CN105645477B - Preparation method of ferroferric oxide - Google Patents
Preparation method of ferroferric oxide Download PDFInfo
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- CN105645477B CN105645477B CN201610164868.4A CN201610164868A CN105645477B CN 105645477 B CN105645477 B CN 105645477B CN 201610164868 A CN201610164868 A CN 201610164868A CN 105645477 B CN105645477 B CN 105645477B
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 81
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000002245 particle Substances 0.000 claims abstract description 22
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims abstract description 20
- 235000008534 Capsicum annuum var annuum Nutrition 0.000 claims abstract description 19
- 240000008384 Capsicum annuum var. annuum Species 0.000 claims abstract description 19
- 239000012153 distilled water Substances 0.000 claims abstract description 19
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 15
- 238000007789 sealing Methods 0.000 claims abstract description 15
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 229940056319 ferrosoferric oxide Drugs 0.000 claims description 25
- 239000007787 solid Substances 0.000 claims description 20
- 235000002567 Capsicum annuum Nutrition 0.000 claims description 12
- 240000004160 Capsicum annuum Species 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 229940032296 ferric chloride Drugs 0.000 claims description 10
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 7
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 241001464837 Viridiplantae Species 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 2
- 239000013049 sediment Substances 0.000 abstract 1
- 238000010008 shearing Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000001738 isopycnic centrifugation Methods 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003592 biomimetic effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
Classifications
-
- 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
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Cosmetics (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a preparation method of ferroferric oxide. The preparation method comprises the following steps: S1, preparing a sodium hydroxide (NaOH) solution and a ferric chloride solution; then extracting green pepper juice: removing seeds of green pepper, weighing the green pepper, shearing the green pepper open by a shear, putting into a mortar, adding a proper amount of distilled water, grinding, centrifuging, filtering, transferring a filtering medium into a volumetric flask for volume fixing, sealing and storing for standby application; S2, preparing the ferroferric oxide: adding the green pepper juice into the ferric chloride solution, then dropwise adding the NaOH solution until the pH is 3.5-9.5, putting into a thermostat water bath at 50-60 DEG C, and reacting for 3h; centrifuging obtained reacted matters for 10min by using a centrifuge, washing centrifuged sediment, and putting into a drying oven at 70-90 DEG C for drying, thus obtaining black ferroferric oxide particles. According to the preparation method, biomolecules in green plant juice are used, and are lower in cost and easy to get, environment pollution cannot be caused, the research requirements of green synthesis are met, and a new thought is provided for the green synthesis of the ferroferric oxide.
Description
Technical field
The invention belongs to technical field of function materials, and in particular to a kind of preparation method of ferroso-ferric oxide.
Background technology
Ferroso-ferric oxide is a kind of conventional magnetic material, also known as iron oxide black, in black or dusty blue.Four oxidation itself
Three iron molecule intermediate ion valence states are different, and electronics can be moved, so ferroso-ferric oxide can also be used as good conduction material
Material.With the gradually maturation with specific function material synthesis technology, the specific function of ferroso-ferric oxide is in magnetic recording material, spy
The aspects such as different catalyst raw material, magnetic paint, medicine have shown out.
Being used for preparing the chemical method of nano ferriferrous oxide at present has a lot, as coprecipitation, hydrothermal/solvent full-boiled process,
Microemulsion method, sol-gel process, metal-organic precursors thermal decomposition method, method of electrostatic spinning etc..The preparation process of these methods and
The pattern and property that equipment requirements have very big difference, its product is also not quite similar.It is contemplated that proposing a kind of brand-new green
Synthetic method is preparing ferroso-ferric oxide.
The content of the invention
The invention provides a kind of preparation method of ferroso-ferric oxide, the method is prepared by green syt, more environmentally friendly.
For achieving the above object, technical scheme below is present invention employs, is comprised the steps：：
S1, preparation sodium hydroxide solution：Take NaOH solids and add appropriate distillation water dissolution, after dissolving by solution shift in
In volumetric flask, plus distilled water constant volume, NaOH solution is configured to, sealing preserve is standby；
Prepare ferric chloride solution：Concentrated hydrochloric acid is slowly added dropwise in distilled water and adjusts pH in less than 2.0, take ferric chloride hexahydrate
Solid falls in wherein, and stirring makes that the solution in beaker is transferred to into constant volume in volumetric flask after solid dissolving, is configured to FeCl3It is molten
Liquid, sealing preserve is standby；
Extract green pepper juice：By Capsicum annuum L. remove seed, cut off with shears and be put in mortar, added appropriate distilled water grinding, connect
Centrifugation, is filtered, filtrate is proceeded to into constant volume sealing preserve in volumetric flask standby；
S2, prepare ferroso-ferric oxide：Green pepper juice is added in ferric chloride solution, then Deca NaOH to pH be 3.5～
9.5, it is put in thermostat water bath and reacts 3h；The reacting substance for obtaining centrifuge 10min, the precipitate after centrifugation are washed
After washing, it is placed in 70～90 DEG C of drying baker and is dried, that is, obtains the ferriferrous oxide particles of black.
Preferably, the ferric chloride hexahydrate solid is 6.7576g, and the Capsicum annuum L. is 119.5460g.
Preferably, Deca NaOH to pH is 3.5～9.5 in step S2.
Preferably, the thermostat water bath is set to 50～60 DEG C.
Preferably, the rotating speed of the centrifuge is set to 4000r/min.
Preferably, the temperature of the drying baker is set to 80 DEG C.
The beneficial effects of the present invention is：
1), the present invention combines bio-mimetic syntheses principle and chemical coprecipitation prepares ferroso-ferric oxide, using in Capsicum annuum L. juice
Vitamin biomolecule reduction FeCl3The part Fe of solution3+Generate Fe2+, then Deca sodium hydroxide solution, in green pepper juice
Biomolecule regulation and control are lower to synthesize ferroso-ferric oxide particle, and test shows, can be with green syt unformed four in Capsicum annuum L. juice
Fe 3 O.
, using the biomolecule in green plantss juice, cost is relatively low and easy acquisition, simple to operate, and will not for the present invention
To environment, meet the research requirement of green syt.
2), in the range of 3.5～9.5, the particle diameter of the ferroso-ferric oxide of generation is with pH for Deca NaOH control ph of the present invention
Value increases and increases, and can control ferroso-ferric oxide particle diameter by adjusting pH.
Description of the drawings
Fig. 1 is 4 times of mirror figures of imaged particles analysis system of pH=3.5 systems product of the present invention.
Fig. 2 is 4 times of mirror figures of imaged particles analysis system of pH=7.0 systems product of the present invention.
Fig. 3 is 4 times of mirror figures of imaged particles analysis system of pH=9.5 systems product of the present invention.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the present invention is clearly and completely retouched
State.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Embodiment 1
A kind of preparation method of ferroso-ferric oxide, specifically includes following steps：
S1, preparation sodium hydroxide solution：2.0000g NaOH solids are accurately weighed on analytical balance, appropriate steaming is added
Distilled water dissolves, and solution is shifted in 50mL volumetric flasks after dissolving, plus distilled water constant volume, is configured to the NaOH that concentration is 1mol/L
Solution, sealing preserve is standby；
Prepare ferric chloride solution：The ferric chloride hexahydrate solid of 6.7576g is accurately weighed on analytical balance, one is taken
The small beaker of 50mL adds appropriate distilled water, the drop concentrated hydrochloric acid of Deca 2～3 to adjust pH in less than 2.0, by weigh six chlorine is hydrated
Change ferrum solid to be transferred in beaker, stirred with Glass rod and the solution in beaker is transferred to into 250mL after solid dissolving to beaker
Constant volume in volumetric flask, is configured to the FeCl that concentration is 0.1mol/L3Solution, sealing preserve is standby；
Extract green pepper juice：By Capsicum annuum L. remove seed, Capsicum annuum L. 119.5460g is weighed, cut off with shears and be put in mortar, added
Appropriate distilled water grinding, ground material is centrifuged, and then filters centrifugal liquid, and filtrate proceeds to fixed in 250mL volumetric flasks
Hold sealing preserve standby；
S2, prepare ferroso-ferric oxide：The green pepper juice of 25mL is added in the ferric chloride solution of 20mL 0.1mol/L, then
The NaOH to pH of Deca 1mol/L is 3.5, is put in 55 DEG C of thermostat water bath and reacts 3h；By the reacting substance for obtaining with desk-top
Multitube equilibrium centrifugation machine is centrifuged 10min, and rotating speed is set to 4000r/min, after the precipitate washing after centrifugation, in being transferred to beaker
It is put in 80 DEG C of drying baker and is dried 8h, that is, obtain the ferriferrous oxide particles 0.0473g of black, yield is 21.87%.
It is illustrated in figure 14 times of mirror figures of imaged particles analysis system of pH=3.5 system products, it can be seen that product section is in
The random product such as circle, triangle, polygon, particle size is concentrated mainly on 2～10um.
Embodiment 2
A kind of preparation method of ferroso-ferric oxide, specifically includes following steps：
S1, preparation sodium hydroxide solution：2.0000g NaOH solids are accurately weighed on analytical balance, appropriate steaming is added
Distilled water dissolves, and solution is shifted in 50mL volumetric flasks after dissolving, plus distilled water constant volume, is configured to the NaOH that concentration is 1mol/L
Solution, sealing preserve is standby；
Prepare ferric chloride solution：The ferric chloride hexahydrate solid of 6.7576g is accurately weighed on analytical balance, one is taken
The small beaker of 50mL adds appropriate distilled water, the drop concentrated hydrochloric acid of Deca 2～3 to adjust pH in less than 2.0, by weigh six chlorine is hydrated
Change ferrum solid to be transferred in beaker, stirred with Glass rod and the solution in beaker is transferred to into 250mL after solid dissolving to beaker
Constant volume in volumetric flask, is configured to the FeCl that concentration is 0.1mol/L3Solution, sealing preserve is standby；
Extract green pepper juice：By Capsicum annuum L. remove seed, Capsicum annuum L. 119.5460g is weighed, cut off with shears and be put in mortar, added
Appropriate distilled water grinding, ground material is centrifuged, and then filters centrifugal liquid, and filtrate proceeds to fixed in 250mL volumetric flasks
Hold sealing preserve standby；
S2, prepare ferroso-ferric oxide：The green pepper juice of 25mL is added in the ferric chloride solution of 20mL 0.1mol/L, then
The NaOH to pH of Deca 1mol/L is 7, is put in 55 DEG C of thermostat water bath and reacts 3h；By the reacting substance for obtaining with desk-top many
Pipe equilibrium centrifugation machine is centrifuged 10min, and rotating speed is set to 4000r/min, after the precipitate washing after centrifugation, is transferred in beaker and puts
8h is dried in the drying baker for entering 80 DEG C, that is, obtains the ferriferrous oxide particles 0.1639g of black, yield is 75.78%.
It is illustrated in figure 24 times of mirror figures of imaged particles analysis system of pH=7 system products, it can be seen that product section is in circle
The random product such as shape, triangle, polygon, particle size is concentrated mainly on 40～60um.
Embodiment 3
A kind of preparation method of ferroso-ferric oxide, specifically includes following steps：
S1, preparation sodium hydroxide solution：2.0000g NaOH solids are accurately weighed on analytical balance, appropriate steaming is added
Distilled water dissolves, and solution is shifted in 50mL volumetric flasks after dissolving, plus distilled water constant volume, is configured to the NaOH that concentration is 1mol/L
Solution, sealing preserve is standby；
Prepare ferric chloride solution：The ferric chloride hexahydrate solid of 6.7576g is accurately weighed on analytical balance, one is taken
The small beaker of 50mL adds appropriate distilled water, the drop concentrated hydrochloric acid of Deca 2～3 to adjust pH in less than 2.0, by weigh six chlorine is hydrated
Change ferrum solid to be transferred in beaker, stirred with Glass rod and the solution in beaker is transferred to into 250mL after solid dissolving to beaker
Constant volume in volumetric flask, is configured to the FeCl that concentration is 0.1mol/L3Solution, sealing preserve is standby；
Extract green pepper juice：By Capsicum annuum L. remove seed, Capsicum annuum L. 119.5460g is weighed, cut off with shears and be put in mortar, added
Appropriate distilled water grinding, ground material is centrifuged, and then filters centrifugal liquid, and filtrate proceeds to fixed in 250mL volumetric flasks
Hold sealing preserve standby；
S2, prepare ferroso-ferric oxide：The green pepper juice of 25mL is added in the ferric chloride solution of 20mL 0.1mol/L, then
The NaOH to pH of Deca 1mol/L is 9.5, is put in 55 DEG C of thermostat water bath and reacts 3h；By the reacting substance for obtaining with desk-top
Multitube equilibrium centrifugation machine is centrifuged 10min, and rotating speed is set to 4000r/min, after the precipitate washing after centrifugation, in being transferred to beaker
It is put in 80 DEG C of drying baker and is dried 8h, that is, obtain the ferriferrous oxide particles 0.1744g of black, yield is 80.64%.
It is illustrated in figure 34 times of mirror figures of imaged particles analysis system of pH=9.5 system products, it can be seen that product section is in
The random product such as circle, triangle, polygon, particle size is concentrated mainly on 40～70um.
The imaged particles analysis system figure of comprehensive Fig. 1, Fig. 2, Fig. 3 understands that product is the ferroso-ferric oxide of irregular shape
Particle；And pH value is obtained and gradually increased, accelerate the nucleating growth speed of ferriferrous oxide particles, product grain particle diameter therefore by
It is cumulative big.
Also, due to containing vitamin C in green pepper juice, all there is 2Fe in embodiment 1,2,33++C6H8O6=C6H6O6+2Fe2+
+2H+And Fe2++2Fe3++8OH-=Fe3O4+4H2O the two reacts.While the various biomolecules coordinated regulation in green pepper juice
Fe3O4Nucleation and growth.Due to the FeCl added in pH=3.5, pH=7.0, pH=9.5 system3Liquor capacity and green pepper juice
The volume of liquid is identical, only changes the amount for adding NaOH, so products collection efficiency is mainly by OH in second step-Amount is determined：PH=3.5
OH in system-At least, so the ferroso-ferric oxide amount for generating is minimum；Secondly, pH=9.5 systems are maximum for pH=7.0 systems.
Claims (4)
1. a kind of preparation method of ferroso-ferric oxide, it is characterised in that comprise the steps：
S1, preparation sodium hydroxide solution：Take NaOH solids and add appropriate distillation water dissolution, solution is shifted in capacity after dissolving
In bottle, plus distilled water constant volume, NaOH solution is configured to, sealing preserve is standby；
Prepare ferric chloride solution：Concentrated hydrochloric acid is slowly added dropwise in distilled water and adjusts pH in less than 2.0, take ferric chloride hexahydrate solid
In wherein, stirring makes that the solution in beaker is transferred to into constant volume in volumetric flask after solid dissolving, is configured to FeCl3Solution, it is close
Envelope is saved backup；
Extract green pepper juice：By Capsicum annuum L. remove seed, cut off with shears and be put in mortar, added the grinding of appropriate distilled water, then from
The heart, filters, and filtrate is proceeded to into constant volume sealing preserve in volumetric flask standby；
S2, prepare ferroso-ferric oxide：Green pepper juice is added in ferric chloride solution, then Deca NaOH to pH is 3.5～9.5, is put
Enter and react in thermostat water bath 3h；By the reacting substance for obtaining centrifuge 10min, after the precipitate washing after centrifugation,
It is placed in 70～90 DEG C of drying baker and is dried, that is, obtains the ferriferrous oxide particles of black；
The thermostat water bath is set to 50～60 DEG C.
2. the preparation method of a kind of ferroso-ferric oxide according to claim 1, it is characterised in that：The ferric chloride hexahydrate
Solid is 6.7576g, and the Capsicum annuum L. is 119.5460g.
3. the preparation method of a kind of ferroso-ferric oxide according to claim 1, it is characterised in that：The rotating speed of the centrifuge
It is set to 4000r/min.
4. the preparation method of a kind of ferroso-ferric oxide according to claim 1, it is characterised in that：The temperature of the drying baker
It is set to 80 DEG C.
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| CN102502879A (en) * | 2011-11-02 | 2012-06-20 | 华东师范大学 | Fe3O4 nano-microsphere and preparation method thereof |
| CN105140494B (en) * | 2015-07-01 | 2017-07-18 | 齐鲁工业大学 | A kind of Fe3O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C |
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