CN105645477A - Preparation method of ferroferric oxide - Google Patents
Preparation method of ferroferric oxide Download PDFInfo
- Publication number
- CN105645477A CN105645477A CN201610164868.4A CN201610164868A CN105645477A CN 105645477 A CN105645477 A CN 105645477A CN 201610164868 A CN201610164868 A CN 201610164868A CN 105645477 A CN105645477 A CN 105645477A
- Authority
- CN
- China
- Prior art keywords
- preparation
- green pepper
- solution
- ferric chloride
- green
- 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.)
- Granted
Links
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, it is specifically related to the preparation method of a kind of Z 250.
Background technology
Z 250 is a kind of conventional magneticsubstance, also known as iron oxide black, in black or dusty blue. Z 250 molecule intermediate ion valency state own is different, and electronics can be moved, so Z 250 can also as good electro-conductive material. Along with having the ripe gradually of specific function material synthesis technology, the specific function of Z 250 has shown out in magnetic recording material, special catalyst raw material, magnetic paint, medicine etc.
The chemical process being used for preparing nano ferriferrous oxide at present has a lot, such as coprecipitation method, the hot method of hydrothermal/solvent, microemulsion method, sol-gel method, metallorganics precursor thermal decomposition method, method of electrostatic spinning etc. The preparation process of these methods and equipment requirements have very big difference, and the shape looks of its product and character are also not quite similar. The present invention is intended to propose a kind of brand-new green synthesis method to prepare Z 250.
Summary of the invention
The present invention provides the preparation method of a kind of Z 250, and the method is prepared by green syt, comparatively environmental protection.
For achieving the above object, present invention employs following technical scheme, comprise the steps::
S1, preparation sodium hydroxide solution: getting NaOH solid and add appropriate distilled water dissolving, shift in volumetric flask by solution after dissolving, adding distil water holds surely, is configured to NaOH solution, and sealing saves backup;
Preparation ferric chloride Solution: slow dripping adds concentrated hydrochloric acid adjustment pH in less than 2.0 in distilled water, gets ferric chloride hexahydrate solid and falls in wherein, stirring and be transferred in volumetric flask by the solution in beaker after making dissolution of solid to determine to hold, be mixed with FeCl3Solution, sealing saves backup;
Extract green pepper juice: green pepper is removed seed, is cut off with scissors and put into mortar, add the grinding of appropriate distilled water, then centrifugal, filter, filtered liquid is proceeded to and volumetric flask holds sealing surely saves backup;
S2, prepare Z 250: in ferric chloride Solution, add green pepper juice, then drip that to add NaOH to pH be 3.5��9.5, put into thermostat water bath and react 3h;The centrifugal 10min of reactive material whizzer that will obtain, after the throw out after centrifugal washs, the loft drier being placed in 70��90 DEG C is dry, namely obtains the ferriferrous oxide particles of black.
Preferably, described ferric chloride hexahydrate solid is 6.7576g, and described green pepper is 119.5460g.
Preferably, step S2 drips to add NaOH to pH be 3.5��9.5.
Preferably, described thermostat water bath is set to 50��60 DEG C.
Preferably, the rotating speed of described whizzer is set to 4000r/min.
Preferably, the temperature of described loft drier is set to 80 DEG C.
The useful effect of the present invention is:
1), the present invention prepare Z 250 in conjunction with bio-mimetic syntheses principle and chemical coprecipitation, utilize in green pepper juice VITAMIN biomolecules reduction FeCl3The part Fe of solution3+Generate Fe2+, then drip hydro-oxidation sodium solution, the biomolecules in green pepper juice synthesizes Z 250 particle under regulating and controlling, and test shows, in green pepper juice can green syt without the Z 250 of sizing.
The present invention utilizes the biomolecules in green plants juice, and cost is lower and easily obtains, simple to operate, and can not be polluted by environment, meets the research requirement of green syt.
2), the present invention drip and add NaOH control ph in 3.5��9.5 scopes, the particle diameter of the Z 250 of generation with pH value increase and increase, by regulate pH control Z 250 particle diameter.
Accompanying drawing explanation
Fig. 1 is imaged particles analytical system 4 times of mirror figure of pH=3.5 system product of the present invention.
Fig. 2 is imaged particles analytical system 4 times of mirror figure of pH=7.0 system product of the present invention.
Fig. 3 is imaged particles analytical system 4 times of mirror figure of pH=9.5 system product of the present invention.
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 described. Based on the embodiment in the present invention, those of ordinary skill in the art, not making other embodiments all obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
A preparation method for Z 250, specifically comprises the steps:
S1, preparation sodium hydroxide solution: on analytical balance, accurately take 2.0000gNaOH solid, adding appropriate distilled water to dissolve, shifted in 50mL volumetric flask by solution after dissolving, adding distil water holds surely, being configured to the NaOH solution that concentration is 1mol/L, sealing saves backup;
Preparation ferric chloride Solution: the ferric chloride hexahydrate solid accurately taking 6.7576g on analytical balance, the small beaker getting a 50mL adds appropriate distilled water, drip add 2��3 concentrated hydrochloric acids regulate pH in less than 2.0, by the ferric chloride hexahydrate solid transfer that takes in beaker, it is stirred in beaker after dissolution of solid with glass stick and it is transferred in 250mL volumetric flask by the solution in beaker to determine to hold, be configured to the FeCl that concentration is 0.1mol/L3Solution, sealing saves backup;
Extract green pepper juice: green pepper is removed seed, takes green pepper 119.5460g, cut off with scissors and put into mortar, add the grinding of appropriate distilled water, by centrifugal for ground material, then centrifugate being filtered, filtered liquid proceeds to and surely holds sealing in 250mL volumetric flask and save backup;
S2, preparing Z 250: the green pepper juice adding 25mL in the ferric chloride Solution of 20mL0.1mol/L, then dripping the NaOH to pH adding 1mol/L is 3.5, and the thermostat water bath putting into 55 DEG C reacts 3h;The desk-top multitube centrifugal 10min of equilibrium centrifugation machine of reactive material that will obtain, rotating speed is set to 4000r/min, after the throw out after centrifugal washs, transfers to the dry 8h of the loft drier putting into 80 DEG C in beaker, namely obtaining the ferriferrous oxide particles 0.0473g of black, product rate is 21.87%.
It is illustrated in figure 1 imaged particles analytical system 4 times of mirror figure of pH=3.5 system product, it can be seen that the nothing rule products such as product cross section is rounded, trilateral, Polygons, product particle diameter mainly concentrates on 2��10um.
Embodiment 2
A preparation method for Z 250, specifically comprises the steps:
S1, preparation sodium hydroxide solution: on analytical balance, accurately take 2.0000gNaOH solid, adding appropriate distilled water to dissolve, shifted in 50mL volumetric flask by solution after dissolving, adding distil water holds surely, being configured to the NaOH solution that concentration is 1mol/L, sealing saves backup;
Preparation ferric chloride Solution: the ferric chloride hexahydrate solid accurately taking 6.7576g on analytical balance, the small beaker getting a 50mL adds appropriate distilled water, drip add 2��3 concentrated hydrochloric acids regulate pH in less than 2.0, by the ferric chloride hexahydrate solid transfer that takes in beaker, it is stirred in beaker after dissolution of solid with glass stick and it is transferred in 250mL volumetric flask by the solution in beaker to determine to hold, be configured to the FeCl that concentration is 0.1mol/L3Solution, sealing saves backup;
Extract green pepper juice: green pepper is removed seed, takes green pepper 119.5460g, cut off with scissors and put into mortar, add the grinding of appropriate distilled water, by centrifugal for ground material, then centrifugate being filtered, filtered liquid proceeds to and surely holds sealing in 250mL volumetric flask and save backup;
S2, preparing Z 250: the green pepper juice adding 25mL in the ferric chloride Solution of 20mL0.1mol/L, then dripping the NaOH to pH adding 1mol/L is 7, and the thermostat water bath putting into 55 DEG C reacts 3h; The desk-top multitube centrifugal 10min of equilibrium centrifugation machine of reactive material that will obtain, rotating speed is set to 4000r/min, after the throw out after centrifugal washs, transfers to the dry 8h of the loft drier putting into 80 DEG C in beaker, namely obtaining the ferriferrous oxide particles 0.1639g of black, product rate is 75.78%.
It is illustrated in figure 2 imaged particles analytical system 4 times of mirror figure of pH=7 system product, it can be seen that the nothing rule products such as product cross section is rounded, trilateral, Polygons, product particle diameter mainly concentrates on 40��60um.
Embodiment 3
A preparation method for Z 250, specifically comprises the steps:
S1, preparation sodium hydroxide solution: on analytical balance, accurately take 2.0000gNaOH solid, adding appropriate distilled water to dissolve, shifted in 50mL volumetric flask by solution after dissolving, adding distil water holds surely, being configured to the NaOH solution that concentration is 1mol/L, sealing saves backup;
Preparation ferric chloride Solution: the ferric chloride hexahydrate solid accurately taking 6.7576g on analytical balance, the small beaker getting a 50mL adds appropriate distilled water, drip add 2��3 concentrated hydrochloric acids regulate pH in less than 2.0, by the ferric chloride hexahydrate solid transfer that takes in beaker, it is stirred in beaker after dissolution of solid with glass stick and it is transferred in 250mL volumetric flask by the solution in beaker to determine to hold, be configured to the FeCl that concentration is 0.1mol/L3Solution, sealing saves backup;
Extract green pepper juice: green pepper is removed seed, takes green pepper 119.5460g, cut off with scissors and put into mortar, add the grinding of appropriate distilled water, by centrifugal for ground material, then centrifugate being filtered, filtered liquid proceeds to and surely holds sealing in 250mL volumetric flask and save backup;
S2, preparing Z 250: the green pepper juice adding 25mL in the ferric chloride Solution of 20mL0.1mol/L, then dripping the NaOH to pH adding 1mol/L is 9.5, and the thermostat water bath putting into 55 DEG C reacts 3h; The desk-top multitube centrifugal 10min of equilibrium centrifugation machine of reactive material that will obtain, rotating speed is set to 4000r/min, after the throw out after centrifugal washs, transfers to the dry 8h of the loft drier putting into 80 DEG C in beaker, namely obtaining the ferriferrous oxide particles 0.1744g of black, product rate is 80.64%.
It is illustrated in figure 3 imaged particles analytical system 4 times of mirror figure of pH=9.5 system product, it can be seen that the nothing rule products such as product cross section is rounded, trilateral, Polygons, product particle diameter mainly concentrates on 40��70um.
The imaged particles analytical system figure of synthesizing map 1, Fig. 2, Fig. 3 is it will be seen that product is the Z 250 particle of irregular shape; And pH value obtains and increases gradually, accelerating the nucleating growth speed of ferriferrous oxide particles, therefore product grain diameter increases gradually.
Further, owing to containing vitamins C in green pepper juice, all there is 2Fe in embodiment 1,2,33++C6H8O6=C6H6O6+2Fe2++2H+And Fe2++2Fe3++8OH-=Fe3O4+4H2O these two reactions. Various biomolecules coordinated regulation Fe in green pepper juice simultaneously3O4Nucleation and growth. Due to the FeCl added in pH=3.5, pH=7.0, pH=9.5 system3Liquor capacity is identical with the volume of green pepper juice, only changes the amount adding NaOH, so product product rate is mainly by OH in the 2nd step-Amount determines: OH in pH=3.5 system-Minimum, so the Z 250 amount generated is minimum; Secondly, pH=9.5 system is maximum for pH=7.0 system.
Claims (5)
1. the preparation method of a Z 250, it is characterised in that comprise the steps:
S1, preparation sodium hydroxide solution: getting NaOH solid and add appropriate distilled water dissolving, shift in volumetric flask by solution after dissolving, adding distil water holds surely, is configured to NaOH solution, and sealing saves backup;
Preparation ferric chloride Solution: slow dripping adds concentrated hydrochloric acid adjustment pH in less than 2.0 in distilled water, gets ferric chloride hexahydrate solid and falls in wherein, stirring and be transferred in volumetric flask by the solution in beaker after making dissolution of solid to determine to hold, be mixed with FeCl3Solution, sealing saves backup;
Extract green pepper juice: green pepper is removed seed, is cut off with scissors and put into mortar, add the grinding of appropriate distilled water, then centrifugal, filter, filtered liquid is proceeded to and volumetric flask holds sealing surely saves backup;
S2, prepare Z 250: in ferric chloride Solution, add green pepper juice, then drip that to add NaOH to pH be 3.5��9.5, put into thermostat water bath and react 3h; The centrifugal 10min of reactive material whizzer that will obtain, after the throw out after centrifugal washs, the loft drier being placed in 70��90 DEG C is dry, namely obtains the ferriferrous oxide particles of black.
2. the preparation method of a kind of Z 250 according to claim 1, it is characterised in that: described ferric chloride hexahydrate solid is 6.7576g, and described green pepper is 119.5460g.
3. the preparation method of a kind of Z 250 according to claim 1, it is characterised in that: described thermostat water bath is set to 50��60 DEG C.
4. the preparation method of a kind of Z 250 according to claim 1, it is characterised in that: the rotating speed of described whizzer is set to 4000r/min.
5. the preparation method of a kind of Z 250 according to claim 1, it is characterised in that: the temperature of described loft drier is set to 80 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610164868.4A CN105645477B (en) | 2016-03-21 | 2016-03-21 | Preparation method of ferroferric oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610164868.4A CN105645477B (en) | 2016-03-21 | 2016-03-21 | Preparation method of ferroferric oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105645477A true CN105645477A (en) | 2016-06-08 |
| CN105645477B CN105645477B (en) | 2017-04-26 |
Family
ID=56495227
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610164868.4A Active CN105645477B (en) | 2016-03-21 | 2016-03-21 | Preparation method of ferroferric oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105645477B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2620432C1 (en) * | 2016-07-05 | 2017-05-25 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Российский химико-технологический университет им. Д.И. Менделеева" | Method of producing the magnetite |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012000529A1 (en) * | 2010-07-01 | 2012-01-05 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e. V. | Process for preparing magnetite or maghemite nanoparticles with controlled size using mild conditions |
| CN102502879A (en) * | 2011-11-02 | 2012-06-20 | 华东师范大学 | Fe3O4 nano-microsphere and preparation method thereof |
| CN105140494A (en) * | 2015-07-01 | 2015-12-09 | 齐鲁工业大学 | Biomimetic synthesis method of Fe3O4/Fe/C nano composite battery electrode material |
| CN105271430A (en) * | 2015-09-28 | 2016-01-27 | 江苏振宇环保科技有限公司 | Preparation method of modified super-dispersed ferriferrous oxide |
-
2016
- 2016-03-21 CN CN201610164868.4A patent/CN105645477B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012000529A1 (en) * | 2010-07-01 | 2012-01-05 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e. V. | Process for preparing magnetite or maghemite nanoparticles with controlled size using mild conditions |
| CN102502879A (en) * | 2011-11-02 | 2012-06-20 | 华东师范大学 | Fe3O4 nano-microsphere and preparation method thereof |
| CN105140494A (en) * | 2015-07-01 | 2015-12-09 | 齐鲁工业大学 | Biomimetic synthesis method of Fe3O4/Fe/C nano composite battery electrode material |
| CN105271430A (en) * | 2015-09-28 | 2016-01-27 | 江苏振宇环保科技有限公司 | Preparation method of modified super-dispersed ferriferrous oxide |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2620432C1 (en) * | 2016-07-05 | 2017-05-25 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Российский химико-технологический университет им. Д.И. Менделеева" | Method of producing the magnetite |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105645477B (en) | 2017-04-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104276595B (en) | A kind of preparation method of basic zinc chloride | |
| CN104667945A (en) | Preparation of supported palladium catalyst Fe3O4/SiO2/Pd and application of supported palladium catalyst Fe3O4/SiO2/Pd in Suzuki reaction | |
| CN102212880B (en) | Elementary substance Bi nano-structured material and preparation method and application thereof | |
| CN106119949A (en) | The preparation method of a kind of high intensity potassium titanate crystal whisker and magnetic modification application thereof | |
| CN103435096A (en) | Method for preparing size controllable nano stannic oxide | |
| CN104229900A (en) | Preparation method of alpha-Fe2O3 cubes | |
| CN103288136A (en) | Hydrothermal synthesis method of shape-controllable molybdenum dioxide submicrocrystals | |
| CN107446138B (en) | A kind of method and application preparing MIL-100 (Fe) using floride-free auxiliary agent sodium carbonate | |
| CN108892163A (en) | A method of the calcium carbonate of phase containing vaterite is prepared by chemical additives of polyacrylic acid | |
| CN105645477A (en) | Preparation method of ferroferric oxide | |
| CN105948097A (en) | Spherical cerium dioxide | |
| CN102850056A (en) | Preparation method of spherical ferrite | |
| CN102101683A (en) | Preparation method of potassium iodide | |
| US3033700A (en) | Silica-coated barium metaborate pigments and processes of producing the same | |
| CN107555491B (en) | It is co-precipitated the method that a step prepares nitrate anion intercalation cobalt aluminium houghite | |
| CN107200345B (en) | A kind of preparation method of γ-cuprous iodide | |
| CN107651712A (en) | It is co-precipitated the method that a step prepares nitrate anion intercalation NiAl-HTLcs | |
| CN106883829A (en) | A kind of regulatable TiO2Composite aqueous nano-fluids of-Au and preparation method thereof | |
| CN109499582B (en) | Composite oxide mimic enzyme material and preparation method and application thereof | |
| CN102320657A (en) | Method for preparing gamma-phase bismuth oxide | |
| CN104030363B (en) | A kind of preparation method of ferriferrous oxide nano-particle | |
| CN107555463B (en) | A kind of barium sulfate raw powder's production technology | |
| CN102730740B (en) | Method for preparing cubic crystal system cerium oxide nanocrystal | |
| CN102134746A (en) | Preparation method of alkali type magnesium chloride whisker | |
| CN104478007A (en) | Preparation method of cobaltosic oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |