CN110194457A - A kind of SiO2The preparation method and size of hollow nanometer rods regulate and control method - Google Patents
A kind of SiO2The preparation method and size of hollow nanometer rods regulate and control method Download PDFInfo
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- CN110194457A CN110194457A CN201910416694.XA CN201910416694A CN110194457A CN 110194457 A CN110194457 A CN 110194457A CN 201910416694 A CN201910416694 A CN 201910416694A CN 110194457 A CN110194457 A CN 110194457A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 45
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 45
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 45
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 45
- 229910002588 FeOOH Inorganic materials 0.000 claims abstract description 44
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 150000002505 iron Chemical class 0.000 claims abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 11
- 239000010703 silicon Substances 0.000 claims abstract description 11
- 238000005554 pickling Methods 0.000 claims abstract description 10
- 239000012266 salt solution Substances 0.000 claims abstract description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims abstract description 6
- 239000012265 solid product Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical group CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 2
- XXZNHVPIQYYRCG-UHFFFAOYSA-N trihydroxy(propoxy)silane Chemical compound CCCO[Si](O)(O)O XXZNHVPIQYYRCG-UHFFFAOYSA-N 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 6
- 238000006482 condensation reaction Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000002775 capsule Substances 0.000 abstract description 2
- 238000005253 cladding Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- JKGITWJSGDFJKO-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical compound CCO[Si](O)(O)O JKGITWJSGDFJKO-UHFFFAOYSA-N 0.000 abstract 1
- 239000012467 final product Substances 0.000 description 14
- 238000002441 X-ray diffraction Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000003001 depressive effect Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002073 nanorod Substances 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- HQSJYYLBSBNWCH-UHFFFAOYSA-N C(CC)(=O)OCCC.[Si] Chemical compound C(CC)(=O)OCCC.[Si] HQSJYYLBSBNWCH-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002328 demineralizing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
Abstract
The invention discloses a kind of SiO2The preparation method of hollow nanometer rods, sequentially includes the following steps: step 1, prepares presoma FeOOH nanometer rods；Step 2 prepares intermediate FeOOH@SiO2, FeOOH nanometer rods made from step 1 are separated into suspension, ammonium hydroxide is added and silicon source is reacted, then collects solid product, it is post-treated to obtain intermediate FeOOH@SiO2；Step 3, pickling reaction removal FeOOH, prepares SiO2Hollow nanometer rods.Invention additionally discloses a kind of SiO2The draw ratios of hollow nanometer rods regulates and controls method, increased as improving the concentration of iron salt solutions in step 1 made from FeOOH nanometer rods draw ratio, to increase SiO2The draw ratio of hollow nanometer rods.The utility model has the advantages that the present invention directly carries out SiO to FeOOH using cheap FeOOH as template, using the condensation reaction of ethyl orthosilicate2Cladding, obtains monodispersed SiO by pickling2Hollow rod-shape capsule, product morphology is complete, and entire preparation method is simple, and synthesis condition is mild, easy to operate, at low cost, is suitble to mass production.
Description
Technical field
The invention belongs to SiO2A kind of field of nano material preparation, and in particular to SiO2The preparation method of hollow nanometer rods and
Size regulates and controls method.
Background technique
Due to its stable chemical property, SiO2Material has in fields such as optics, electronics, refractory materials to be widely applied.
One-dimensional rod-like Nano-meter SiO_22, have compared with big L/D ratio, show special optical characteristics.Hollow Nano SiO2, there is high-ratio surface
Long-pending and internal cavity structures, can be used as the carrier of drug, catalyst.SiO2Hollow nanometer rods have because of its distinctive structure
Unique functionality.For example, by SiO2Hollow nanometer rods load Fe3O4Equal magnetisable materials, available one-dimensional hollow magnetic carrier,
Larger torque is obtained in magnetic field.
SiO2Hollow nanometer material is prepared frequently with template or liquid phase inductive method.Patent document CN101817530A is adopted
It is template with polystyrene microsphere, prepares hollow SiO2Nanosphere.However, it is desirable to which high-temperature heat treatment is micro- to remove polystyrene
Ball leads to SiO2Reunion and SiO2Surface fracture.Patent document CN104556069A is prepared using liquid phase method induction regulating controlling
SiO2Hollow nanometer rods, but there are preparation flow complexity, draw ratio is too small, and pattern, and can not be real close to rectangular, bad dispersibility
The problem of existing partial size and draw ratio regulate and control.In addition, the expensive raw material price that the above method uses, it is standby to be not suitable for quantifying.
Therefore, develop the SiO that a kind of preparation process is simple, low in cost, material morphology is good2Hollow nanometer rods preparation method
Have great importance.
Summary of the invention
In view of this, one of the objects of the present invention is to provide a kind of hollow SiO2The preparation method of nanometer rods.
Its technical solution is as follows:
A kind of SiO2The preparation method of hollow nanometer rods, key are to sequentially include the following steps:
Step 1 prepares presoma FeOOH nanometer rods；
Step 2 prepares intermediate FeOOH@SiO2,
FeOOH nanometer rods made from step 1 are separated into suspension, ammonium hydroxide is added and silicon source is reacted, then
Solid product is collected, it is post-treated to obtain intermediate FeOOH@SiO2；
Step 3, pickling reaction, prepares SiO2Hollow nanometer rods,
By intermediate FeOOH@SiO made from the step 22It is reacted with acid to remove FeOOH, it is post-treated to obtain
To SiO2Hollow nanometer rods.
As optimal technical scheme, in above-mentioned steps two, the FeOOH nanometer rods are distributed to be formed in ethyl alcohol it are suspended
Then liquid is added ammonium hydroxide and distilled water and is mixed into the suspension, finally puts into silicon source, be slowly stirred reaction.
As optimal technical scheme, in above-mentioned steps two, being stirred to react the time is 0.5-48h.
As optimal technical scheme, in above-mentioned steps two, being stirred to react the time is 4h.
As optimal technical scheme, in above-mentioned steps three, the reaction temperature of the pickling reaction is 60-180 DEG C.
As optimal technical scheme, in above-mentioned steps three, the reaction temperature of the pickling reaction is 80-120 DEG C.
As optimal technical scheme, in above-mentioned steps two, the silicon source is methyl orthosilicate or ethyl orthosilicate or positive silicon
Propyl propionate.
As optimal technical scheme, in above-mentioned steps one, iron salt solutions are configured to by molysite is soluble in water, merging hydro-thermal is anti-
It answers in kettle, reacts 0.5-48h at 60-150 DEG C, be then centrifuged for and with distilled water and alcohol washes, finally dry 6 at 60 DEG C
Hour, obtain FeOOH nanometer rods.
The second object of the present invention is to provide a kind of hollow SiO2The draw ratio of nanometer rods regulates and controls method.
A kind of SiO2The draw ratio of hollow nanometer rods regulates and controls method, it is critical that using such as any of the above-described preparation method
It is prepared, wherein improve the concentration of iron salt solutions in said step 1 to increase the draw ratio of FeOOH nanometer rods obtained,
To increase SiO2The draw ratio of hollow nanometer rods.
As optimal technical scheme, the concentration of above-mentioned iron salt solutions is 0.02-0.4M, the FeOOH nanometer rods obtained
Draw ratio be 2-10.
Detailed description of the invention
Fig. 1 is each stage product XRD spectrum made from embodiment 3；
Fig. 2 is final product SiO made from embodiment 4 (a, c) and embodiment 3 (b, d)2The TEM picture of hollow nanometer rods；
Fig. 3 is final product SiO made from embodiment 52Result is swept in the STEM picture of hollow nanometer rods and the face EDS；
Fig. 4 is final product SiO made from embodiment 42Result is swept in the STEM picture of hollow nanometer rods and the face EDS；
Fig. 5 is embodiment 5 (a), embodiment 6 (a) and final product SiO made from embodiment 7 (c)2The TEM of hollow nanometer rods
Picture and its length and diameter distribution map.
Specific embodiment
The invention will be further described with attached drawing with reference to embodiments.
One, SiO2The preparation of hollow nanometer rods
Step 1, in water by iron salt dissolved, and ultrasonic dissolution, iron salt solutions are configured to, 100ml iron salt solutions are set
In hydrothermal reaction kettle, it is placed in constant temperature oven and reacts, be then centrifuged for and successively cleaned several times with distilled water and alcohol, last 60
It is 6 hours dry at DEG C, obtain FeOOH nanometer rods.Molysite is FeCl3, Fe can also be used3(SO4)2Or Fe (NO3)3Add in solution
Add NaCl, is used as reactant after completely dissolution.The concentration of iron salt solutions is with Fe in solution3+Meter。
Step 2 weighs a certain amount of FeOOH nanometer rods, simultaneously ultrasound 10min is added in the ethyl alcohol of 150ml, then to above-mentioned
The ammonium hydroxide and 15ml distilled water of the 27wt.% of 5-20ml are added in solution, by gained mixed solution ultrasound 3min.It puts into a certain amount of
Silicon source, be slowly stirred reaction at room temperature.Acquired solution is centrifuged and uses water and alcohol washes 3 times, dry 4h at 60 DEG C.In obtaining
Mesosome FeOOH@SiO2.Silicon source is ethyl orthosilicate in the present embodiment, it is possible to use methyl orthosilicate or positive silicic acid propyl ester.
Step 3, by gained FeOOH@SiO2Intermediate is put into the 0.2M hydrochloric acid of 30ml, in 120 DEG C of cleaning 4h.Centrifugation
And with water and alcohol washes 3 times, and the dry 4h at 60 DEG C, obtain SiO2Hollow nanometer rods.Outside demineralizing acid, pickling reaction can make
With except HF acid in addition to inorganic acid or organic acid, such as sulfuric acid, nitric acid or acetic acid.
The specific reaction condition of the different embodiments of table one
Two, Characterization of The Products
X-ray diffraction (XRD) analysis, transmission electron microscope (TEM) analysis, scanning transmission electron microscope (STEM) point
Analysis and energy depressive spectroscopy (EDS) elemental analysis are usually used in the characterization of crystal, wherein XRD spectrum is capable of the crystalline substance of reaction test sample
Body structure can intuitively observe sample topography by scanning electron microscope (SEM), can be to sample using energy depressive spectroscopy (EDS)
Product element composition content is detected.
(1) XRD analysis
Fig. 1 is the presoma FeOOH nanometer rods prepared using the method for embodiment 3, intermediate FeOOH@SiO2Nucleocapsid knot
Structure and final product SiO2The XRD diagram of hollow nanometer rods, it was demonstrated that product is through essentially SiO after overpickling2, this and final product
White appearance it is consistent.
(2)SiO2The pattern and wall thickness of hollow nanometer rods
Final product SiO made from embodiment 42Shown in the TEM picture of hollow nanometer rods such as Fig. 2 (a, c), it can be seen that produce
Object is in apparent hollow rod-shape, and pattern is complete, and Fig. 2 (c) is single SiO in Fig. 2 (a)2The enlarged drawing of hollow nanometer rods, by Fig. 2
(c) the wall thickness about 50nm of the nanometer rods known to.
Final product SiO made from embodiment 32Shown in the TEM picture of hollow nanometer rods such as Fig. 2 (b, d), Fig. 2 (d) is Fig. 2
(b) single SiO in2The partial enlarged view of hollow nanometer rods, Fig. 2 (d) illustrate the wall thickness about 20nm of the nanometer rods.
(3) elemental analysis
Final product SiO made from embodiment 52Shown in STEM picture such as Fig. 3 (a) of hollow nanometer rods, EDS sweeps result in face
As shown in Fig. 3 (b, c, d, e), the mass percentage of Fe is 0.04at.%.
Final product SiO made from embodiment 42Shown in STEM picture such as Fig. 4 (a) of hollow nanometer rods, EDS sweeps result in face
As shown in Fig. 4 (b, c, d, e), Fe element is not detected.
Three, SiO2The size of hollow nanometer rods regulates and controls
Use the length of the FeOOH nanometer rods made from the above method for 100-1000nm.
Improve the ratio of reactant silicon source and FeOOH nanometer rods in the step 2 to increase SiO2Hollow nanometer rods
Wall thickness；The volume of the reactant silicon source and the mass ratio of FeOOH nanometer rods are 1-3 μ l/mg, the SiO obtained2It is hollow to receive
The wall thickness of rice stick is 5-200nm.
Comparing embodiment 5~7 only changes the concentration of initial reactant iron salt solutions, keeps other reaction conditions consistent, makes
The final product SiO obtained2The TEM picture of hollow nanometer rods and the nanorod diameter and length such as Fig. 5 counted according to the picture
Shown, wherein a, b, c are respectively the final product characterization result of embodiment 5, embodiment 6 and embodiment 7.
It can be seen from the figure that SiO made from three kinds of embodiments2Hollow nanorod length and width show good
Unimodal Distribution characteristic, average-size are as shown in Table 2.It follows that in the initial reaction for preparing FeOOH nanometer rods, in solution
Fe3+Concentration is higher, and obtained FeOOH draw ratio is bigger.Since the hydrolysis condensation reaction of ethyl orthosilicate is with FeOOH nanometer rods
It is carried out for template, FeOOH draw ratio is bigger, final product SiO obtained2The draw ratio of hollow nanometer rods is also bigger.
Table two changes iron salt concentration in initial reaction and regulates and controls to obtain various sizes of final product
The utility model has the advantages that the present invention is using cheap FeOOH as template, it is directly right using the condensation reaction of ethyl orthosilicate
FeOOH carries out SiO2Cladding, obtains monodispersed SiO by pickling2Hollow rod-shape capsule, product morphology are complete.Preparation method letter
It is single, it is easy to operate, and also synthesis condition is mild, does not use expensive raw material, is suitble to mass production.In addition, the present invention can be with
By changing the partial size and draw ratio of FeOOH, and change ethyl orthosilicate additive amount, direct regulation and control SiO2Hollow nanometer rods
Partial size, major diameter when SiO2Thickness.
Finally, it should be noted that foregoing description is only the preferred embodiment of the present invention, the ordinary skill people of this field
Member under the inspiration of the present invention, without prejudice to the purpose of the present invention and the claims, can make multiple similar tables
Show, such transformation is fallen within the scope of protection of the present invention.
Claims (10)
1. a kind of SiO2The preparation method of hollow nanometer rods, it is characterised in that sequentially include the following steps:
Step 1 prepares presoma FeOOH nanometer rods；
Step 2 prepares intermediate FeOOH@SiO2,
FeOOH nanometer rods made from step 1 are separated into suspension, ammonium hydroxide is added and silicon source is reacted, then collects
Solid product, it is post-treated to obtain intermediate FeOOH@SiO2；
Step 3, pickling reaction, prepares SiO2Hollow nanometer rods,
By intermediate FeOOH@SiO made from the step 22It reacts with acid to remove FeOOH, it is post-treated to obtain SiO2
Hollow nanometer rods.
2. a kind of SiO according to claim 12The preparation method of hollow nanometer rods, it is characterised in that: in the step 2,
The FeOOH nanometer rods are distributed in ethyl alcohol and form suspension, ammonium hydroxide and distilled water then is added simultaneously into the suspension
Mixing, finally puts into silicon source, is slowly stirred reaction.
3. a kind of SiO according to claim 1 or 22The preparation method of hollow nanometer rods, it is characterised in that: the step 2
In, being stirred to react the time is 0.5-48h.
4. a kind of SiO according to claim 32The preparation method of hollow nanometer rods, it is characterised in that: in the step 2,
Being stirred to react the time is 4h.
5. a kind of SiO according to claim 1 or 22The preparation method of hollow nanometer rods, it is characterised in that: the step 3
In, the reaction temperature of the pickling reaction is 60-180 DEG C.
6. a kind of SiO according to claim 52The preparation method of hollow nanometer rods, it is characterised in that: in the step 3,
The reaction temperature of the pickling reaction is 80-120 DEG C.
7. a kind of SiO according to claim 1 or 22The preparation method of hollow nanometer rods, it is characterised in that: the step 2
In, the silicon source is methyl orthosilicate or ethyl orthosilicate or positive silicic acid propyl ester.
8. a kind of SiO according to claim 1 or 22The preparation method of hollow nanometer rods, it is characterised in that: the step 1
In, iron salt solutions are configured to by molysite is soluble in water, are placed in hydrothermal reaction kettle, 0.5-48h are reacted at 60-150 DEG C, then
It is centrifuged and uses distilled water and alcohol washes, it is finally 6 hours dry at 60 DEG C, obtain FeOOH nanometer rods.
9. a kind of SiO2The size of hollow nanometer rods regulates and controls method, it is characterised in that: using preparation side as claimed in claim 8
Prepared by method, wherein improving the concentration of iron salt solutions in said step 1 to increase the major diameter of FeOOH nanometer rods obtained
Than to increase SiO2The draw ratio of hollow nanometer rods.
10. a kind of SiO according to claim 92The size of hollow nanometer rods regulates and controls method, it is characterised in that: the molysite
The concentration of solution is 0.02-0.4 M, and the draw ratio of the FeOOH nanometer rods obtained is 2-10.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111939911A (en) * | 2020-09-17 | 2020-11-17 | 中国石油大学(华东) | β-FeOOH/SiO2Preparation method and application of composite catalyst |
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| WO2014137135A1 (en) * | 2013-03-05 | 2014-09-12 | 계명대학교 산학협력단 | Method for synthesizing hollow nano-silica material |
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