide.
The magnetic ferroferric oxide is not stable in chemical property, so that the magnetic ferroferric oxide is not suitable for long-time storage; furthermore, the particle agglomeration phenomenon is liable to occur due to the influence of the acting force (van der Waals force and magnetic force) existing on the particle surface. Therefore, the research on the surface modification of the nano magnetic ferroferric oxide particles is carried out. Recently, the ferroferric oxide material coated by carbon-based shell is concerned about due to larger specific surface area and more stable chemical property, and a plurality of related researchers explore a plurality of methods for preparing nano-scale carbon-coated magnetic ferroferric oxide by pure chemicals.
The invention relates to a method for preparing nano-scale carbon-coated magnetic ferroferric oxide by taking backwashing iron mud as a raw material. The water treatment plant using the underground water with the excessive iron as a water source can lead the ferrous iron in the water body to generate stable iron oxide solids (the main components are indefinite ferric hydroxide, alpha-FeOOH and gamma-FeOOH with poor crystallization) by a biological purification filter layer method, thereby being intercepted by the filter layer, purifying the water quality, and finally discharging the generated iron oxide along with the back flush of the filter tank. A large number of iron-containing underground water treatment plants in China generate a large amount of iron-containing mud backwashing water every year, and the direct discharge can cause serious pollution to water bodies. The invention tries to synthesize the nano-scale carbon-coated magnetic ferroferric oxide by using the backwashing iron oxide (also called iron mud) as an iron source, thereby not only saving the cost for treating the waste iron mud, but also realizing the resource recycling of the iron mud.
The invention content is as follows:
the invention is realized by the following technical scheme:
a preparation method of nanoscale carbon-coated magnetic ferroferric oxide comprises the following two steps: comprises (1) purification and concentration of iron ions and (2) preparation of nano-scale carbon-coated magnetic ferroferric oxide;
(1) and (3) purifying and concentrating iron ions: standing and precipitating the backwashing wastewater of the biological filter for removing iron and manganese in the water plant for 2-5 days, and drying the sludge at the bottom for subsequent use. Adding the iron mud into hydrochloric acid, continuously stirring for 1 hour, standing for 8-14 hours, taking out supernatant after solid matters are precipitated, adding NaOH solution to adjust pH so that iron ions in the solution generate precipitates, after solid-liquid separation, adding hydrochloric acid again to dissolve the precipitates, evaporating and concentrating the obtained solution, and waiting for subsequent reaction for later use.
(2) Preparing nano-scale carbon-coated magnetic ferroferric oxide: dissolving glucose and urea in the prepared iron solution, and magnetically stirring for 30-60 min to make the solution free of solid matter residue. Transferring the solution to a polytetrafluoroethylene lining high-pressure reaction kettle, screwing the reaction kettle, and sealing the kettle body. Then the reaction kettle is placed into an oven and kept at 200 ℃ for 12-16 hours at 180 ℃. Naturally cooling the reaction kettle to room temperature, opening the reaction kettle, taking out the generated black precipitate, dispersing for 5min under ultrasonic wave, washing with distilled water for 5-7 times, and separating water from the product by an external magnetic field during the washing process. Finally, the obtained product is put into a drying oven and dried for 4 to 8 hours at the temperature of between 50 and 60 ℃ to obtain the nano-scale carbon-coated magnetic ferroferric oxide.
Further, the raw material is derived from waste iron mud of water treatment plants or other industrial waste iron oxides (mainly ferric iron).
Further, the concentrations of hydrochloric acid and NaOH used in the step (1) are 3mol/L and 1mol/L, respectively.
Further, the added iron mud and the hydrochloric acid can be mixed according to the proportion of 12-15g of iron mud: 100-120ml hydrochloric acid.
Further, NaOH solution is added in the step (1) to adjust the pH value to 3.1-3.7, so that most of iron ions in the solution are precipitated.
Further, the mass ratio of the iron ions, the glucose and the urea in the hydrothermal reaction process in the step (2) is as follows: 0.009-0.01mol:0.01-0.012mol:0.1-0.12 mol.
Furthermore, in the step (2), the drying temperature can be 60 ℃, and the drying time can be 5 hours.
The nanometer carbon-coated magnetic ferroferric oxide powder can be prepared by using the back washing iron mud as the raw material through the process, and the method has the following advantages: in the preparation process, all iron elements come from water treatment waste (back washing iron mud), so that the resource utilization of the waste is realized.
Secondly, the generated carbon-based coated ferroferric oxide powder is more stable and is more beneficial to storage in natural environment.
Description of the drawings:
FIG. 1 is a TEM image of a nanoscale carbon-coated magnetic ferroferric oxide obtained by the present invention;
FIG. 2 is a TEM image of a carbon coating layer of nanoscale carbon-coated magnetic ferroferric oxide obtained by the present invention;
the specific implementation mode is as follows:
a preparation method of nanoscale carbon-coated magnetic ferroferric oxide comprises the following two steps: comprises (1) purification and concentration of iron ions and (2) preparation of nano-scale carbon-coated magnetic ferroferric oxide;
(1) and (3) purifying and concentrating iron ions: standing and precipitating the backwashing wastewater of the biological filter for removing iron and manganese in the water plant for 2-5 days, and drying the sludge at the bottom for subsequent use. Adding 15g of iron mud into 100ml of 3mol/L hydrochloric acid, continuously stirring, standing, taking out supernatant after solid substances are precipitated, adding 1mol/L NaOH solution to adjust the pH value to 3.3 so that iron ions in the solution generate precipitates, after solid-liquid separation, adding hydrochloric acid again to dissolve the precipitates, evaporating and concentrating the obtained solution, detecting the concentration of the iron ions in the solution to 14g/L, and waiting for subsequent reaction for later use.
(2) Preparing nano-scale carbon-coated magnetic ferroferric oxide: about 3g of glucose and 12g of urea were dissolved in 60ml of the iron solution prepared above, and stirred. The solution was transferred to a 100ml teflon lined autoclave. The reaction vessel was then placed in an oven and held at 180 ℃ for 14 hours. Naturally cooling the reaction kettle to room temperature, opening the reaction kettle, taking out the generated black precipitate, washing with distilled water for 5-7 times, and separating water from the product by an external magnetic field during washing. And finally, drying the obtained product to obtain about 2.5g of nano-scale carbon-coated magnetic ferroferric oxide. The specific saturation magnetization of the obtained product at room temperature can reach 33.51emu/g, solid-liquid separation can be easily realized from a water body under an external magnetic field, and the product can be stored for at least more than 10 months under a sealed condition.
Claims (4)
1. A method for preparing nano-scale carbon-coated magnetic ferroferric oxide by taking backwashing iron mud as a raw material is characterized by comprising the following steps of: the preparation process is divided into two steps: comprises (1) purification and concentration of iron ions and (2) preparation of nano-scale carbon-coated magnetic ferroferric oxide;
(1) and (3) purifying and concentrating iron ions: standing and precipitating the backwash wastewater of the iron and manganese removal biofilter of the water plant for 2-5 days, and drying sludge at the bottom to obtain backwash iron mud for subsequent use; adding iron mud into hydrochloric acid, continuously stirring for 1 hour, standing for 8-14 hours, taking out supernatant after solid substances are precipitated, adding NaOH solution to adjust pH so that iron ions in the solution generate precipitates, after solid-liquid separation, adding hydrochloric acid again to dissolve the precipitates, evaporating and concentrating the obtained solution to obtain an iron solution, and standing for later use after subsequent reaction; adding NaOH solution to adjust the pH value to 3.1-3.7;
(2) preparing nano-scale carbon-coated magnetic ferroferric oxide: dissolving glucose and urea in the iron solution prepared in the step (1), and magnetically stirring for 30-60 minutes to ensure that the solution has no solid matter residue; wherein the mass ratio of the iron ions, the glucose and the urea is as follows: 0.009-0.01mol:0.01-0.012mol:0.1-0.12 mol; transferring the solution to a polytetrafluoroethylene lining high-pressure reaction kettle, screwing the reaction kettle, and sealing the kettle body; then the reaction kettle is placed in an oven and kept at the temperature of 180 ℃ and 200 ℃ for 12-16 hours; naturally cooling the reaction kettle to room temperature, opening the reaction kettle, taking out the generated black precipitate, dispersing for 5min under ultrasonic waves, washing with distilled water for 5-7 times, and separating water from the product by an external magnetic field in the washing process; finally, the obtained product is put into a drying oven and dried for 4 to 8 hours at the temperature of between 50 and 60 ℃ to obtain the nano-scale carbon-coated magnetic ferroferric oxide.
2. The method for preparing nano-scale carbon-coated magnetic ferroferric oxide according to claim 1, wherein the method comprises the following steps: the concentrations of hydrochloric acid and NaOH used in the step (1) are respectively 3mol/L and 1 mol/L.
3. The method for preparing nano-scale carbon-coated magnetic ferroferric oxide according to claim 1, wherein the method comprises the following steps: adding 12-15g of iron mud and hydrochloric acid in the amount of the iron mud added in the step (1): 100-120mL hydrochloric acid.
4. The method for preparing nano-scale carbon-coated magnetic ferroferric oxide according to claim 1, wherein the method comprises the following steps: and (3) selecting the drying temperature of 60 ℃ in the step (2), and drying for 5 hours.
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| CN102442658A (en) * | 2011-10-10 | 2012-05-09 | 西南石油大学 | Preparation method for magnetic carbon-coated ferroferric oxide nano-composite material |
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| CN104445436A (en) * | 2014-12-04 | 2015-03-25 | 黑龙江大学 | Method for preparing nanometer ferroferric oxide by taking waterworks sludge as raw material |
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Patent Citations (6)
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Inventor after: Zeng Huiping Inventor after: Zhai Longxue Inventor after: Li Dong Inventor after: Zhang Jie Inventor after: Qiao Tongda Inventor before: Zeng Huiping Inventor before: Qiao Tongda Inventor before: Li Dong Inventor before: Zhang Jie |
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