CN106964318B - A kind of mesoporous silicon fiml and its an one step preparation method and purposes - Google Patents
A kind of mesoporous silicon fiml and its an one step preparation method and purposes Download PDFInfo
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Abstract
The present invention provides a kind of mesoporous silicon fiml and its an one step preparation methods and purposes to be stirred to react the preparation method is as follows: cotton is placed in sulfuric acid solution, takes out, is diluted after completion of the reaction with distilled water, stratification；Supernatant liquor is outwelled, lower layer's suspension is centrifugated, washing；Suspension after centrifugation is transferred in dialysis membrane and is dialysed, pH is adjusted, ultrasound obtains nanocrystalline cellulose, for use；It by nanocrystalline cellulose ultrasound, places in a round bottom flask, glucose is added, the mixed liquor A of diethylphosphoryl ethyl triethoxysilane and tetraethyl orthosilicate is added in stirring, stirs, and it is dry, obtain mesoporous silicon fiml A；Mesoporous silicon fiml A is placed in sulfuric acid solution and removes removing template, obtains mesoporous silicon fiml B；Mesoporous silicon fiml B is placed in concentrated hydrochloric acid and is reacted, mesoporous silicon fiml C is obtained；Mesoporous silicon fiml C distilled water and dehydrated alcohol are rinsed, drying obtains final mesoporous silicon fiml.The present invention is from a wealth of sources using biomass cellulose as template, environmentally protective.
Description
Technical field
The present invention relates to the preparation methods that a kind of pair of lanthanum has highly selective and high adsorption capacity mesoporous silicon fiml, using a step
The preparation method of synthesis, and applied to the adsorption recovery of rare-earth elements of lanthanum, belong to material preparation and separation technology field.
Background technique
Rare earth has the title of industrial " gold " that can increase substantially other productions because of physical characteristics such as its excellent photoelectromagnetics
The quality and performance of product, are accordingly used in the new material different, various in style with other materials component property.Moreover, rare earth is
Many high-tech lubricants such as electronics, laser, nuclear industry, superconduction, mainly for the manufacture of special alloy precision optics glass processed,
High refractive optics fiberboard.Catalyst as a variety of reactions, the oxidation reaction of catalytic CO, mixes when such as adulterating cadmium oxide
Catalytic CO is hydrogenated to the reaction of methane when miscellaneous palladium.The lanthana for being impregnated into lithia or zirconium oxide (1%) can be used for
Manufacture ferrimagnet.It is the very effective catalysts selective that methane oxidation coupling generates ethane and ethylene.
But by the super-strength of over half a century exploit, China rare earth resource reserves and ensure the time limit it is continuous under
Drop, main mining area resource accelerate decaying, and original mine resources are mostly exhausted.Currently, adopting, rich abandoning is poor, it is still tight to adopt the difficult phenomenon of easily abandoning
Weight, resource recovery are lower.Rare earth mining selects backward production technology and technology existing for smelting, separation, seriously destroys earth's surface plant
Quilt causes soil erosion and soil pollution, acidification, so that crop production reduction even has no harvest, to the life and health and ecology of the public
Environment brings heavy losses.Therefore, effective adsorption recovery rare earth resources have a very important significance.
With biomass nano cellulose crystals (NCC) for template, with diethylphosphoryl ethyl triethoxysilane (PETES)
Membrane material is synthesized with tetraethyl orthosilicate (TEOS), is better than powder adsorbent, convenient for continuous operation, is easily recycled.In various absorption
Tool has great advantage in material.On the one hand, which contains-PO (OH)2Function base, it not only contain can with cation into
The proton of row exchange, meanwhile, the also ≡ P=O base containing an energy directly with metal coordination, to lanthanum and cerium have it is highly selective and
High adsorption capacity；On the other hand, which is easy to amplify convenient for continuous operation, and low energy consumption, and it is " greenization that capacity usage ratio is high
The typical case of ".
Summary of the invention
The present invention be a kind of pair of lanthanum have highly selective and high adsorption capacity mesoporous silicon fiml one-step method prepare, and for pair
The selective absorption of rare earth element La in solution.
A kind of mesoporous silicon fiml, the mesoporous silicon fiml be plane in multilayer cavernous structure, helically distort it is rodlike, orientation, have
Sequence；The mesoporous silicon fiml contains-PO (OH)2Function base and ≡ P=O base that can directly with metal coordination.
A kind of two one step preparation methods of mesoporous silicon fiml, steps are as follows:
Cotton is placed in sulfuric acid solution by step 1, is stirred to react, takes out after completion of the reaction, is diluted with distilled water, stands
Layering；Supernatant liquor is outwelled, lower layer's suspension is centrifugated, washing；Suspension after centrifugation is transferred in dialysis membrane thoroughly
Analysis, adjusts pH, and ultrasound obtains nanocrystalline cellulose (NCC), for use；
Step 2, the nanocrystalline cellulose ultrasound for obtaining step 1, place in a round bottom flask, glucose are added, stir,
The mixed liquor A of diethylphosphoryl ethyl triethoxysilane (PETES) and tetraethyl orthosilicate (TEOS) is added, stirs, it is dry, it obtains
To mesoporous silicon fiml A；
Step 3, the mesoporous silicon fiml A for obtaining step 2 are placed in sulfuric acid solution and remove removing template, obtain mesoporous silicon fiml B；
Step 4, the mesoporous silicon fiml B for obtaining step 3 are placed in concentrated hydrochloric acid and react, and obtain mesoporous silicon fiml C；
Step 5, the mesoporous silicon fiml C distilled water that step 4 is obtained and dehydrated alcohol rinse, and drying obtains final Jie
Hole silicon fiml.
In step 1, the volume fraction of the sulfuric acid solution is 50~70%；It is described to be stirred to react to be stirred at 35~55 DEG C
Mix 2~4h of reaction；The molecular cut off of the dialysis membrane is 11000~15000, and dialysis time is 1~4 day；The pH is
2.4。
In step 2, the nanocrystalline cellulose (NCC), glucose, diethylphosphoryl ethyl triethoxysilane
(PETES) and the amount ratio of tetraethyl orthosilicate (TEOS) is the μ of 1mL:10~20mg:4~6 μ of L:30~50 L；The ultrasonic time
For 10~30min；Mixing time after the addition glucose is 1~3h；Whipping temp after the addition mixed liquor A is 50
~70 DEG C, the time is 2~4h；The drying be in surface plate in 20~25 DEG C drying with water bath 1~2 day.
In step 3, the sulfuric acid solution volume fraction is 30~40%；The mesoporous silicon fiml A is in sulfuric acid solution
Concentration be 10~20g/L, time of the mesoporous silicon fiml A in sulfuric acid solution be 7~10 days.
In step 4, concentration of the mesoporous silicon fiml B in concentrated hydrochloric acid is 10~20g/L；The concentration of the concentrated hydrochloric acid is 12mol/
L；The reaction temperature is 100~120 DEG C, and the reaction time is 6~8h.
The mesoporous silicon fiml is used for selective absorption lanthanum.
In the above technical solution, mesoporous silicon fiml is immersed and removes template molecule nanocrystalline cellulose in sulfuric acid solution
(NCC)。
In the above technical solution, mesoporous silicon fiml is immersed in concentrated hydrochloric acid becomes phosphate by dealkylation reaction
Group.
Nano cellulose crystal (NCC) as described in the above technical scheme, it acts as template molecules.
Glucose as described in the above technical scheme, it acts as increase toughness.
Diethylphosphoryl ethyl triethoxysilane (PETES) as described in the above technical scheme, it acts as function lists
Body.
Tetraethyl orthosilicate (TEOS) as described in the above technical scheme, it acts as host materials.
Above-mentioned mesoporous silicon fiml is applied to the lanthanum ion in adsorption aqueous solution, and specific method carries out as steps described below:
(1) lanthanum nitrate hexahydrate is accurately weighed, 200mg/L titer is configured to.Adjusting pH respectively is 2,3,4,5,6,7, point
Do not accurately weigh 10mg composite adsorption membrane material be added in 10mL colorimetric cylinder successively select the solution of different pH demarcated to
10mL investigates adsorbance, the concentration inductively coupled plasma of unadsorbed solute after standing 24 hours in 25 DEG C of water bath with thermostatic control
The measurement of body spectrometer.
(2) lanthanum nitrate hexahydrate is accurately weighed, 200mg/L titer is configured to.Titer is diluted to a series of differences
Concentration (10,25,50,75,100,125,150,175,200mg/L), and adjusting pH is 7.Weigh 10mg composite adsorption membrane material
It is added in 10mL colorimetric cylinder and various concentration lanthanum ion solution is successively selected to be demarcated to 10mL, it is quiet in 25 DEG C of waters bath with thermostatic control
It sets, investigates adsorbance after 24 hours, if the mixed liquor volume being added is V (L), the initial concentration of matched solution is C0(mg/
L), its concentration is C after certain time absorption1(mg/L), then the adsorbance Q (mg/g) of film are as follows:
Q=(C0-C1)*V/m
(3) it accurately weighs 10mg composite adsorption membrane material and is added to selection 200mg/mL standard lanthanum ion in 10mL colorimetric cylinder
Solution is demarcated to 10mL.Colorimetric cylinder is placed in 25 DEG C of water bath with thermostatic control and stands 5 respectively, 15,30,60,90,120,180,
360, after 720min；The concentration of unadsorbed solute is measured with inductively-coupled plasma spectrometer.
(4) accurately weighing 10mg composite adsorption membrane material and being added to selection concentration in 10mL colorimetric cylinder is 200mg/L's
Lanthanum, cerium, neodymium, praseodymium, samarium blending aqueous solution demarcated to 10mL, stood in 25 DEG C of insulating boxs, after 24 hours investigate absorption
Amount, the concentration of unadsorbed solute are measured with inductively-coupled plasma spectrometer.
Technological merit of the invention:
(1) with nano cellulose crystal (NCC) for template, with diethylphosphoryl ethyl triethoxysilane (PETES) and
Tetraethyl orthosilicate (TEOS) synthesizes membrane material, is better than powder adsorbent, convenient for continuous operation, is easily recycled.
(2) composite membrane is from a wealth of sources using biomass cellulose as template, environmentally protective.
(3) composite membrane contains-PO (OH)2The ≡ P=O base of function base and an energy directly with metal coordination, to lanthanum and
Cerium has highly selective and high adsorption capacity.
(4) the one-step synthesis method composite membrane is time saving and energy saving, energy saving.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of material prepared by the present invention；
Fig. 2 is the XRD diagram of material prepared by the present invention, and wherein curve (a) is the XRD diagram for not removing the material of template, curve
It (b) is the XRD diagram for removing the material of template；
Fig. 3 is that the BET of material prepared by the present invention schemes；
Fig. 4 is the adsorption isotherm map of material prepared by the present invention.
Specific embodiment
Below with reference to specific implementation example, the present invention will be further described.
Embodiment 1
(1) it takes the commercially available cotton of 10g to be placed in the sulfuric acid solution that 150mL volume fraction is 50%, is then stirred at 35 DEG C
It after reacting 2h, is transferred in beaker, is diluted to 600mL with distilled water, then overnight stand is layered, and outwells supernatant, will be suspended
Liquid centrifugation, distillation water washing remove noncrystalline three times, suspension are transferred in dialysis membrane and is dialysed 1~4 day, and adjusting pH is 2.4, so
Ultrasound 10min afterwards, it is stand-by that dilution obtains nano cellulose crystal (NCC)；
(2) NCC, the ultrasonic 20min that processing obtains in 10mL step (1) are pipetted, places in a round bottom flask, is added
100mg glucose stirs 1h, rear that 40 μ L diethylphosphoryl ethyl triethoxysilanes (PETES) and 410 μ L silicic acid tetrems are added
The mixed solution of ester (TEOS), 50 DEG C are stirred to react 2h, pour into surface plate in 25 DEG C drying with water bath 1~2 day；
(3) will synthesis obtains in step (2) mesoporous silicon fiml be placed in 500mL volume fraction be 7 in 30% sulfuric acid solution~
Remove removing template within 10 days；
(4) the processed mesoporous silicon fiml of step (3) is placed in 100mL concentrated hydrochloric acid (12mol/L), 100 DEG C of reaction 6h,
(5) mesoporous silicon fiml distilled water and dehydrated alcohol that step (4) processing obtains alternately are flushed three times, after drying
There is highly selective and high adsorption capacity mesoporous silicon fiml to lanthanum.
(6) obtained mesoporous silicon fiml is subjected to optimal adsorption pH test.
Lanthanum nitrate hexahydrate is accurately weighed, 200mg/L titer is configured to.Adjusting pH respectively is 2,3,4,5,6,7, quasi- respectively
Really weighing 10mg composite adsorption membrane material and be added in 10mL colorimetric cylinder successively selects the solution of different pH to be demarcated to 10mL,
Adsorbance, the concentration inductively-coupled plasma spectrometer of unadsorbed solute are investigated after standing 24 hours in 25 DEG C of insulating box
Measurement, obtaining optimal adsorption pH is 7
(7) obtained mesoporous silicon fiml is carried out, the assessment of thermoisopleth absorption property.
Lanthanum nitrate hexahydrate is accurately weighed, 200mg/L titer is configured to.Titer is diluted to a series of various concentrations
The solution of (10,25,50,75,100,125,150,175,200mg/L), and adjusting pH is 7.Weigh 10mg composite adsorption membrane material
Material, which is added in 10mL colorimetric cylinder, successively selects various concentration lanthanum ion solution to be demarcated to 10mL, quiet in 25 DEG C of insulating boxs
It sets, investigates adsorbance after 24 hours, if the mixed liquor volume being added is V (L), the initial concentration of matched solution is C0(mg/
L), its concentration is C after certain time absorption1(mg/L), then the adsorbance Q (mg/g) of film are as follows:
Q=(C0-C1)*V/m
(8) obtained mesoporous silicon fiml is subjected to dynamic analysis test.
Accurately weigh 10mg composite adsorption membrane material be added in 10mL colorimetric cylinder select 200mg/L titer lanthanum ion it is molten
Liquid is demarcated to 10mL.Colorimetric cylinder is placed in 25 DEG C of insulating box and stands 5 respectively, 15,30,60,90,120,180,360,
After 720min；The concentration of unadsorbed solute is measured with inductively-coupled plasma spectrometer.
(9) obtained mesoporous silicon fiml is subjected to selectivity analysis test.
Accurately weigh 10mg composite adsorption membrane material be added in 10mL colorimetric cylinder select concentration be 200mg/L lanthanum,
Cerium, neodymium, praseodymium, samarium blending aqueous solution demarcate to 10mL, stood in 25 DEG C of insulating boxs, adsorbance investigated after 24 hours, is not inhaled
The concentration of attached solute is measured with inductively-coupled plasma spectrometer.
Embodiment 2
(1) it takes the commercially available cotton of 10g to be placed in the sulfuric acid solution that 40mL volume fraction is 60%, is then stirred at 45 DEG C anti-
After answering 3h, be transferred in beaker, be diluted to 600mL with distilled water, then overnight stand be layered, outwell supernatant, will precipitate from
The heart, distillation water washing remove the mixed solution being attached in precipitating three times, precipitating are transferred in dialysis membrane and is dialysed 1~4 day, adjust pH
It is 3 in half an hour, then ultrasound 20min, dilution obtain nano cellulose crystal (NCC) for use；
(2) nano cellulose crystal (NCC) 10mL ultrasound 20min that processing obtains in removing step (1), is placed in round bottom
In flask, 130mg glucose is added, stirs 3h, it is rear be added 50 μ L diethylphosphoryl ethyl triethoxysilanes (PETES) and
The mixed solution of 400 μ L tetraethyl orthosilicates (TEOS), 60 DEG C are stirred to react 3h, pour into surface plate in 25 DEG C of drying with water baths 1~2
It；
(3) will synthesis obtains in step (2) mesoporous silicon fiml be placed in 500mL volume fraction be 7 in 35% sulfuric acid solution~
Remove removing template within 10 days；
(4) the processed mesoporous silicon fiml of step (3) is placed in 90mL concentrated hydrochloric acid (12mol/L), 110 DEG C of reaction 7h,
(5) mesoporous silicon fiml distilled water and dehydrated alcohol that step (4) processing obtains alternately are flushed three times, after drying
There is highly selective and high adsorption capacity mesoporous silicon fiml to lanthanum.
(6) obtained mesoporous silicon fiml is subjected to optimal adsorption pH test.
The lanthanum solution of 200mg/L is prepared, adjusting pH respectively is 2,3,4,5,6,7, accurately weighs 10mg sample respectively, puts respectively
In the solution for entering 10mL preparation, adsorbance is investigated after standing 24 hours in 25 DEG C of water bath with thermostatic control, the concentration of unadsorbed solute is used
Inductively-coupled plasma spectrometer measurement, it is 7 that optimal adsorption pH, which is calculated,.
(7) obtained mesoporous silicon fiml is subjected to the assessment of thermoisopleth absorption property.
Prepare 200mg/L lanthanum solution, rear gradient dilution be 175,150,125,100,75,50,25, the lanthanum of 10mg/L it is molten
Liquid accurately weighs 10mg sample respectively, is respectively put into the solution of 10mL preparation, examines after standing 24 hours in 25 DEG C of insulating box
Adsorbance is examined, the concentration of unadsorbed solute is measured with inductively-coupled plasma spectrometer.
(8) obtained mesoporous silicon fiml is subjected to dynamic analysis test.
The lanthanum solution for preparing 200mg/L, accurately weighs 10mg sample respectively, is respectively put into the solution of 10mL preparation, 25
DEG C water bath with thermostatic control in stand 5 respectively, 15,30,60,90,120,180,360, investigate adsorbance, unadsorbed solute after 720min
Concentration measured with inductively-coupled plasma spectrometer.
(9) obtained mesoporous silicon fiml is subjected to selectivity analysis test.
The blending aqueous medium solution for preparing the lanthanum of 200mg/L, cerium, neodymium, praseodymium, samarium, accurately weighs 10mg sample and is put into
In the solution that 10mL is prepared, standing adsorption investigates adsorbance, the concentration electricity consumption of unadsorbed solute afterwards for 24 hours in 25 DEG C of water bath with thermostatic control
Feel coupled plasma spectrometer measurement.
Embodiment 3
(1) it takes the commercially available cotton of 10g to be placed in the sulfuric acid solution that 150mL volume fraction is 70%, is then stirred at 55 DEG C
It after reaction 4 hours, is transferred in beaker, is diluted to 600mL with distilled water, then overnight stand is layered, and is outwelled supernatant, will be sunk
It forms sediment and is centrifuged, distillation water washing removes the mixed solution being attached in precipitating three times, and precipitating is transferred in dialysis membrane and is dialysed 1~4 day,
Adjusting pH is 2.4, then ultrasound 10min, and it is stand-by that dilution obtains nano cellulose crystal (NCC)；
(2) 10mL is pipetted after the NCC that processing obtains in removing step (1), ultrasonic 20min, is placed in a round bottom flask, is added
Enter 200mg glucose, stirs 2h, it is rear that 60 μ L diethylphosphoryl ethyl triethoxysilanes (PETES) and 390 μ L silicic acid four are added
The mixed solution of ethyl ester (TEOS), 70 DEG C are stirred to react 4h, pour into surface plate in 25 DEG C drying with water bath 1~2 day；
(3) will synthesis obtains in step (2) mesoporous silicon fiml be placed in 500mL volume fraction be 7 in 40% sulfuric acid solution~
Remove removing template within 10 days；
(4) the processed mesoporous silicon fiml of step (3) is placed in 80mL concentrated hydrochloric acid (12mol/L), 120 DEG C of reaction 8h,
(5) mesoporous silicon fiml distilled water and dehydrated alcohol that step (4) processing obtains alternately are flushed three times, after drying
There is highly selective and high adsorption capacity mesoporous silicon fiml to lanthanum.
(6) obtained mesoporous silicon fiml is subjected to optimal adsorption pH test.
The lanthanum solution of 200mg/L is prepared, adjusting pH respectively is 2,3,4,5,6,7, accurately weighs 10mg sample respectively, puts respectively
In the solution for entering 10mL preparation, adsorbance is investigated after standing 24 hours in 25 DEG C of water bath with thermostatic control, the concentration of unadsorbed solute is used
Inductively-coupled plasma spectrometer measurement, it is 7 that optimal adsorption pH, which is calculated,.
(7) obtained mesoporous silicon fiml is subjected to the assessment of thermoisopleth absorption property.
Prepare 200mg/L lanthanum solution, rear gradient dilution be 175,150,125,100,75,50,25, the lanthanum of 10mg/L it is molten
Liquid accurately weighs 10mg sample respectively, is respectively put into the solution of 10mL preparation, examines after standing 24 hours in 25 DEG C of insulating box
Adsorbance is examined, the concentration of unadsorbed solute is measured with inductively-coupled plasma spectrometer.
(8) obtained mesoporous silicon fiml is subjected to dynamic analysis test.
The lanthanum solution of 200mg/L is prepared, 10mg sample is accurately weighed respectively, is respectively put into the solution of 10mL preparation, 25
DEG C water bath with thermostatic control in stand 5 respectively, 15,30,60,90,120,180,360, investigate adsorbance, unadsorbed solute after 720min
Concentration measured with inductively-coupled plasma spectrometer.
(9) obtained mesoporous silicon fiml is subjected to selectivity analysis test.
The blending aqueous medium solution for preparing the lanthanum of 200mg/L, cerium, neodymium, praseodymium, samarium, accurately weighs 10mg sample and is put into
In the solution that 10mL is prepared, standing adsorption investigates adsorbance, the concentration electricity consumption of unadsorbed solute afterwards for 24 hours in 25 DEG C of water bath with thermostatic control
Feel coupled plasma spectrometer measurement.
Fig. 1 is the transmission electron microscope picture of material prepared by the present invention: as can be seen from the figure the composite membrane is multilayer in plane
Cavernous structure helically distorts stick-like, orientation, orderly, is generated since its chiral nematic arranges.
Fig. 2 is the XRD diagram of material prepared by the present invention: two groups of figure lines relatively learn that the composite membrane successfully washes away from figure
Template.
Fig. 3 is that the BET of material prepared by the present invention schemes: by the specific area measuring composite membrane ratio modified by PETES
Pure membrane aperture reduces, and illustrates successfully to graft functional group, and the composite membrane is meso-hole structure.
Fig. 4 is the adsorption isotherm map of material prepared by the present invention: the as can be seen from the figure equilibrium adsorption of the composite membrane
Capacity is 80mg/g.
Claims (7)
1. a kind of mesoporous silicon fiml, which is characterized in that the mesoporous silicon fiml is multilayer cavernous structure in plane, helically distorts stick
Shape, it is described it is rodlike in it is helically twisted be orientation, orderly；The mesoporous silicon fiml contains-PO (OH)2Function base and can be direct
With ≡ P=O base of metal coordination.
2. an a kind of one step preparation method of mesoporous silicon fiml as described in claim 1, which is characterized in that steps are as follows:
Cotton is placed in sulfuric acid solution by step 1, is stirred to react, takes out after completion of the reaction, is diluted with distilled water, stratification；
Supernatant liquor is outwelled, lower layer's suspension is centrifugated, washing；Suspension after centrifugation is transferred in dialysis membrane and is dialysed, is adjusted
PH, ultrasound, obtains nanocrystalline cellulose, for use；
Step 2, the nanocrystalline cellulose ultrasound for obtaining step 1, place in a round bottom flask, glucose are added, stir, be added
The mixed liquor A of diethylphosphoryl ethyl triethoxysilane and tetraethyl orthosilicate stirs, dry, obtains mesoporous silicon fiml A；
Step 3, the mesoporous silicon fiml A for obtaining step 2 are placed in sulfuric acid solution and remove removing template, obtain mesoporous silicon fiml B；
Step 4, the mesoporous silicon fiml B for obtaining step 3 are placed in concentrated hydrochloric acid and react, and obtain mesoporous silicon fiml C；
Step 5, the mesoporous silicon fiml C distilled water that step 4 is obtained and dehydrated alcohol rinse, and drying obtains final mesoporous silicon
Film.
3. an a kind of one step preparation method of mesoporous silicon fiml as claimed in claim 2, which is characterized in that in step 1, the sulfuric acid
The volume fraction of solution is 50 ~ 70%；It is described to be stirred to react to be stirred to react 2 ~ 4h at 35 ~ 55 DEG C；The retention of the dialysis membrane
Molecular weight is 11000 ~ 15000, and dialysis time is 1 ~ 4 day；The pH is 2.4.
4. an a kind of one step preparation method of mesoporous silicon fiml as claimed in claim 2, which is characterized in that in step 2, described is received
Rice crystalline cellulose, glucose, diethylphosphoryl ethyl triethoxysilane and tetraethyl orthosilicate amount ratio be 1mL:10 ~
20mg:4~6µL:30~50µL；The ultrasonic time is 10 ~ 30min；Mixing time after the addition glucose is 1 ~ 3h；Institute
Stating the whipping temp after mixed liquor A is added is 50 ~ 70 DEG C, and the time is 2 ~ 4h；The drying is in surface plate in 20 ~ 25 DEG C of water
Bath is 1 ~ 2 day dry.
5. an a kind of one step preparation method of mesoporous silicon fiml as claimed in claim 2, which is characterized in that in step 3, the sulphur
Acid solution volume fraction is 30 ~ 40%；Concentration of the mesoporous silicon fiml A in sulfuric acid solution is 10 ~ 20g/L, the mesoporous silicon
Time of the film A in sulfuric acid solution is 7 ~ 10 days.
6. an a kind of one step preparation method of mesoporous silicon fiml as claimed in claim 2, which is characterized in that in step 4, mesoporous silicon fiml
Concentration of the B in concentrated hydrochloric acid is 10 ~ 20g/L；The concentration of the concentrated hydrochloric acid is 12mol/L；The reaction temperature is 100 ~ 120
DEG C, the reaction time is 6 ~ 8h.
7. the purposes that mesoporous silicon fiml described in claim 1 is used for selective absorption lanthanum and cerium.
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| CN109200990A (en) * | 2018-08-21 | 2019-01-15 | 江苏大学 | A kind of preparation method and its usage of the lanthanum coordination functional mesoporous silicon dioxide film of diamino |
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