CN107261860A - A kind of method that sol-gal process prepares metal oxide membrane for water treatment - Google Patents
A kind of method that sol-gal process prepares metal oxide membrane for water treatment Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- B01D67/0039—Inorganic membrane manufacture
- B01D67/0048—Inorganic membrane manufacture by sol-gel transition
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
- B01D69/105—Support pretreatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/025—Aluminium oxide
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- B01D71/02—Inorganic material
- B01D71/024—Oxides
- B01D71/027—Silicium oxide
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/10—Catalysts being present on the surface of the membrane or in the pores
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
A kind of method that sol-gal process prepares metal oxide membrane for water treatment, the present invention relates to water-treatment technology field, and in particular to uses sol-gal process synthesis of metal oxide film.The invention solves the problems that preparing metal oxide film using conventional solid sintering process needs more than 1000 DEG C high temperature, it is difficult to the technical problem of control operation.Method：First, colloidal sol is prepared；2nd, stainless (steel) wire is handled；3rd, colloidal sol is spin-coated on stainless (steel) wire；4th, the stainless (steel) wire after plated film is put into calcining in Muffle furnace and obtains metal-oxide film.Preparing metal-oxide film using sol-gal process has that synthesis temperature is low, easy to operate, prepare the low feature of cost, and it also has the features such as catalytic, magnetic in addition to film retention filtering feature in itself for characteristic metal sull.The invention has more important meaning for embrane method group technology water technology, is with a wide range of applications in water treatment field.
Description
Technical field
The present invention relates to water-treatment technology field, and in particular to uses sol-gel process synthesis of metal oxide film.
Background technology
In Membrane Separation for Water Treatment field, the use of organic film is relatively broad.But compared with conventional organic film, nothing
Machine ceramic membrane has a chemical resistance, high mechanical strength, the outstanding advantages such as service life length, therefore it is in the ring of inclement condition
Often used in border, for example ceramic membrane is often effectively applied in oiliness sewage treatment.Compared with organic film material, application
It is very limited in the ceramic membrane materials of water process, mainly with TiO2、SiO2、Al2O3、ZrO2Based on.
The major technique of inorganic ceramic film preparation has:Traditional solid particles sintering process, the method mainly prepares basement membrane, load
Body；The feature professional technique such as chemical vapor deposition, physical vapour deposition (PVD), electroless plating, the method is commonly used to prepare microporous barrier or densification
Film；Sol-gel process, the method often prepares milipore filter, microfiltration membranes.The appearance of wherein sol-gel technique greatly advances ceramics
The development of membrane preparation technology.The general principle of sol-gel process is, for solvent, to add with water or organic solvent (such as ethylene glycol monomethyl ether)
Plus metal alkoxide or metal acetate salt or inorganic salts are as presoma, then add dispersant (such as acetylacetone,2,4-pentanedione) additive and formed
Homogeneous solution.Hydrolysis, polycondensation reaction formation colloidal sol occur for above-mentioned substance under certain humidity, temperature and stirring action.Colloidal sol reaches
Coating problems can be carried out to carrier, film mode mainly includes after to certain viscosity：Rotary process and dipping-pulling method.After coating
Film through gelation, dry heat treatment after at a certain temperature sintering i.e. obtain inorganic ceramic membrane.
The content of the invention
The invention solves the problems that preparing metal oxide film using conventional solid sintering process needs more than 1000 DEG C high temperature, it is difficult to
The technical problem of control operation, and a kind of method that sol-gel process prepares metal oxide membrane for water treatment is provided.
A kind of method that sol-gel process prepares metal oxide membrane for water treatment, is specifically carried out according to the following steps：
First, metal nitrate is added in deionized water, adds citric acid, magnetic force heating stirring is uniform, Ran Houjia
Enter ethylene glycol, magnetic force heating stirring is uniform, it is 95 DEG C to control temperature, oil bath heating stirring obtains colloidal sol；
2nd, stainless (steel) wire is cleaned, dried；The aperture of stainless (steel) wire is 3 μm；
Three, the stainless (steel) wire that step 2 is handled is put into sol evenning machine, the colloidal sol obtained using step one carries out spin coating, so
After dry, repeat spin coating and dry 3~5 times, obtain the stainless (steel) wire of plated film；
4th, the stainless (steel) wire of step 3 plated film is put into Muffle furnace, it is heated to 700 by the way of temperature programming~
900 DEG C, 0.5h~2h is incubated, room temperature is cooled to the furnace, obtain metal oxide membrane for water treatment, completion a kind of colloidal sol-solidifying
The method that glue method prepares metal oxide membrane for water treatment.
The metal nitrate, citric acid and ethylene glycol are that analysis is pure.
The present invention uses sol-gel process, using 3 μm of stainless (steel) wires for aperture as carrier, carried metal on this
Sull, the metal oxide of synthesis is not limited solely to above-mentioned Al2O3、SiO2、TiO2、ZrO2, therefore extend should
Material ranges for the ceramic membrane in water-treatment technology field.The synthesis temperature for preparing inoranic membrane by such a method is low, compared with
Solid sintering technology film is low more than 200 DEG C, and course of reaction is easily controllable, readily available uniform multi-component oxide, system
Standby cost is low, therefore the present invention has actual application value.
The beneficial effects of the invention are as follows：A series of metal oxides can be synthesized using the method for above-mentioned sol-gel
Film.This method not only overcomes conventional solid sintering process to need the defect more than 1000 DEG C of high temperature, and prepares that cost is low, reaction
Process is easily controllable, readily available uniform multi-component oxide.The metal oxide of synthesis is not limited solely to traditional ceramics film
The Al of use2O3、SiO2、TiO2、ZrO2Four kinds of oxides, but metallic element composition can be converted to a certain degree, so as to increase
The function of ceramic membrane, the function such as catalysis, magnetic, therefore extend the material applied to the ceramic membrane in water-treatment technology field
Expect scope and the function of ceramic membrane.
Metal-oxide film prepared by the present invention is used in water-treatment technology field.
Brief description of the drawings
Fig. 1 is coppe ferrite (CuFe prepared by embodiment one2O4) film X-ray diffraction (XRD) spectrogram；
Fig. 2 is that embodiment one does not prepare coppe ferrite (CuFe2O4) film stainless (steel) wire scanning electron microscope (SEM) photograph；
Fig. 3 is Fig. 2 partial enlarged drawings；
Fig. 4 is the coppe ferrite (CuFe that embodiment one is prepared2O4) membrane for water treatment scanning electron microscope (SEM) photograph；
Fig. 5 is Fig. 4 partial enlarged drawings.
Embodiment
Technical solution of the present invention is not limited to the embodiment of act set forth below, in addition to each embodiment it
Between any combination.
Embodiment one：The method that a kind of sol-gel process of present embodiment prepares metal oxide membrane for water treatment,
Specifically carry out according to the following steps：
First, metal nitrate is added in deionized water, adds citric acid, magnetic force heating stirring is uniform, Ran Houjia
Enter ethylene glycol, magnetic force heating stirring is uniform, it is 95 DEG C to control temperature, oil bath heating stirring obtains colloidal sol；
2nd, stainless (steel) wire is cleaned, dried；The aperture of stainless (steel) wire is 3 μm；
Three, the stainless (steel) wire that step 2 is handled is put into sol evenning machine, the colloidal sol obtained using step one carries out spin coating, so
After dry, repeat spin coating and dry 3~5 times, obtain the stainless (steel) wire of plated film；
4th, the stainless (steel) wire of step 3 plated film is put into Muffle furnace, it is heated to 700 by the way of temperature programming~
900 DEG C, 0.5h~2h is incubated, room temperature is cooled to the furnace, obtain metal oxide membrane for water treatment, completion a kind of colloidal sol-solidifying
The method that glue method prepares metal oxide membrane for water treatment.
Embodiment two：Present embodiment from unlike embodiment one：Metal nitrate in step one
For one kind in ferric nitrate, copper nitrate, manganese nitrate, aluminum nitrate and calcium nitrate or any two kinds of mixing.Other and specific implementation
Mode one is identical.
Embodiment three：Present embodiment from unlike embodiment one or two：Metal nitre in step one
Hydrochlorate is the mixing of ferric nitrate and copper nitrate, wherein Cu (NO3)2·3H2O and Fe (NO3)3·9H2O mol ratio is 1: 2.It is other
It is identical with embodiment one or two.
Embodiment four：Unlike one of present embodiment and embodiment one to three：Lemon in step one
The mol ratio of lemon acid and metal cation in metal nitrate is (1.2~1.5): 1.It is other with embodiment one to three it
One is identical.
Embodiment five：Unlike one of present embodiment and embodiment one to four：Second in step one
The mol ratio of glycol and citric acid is (1.5~2): 1.It is other identical with one of embodiment one to four.
Embodiment six：Unlike one of present embodiment and embodiment one to five：It is clear in step 2
Stainless (steel) wire is put into concussion 1h~3h, 20~130KHz of ultrasonic frequency in ultrasonic cleaning machine when washing.Other and specific implementation
One of mode one to five is identical.
Embodiment seven：Unlike one of present embodiment and embodiment one to six：Done in step 2
It is 60~90 DEG C that drying box temperature is controlled when dry.It is other identical with one of embodiment one to six.
Embodiment eight：Unlike one of present embodiment and embodiment one to seven：Done in step 3
The dry time is 5~10min.It is other identical with one of embodiment one to seven.
Embodiment nine：Unlike one of present embodiment and embodiment one to eight：Step 4 intermediate range
Sequence heating mode be：From room temperature to 100 DEG C, 1h is incubated；300 DEG C are warming up to again, are incubated 2h；500 DEG C, guarantor are warming up to again
Warm 1h；800 DEG C are finally warming up to, 0.5h is incubated；Whole heating rate is 3 DEG C/min.It is other with embodiment one to
One of eight is identical.
Embodiment ten：Unlike one of present embodiment and embodiment one to nine：Step 4 intermediate range
Sequence heating mode be：From room temperature to 100 DEG C, 2h is incubated；300 DEG C are warming up to again, are incubated 2h；500 DEG C, guarantor are warming up to again
Warm 2h；700 DEG C are finally warming up to, 2h is incubated；Whole heating rate is 3 DEG C/min.Other and embodiment one to nine
One of it is identical.
Embodiment 11：Unlike one of present embodiment and embodiment one to ten：In step 4
The mode of temperature programming is：From room temperature to 100 DEG C, 2h is incubated；300 DEG C are warming up to again, are incubated 1h；500 DEG C are warming up to again,
It is incubated 2h；800 DEG C are finally warming up to, 1h is incubated；Whole heating rate is 3 DEG C/min.It is other with embodiment one to
One of ten is identical.
Embodiment 12：Present embodiment from unlike embodiment one to one of 11：Step 4
Program heating mode be：From room temperature to 100 DEG C, 1h is incubated；300 DEG C are warming up to again, are incubated 1h；500 are warming up to again
DEG C, it is incubated 2h；900 DEG C are finally warming up to, 0.5h is incubated；Whole heating rate is 3 DEG C/min.Other and embodiment
One to one of 11 is identical.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：
The method that a kind of sol-gel process of the present embodiment prepares metal oxide membrane for water treatment, specifically enters according to the following steps
Capable：
First, by Cu (NO3)2·3H2O and Fe (NO3)3·9H2O is added in 60mL deionized waters, adds citric acid, magnetic
Power heating stirring is uniform, then adds ethylene glycol, and magnetic force heating stirring is uniform, and it is 95 DEG C to control temperature, and oil bath heating stirring is obtained
To colloidal sol；Wherein Cu (NO3)2·3H2O、Fe(NO3)3·9H2O, citric acid and ethylene glycol consumption is respectively：4.832g、
16.16g, 13.84g and 8.1mL；
2nd, the stainless (steel) wire that aperture is 3 μm is put into ultrasonic cleaning machine and shakes 1h, then dried, control drying box temperature
Spend for 90 DEG C；
Three, the stainless (steel) wire that step 2 is handled is put into sol evenning machine, the colloidal sol obtained using step one carries out spin coating, so
10min is dried afterwards, is repeated spin coating and is dried 3 times, obtains the stainless (steel) wire of plated film；
4th, the stainless (steel) wire of step 3 plated film is put into Muffle furnace, use the mode of temperature programming for：From room temperature
To 100 DEG C, 1h is incubated；300 DEG C are warming up to again, are incubated 2h；500 DEG C are warming up to again, are incubated 1h；Finally it is warming up to 800 DEG C, insulation
0.5h；Whole heating rate is 3 DEG C/min, cools to room temperature with the furnace, obtains coppe ferrite (CuFe2O4) film, complete described one
Plant the method that sol-gel process prepares metal oxide membrane for water treatment.
Coppe ferrite (CuFe manufactured in the present embodiment2O4) film X-ray diffraction (XRD) spectrogram it is as shown in Figure 1；It is got the bid
The peak of note " △ " represents CuFe2O4The XRD characteristic peaks of standard substance；
Coppe ferrite (CuFe is not prepared2O4) film stainless (steel) wire scanning electron microscope (SEM) photograph as shown in Figures 2 and 3, wherein Fig. 3
For partial enlarged drawing；Coppe ferrite (the CuFe prepared2O4) film scanning electron microscope (SEM) photograph as shown in Figure 4 and Figure 5, wherein Fig. 5 is
Partial enlarged drawing；Drawn by figure：Coppe ferrite uniform load is on stainless steel mesh carrier.
Embodiment two：
The method that a kind of sol-gel process of the present embodiment prepares metal oxide membrane for water treatment, specifically enters according to the following steps
Capable：
First, by Cu (NO3)2·3H2O and Fe (NO3)3·9H2O is added in 100mL deionized waters, adds citric acid,
Magnetic force heating stirring is uniform, then adds ethylene glycol, and magnetic force heating stirring is uniform, and it is 95 DEG C to control temperature, oil bath heating stirring,
Obtain colloidal sol；Wherein, Cu (NO3)2·3H2O、Fe(NO3)3·9H2O, citric acid and ethylene glycol consumption is respectively：4.832g、
16.16g, 17.29g and 7.6mL；
2nd, the stainless (steel) wire that aperture is 3 μm is put into ultrasonic cleaning machine and shakes 2h, then dried, control drying box temperature
Spend for 80 DEG C；
Three, the stainless (steel) wire that step 2 is handled is put into sol evenning machine, the colloidal sol obtained using step one carries out spin coating, so
8min is dried afterwards, is repeated spin coating and is dried 4 times, obtains the stainless (steel) wire of plated film；
4th, the stainless (steel) wire of step 3 plated film is put into Muffle furnace, use the mode of temperature programming for：From room temperature
To 100 DEG C, 2h is incubated；300 DEG C are warming up to again, are incubated 2h；500 DEG C are warming up to again, are incubated 2h；Finally it is warming up to 700 DEG C, insulation
2h；Whole heating rate is 3 DEG C/min, cools to room temperature with the furnace, obtains coppe ferrite (CuFe2O4) film, complete described one kind
The method that sol-gel process prepares metal oxide membrane for water treatment.
Embodiment three：
The method that a kind of sol-gel process of the present embodiment prepares metal oxide membrane for water treatment, specifically enters according to the following steps
Capable：
First, by Cu (NO3)2·3H2O and Fe (NO3)3·9H2O is added in 80mL deionized waters, adds citric acid, magnetic
Power heating stirring is uniform, then adds ethylene glycol, and magnetic force heating stirring is uniform, and it is 95 DEG C to control temperature, and oil bath heating stirring is obtained
To colloidal sol；Wherein, Cu (NO3)2·3H2O、Fe(NO3)3·9H2O, citric acid and ethylene glycol consumption is respectively：4.832g、
16.16g, 23.07g and 10.125mL；
2nd, the stainless (steel) wire that aperture is 3 μm is put into ultrasonic cleaning machine and shakes 2h, then dried, control drying box temperature
Spend for 60 DEG C；
Three, the stainless (steel) wire that step 2 is handled is put into sol evenning machine, the colloidal sol obtained using step one carries out spin coating, so
6min is dried afterwards, is repeated spin coating and is dried 5 times, obtains the stainless (steel) wire of plated film；
4th, the stainless (steel) wire of step 3 plated film is put into Muffle furnace, use the mode of temperature programming for：From room temperature
To 100 DEG C, 2h is incubated；300 DEG C are warming up to again, are incubated 1h；500 DEG C are warming up to again, are incubated 2h；Finally it is warming up to 800 DEG C, insulation
1h；Whole heating rate is 3 DEG C/min, cools to room temperature with the furnace, obtains coppe ferrite (CuFe2O4) film, complete described one kind
The method that sol-gel process prepares metal oxide membrane for water treatment.
Example IV：
The method that a kind of sol-gel process of the present embodiment prepares metal oxide membrane for water treatment, specifically enters according to the following steps
Capable：
First, by Cu (NO3)2·3H2O and Fe (NO3)3·9H2O is added in 100mL deionized waters, adds citric acid,
Magnetic force heating stirring is uniform, then adds ethylene glycol, and magnetic force heating stirring is uniform, and it is 95 DEG C to control temperature, oil bath heating stirring,
Obtain colloidal sol；Wherein, Cu (NO3)2·3H2O、Fe(NO3)3·9H2O, citric acid and ethylene glycol consumption is respectively：4.832g、
16.16g, 13.84g and 6.075mL；
2nd, the stainless (steel) wire that aperture is 3 μm is put into ultrasonic cleaning machine and shakes 2.5h, then dried, control drying box
Temperature is 70 DEG C；
Three, the stainless (steel) wire that step 2 is handled is put into sol evenning machine, the colloidal sol obtained using step one carries out spin coating, so
10min is dried afterwards, is repeated spin coating and is dried 5 times, obtains the stainless (steel) wire of plated film；
4th, the stainless (steel) wire of step 3 plated film is put into Muffle furnace, use the mode of temperature programming for：From room temperature
To 100 DEG C, 1h is incubated；300 DEG C are warming up to again, are incubated 1h；500 DEG C are warming up to again, are incubated 2h；Finally it is warming up to 900 DEG C, insulation
0.5h；Whole heating rate is 3 DEG C/min, cools to room temperature with the furnace, obtains coppe ferrite (CuFe2O4) film, complete described one
Plant the method that sol-gel process prepares metal oxide membrane for water treatment.
Claims (10)
1. a kind of method that sol-gel process prepares metal oxide membrane for water treatment, it is characterised in that this method is specifically by following
What step was carried out：
First, metal nitrate is added in deionized water, adds citric acid, magnetic force heating stirring is uniform, then adds second
Glycol, magnetic force heating stirring is uniform, and it is 95 DEG C to control temperature, and oil bath heating stirring obtains colloidal sol；
2nd, stainless (steel) wire is cleaned, dried；The aperture of stainless (steel) wire is 3 μm；
Three, the stainless (steel) wire that step 2 is handled is put into sol evenning machine, the colloidal sol obtained using step one carries out spin coating, Ran Hougan
It is dry, repeat spin coating and dry 3~5 times, obtain the stainless (steel) wire of plated film；
4th, the stainless (steel) wire of step 3 plated film is put into Muffle furnace, 700~900 DEG C is heated to by the way of temperature programming,
0.5h~2h is incubated, room temperature is cooled to the furnace, metal oxide membrane for water treatment is obtained, a kind of sol-gel legal system is completed
The method of standby metal oxide membrane for water treatment.
2. the method that a kind of sol-gel process according to claim 1 prepares metal oxide membrane for water treatment, its feature exists
Metal nitrate is one kind in ferric nitrate, copper nitrate, manganese nitrate, aluminum nitrate and calcium nitrate or any two kinds in step one
Mixing.
3. the method that a kind of sol-gel process according to claim 1 prepares metal oxide membrane for water treatment, its feature exists
The mol ratio of citric acid and metal cation in metal nitrate is (1.2~1.5) in step one: 1.
4. the method that a kind of sol-gel process according to claim 1 prepares metal oxide membrane for water treatment, its feature exists
The mol ratio of ethylene glycol and citric acid is (1.5~2) in step one: 1.
5. the method that a kind of sol-gel process according to claim 1 prepares metal oxide membrane for water treatment, its feature exists
Stainless (steel) wire is put into concussion 1h~3h, 20~130KHz of ultrasonic frequency in ultrasonic cleaning machine when being cleaned in step 2.
6. the method that a kind of sol-gel process according to claim 1 prepares metal oxide membrane for water treatment, its feature exists
It is 60~90 DEG C that drying box temperature is controlled when being dried in step 2.
7. the method that a kind of sol-gel process according to claim 1 prepares metal oxide membrane for water treatment, its feature exists
Drying time is 5~10min in step 3.
8. the method that a kind of sol-gel process according to claim 1 prepares metal oxide membrane for water treatment, its feature exists
It is in the mode of step 4 Program heating：From room temperature to 100 DEG C, 1h is incubated；300 DEG C are warming up to again, are incubated 2h；Rise again
Temperature is incubated 1h to 500 DEG C；800 DEG C are finally warming up to, 0.5h is incubated；Whole heating rate is 3 DEG C/min.
9. the method that a kind of sol-gel process according to claim 1 prepares metal oxide membrane for water treatment, its feature exists
It is in the mode of step 4 Program heating：From room temperature to 100 DEG C, 2h is incubated；300 DEG C are warming up to again, are incubated 2h；Rise again
Temperature is incubated 2h to 500 DEG C；700 DEG C are finally warming up to, 2h is incubated；Whole heating rate is 3 DEG C/min.
10. the method that a kind of sol-gel process according to claim 1 prepares metal oxide membrane for water treatment, its feature
It is that the mode that step 4 Program heats up is：From room temperature to 100 DEG C, 2h is incubated；300 DEG C are warming up to again, are incubated 1h；Again
500 DEG C are warming up to, 2h is incubated；800 DEG C are finally warming up to, 1h is incubated；Whole heating rate is 3 DEG C/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109876667A (en) * | 2019-04-04 | 2019-06-14 | 江苏海发新材料科技有限公司 | A kind of preparation method of porous stainless steel membrane |
| CN111499415A (en) * | 2020-04-26 | 2020-08-07 | 北京水研环境科技股份有限公司 | Ceramic flat membrane coating preparation method based on capillary impregnation method |
| CN113318601A (en) * | 2021-05-17 | 2021-08-31 | 浙江理工大学 | Preparation method of ceramic membrane with antibacterial function |
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