CN110038436A - A kind of preparation method of titanium dioxide graphene oxide polyethylene glycol composite ceramics nanofiltration membrane - Google Patents
A kind of preparation method of titanium dioxide graphene oxide polyethylene glycol composite ceramics nanofiltration membrane Download PDFInfo
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- CN110038436A CN110038436A CN201910273976.9A CN201910273976A CN110038436A CN 110038436 A CN110038436 A CN 110038436A CN 201910273976 A CN201910273976 A CN 201910273976A CN 110038436 A CN110038436 A CN 110038436A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0083—Thermal after-treatment
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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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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- 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
- B01D71/06—Organic material
- B01D71/38—Polyalkenylalcohols; Polyalkenylesters; Polyalkenylethers; Polyalkenylaldehydes; Polyalkenylketones; Polyalkenylacetals; Polyalkenylketals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/20—By influencing the flow
- B01D2321/2066—Pulsated flow
- B01D2321/2075—Ultrasonic treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/28—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling by soaking or impregnating
Abstract
The invention discloses a kind of preparation methods of titanium dioxide graphene oxide polyethylene glycol composite ceramics nanofiltration membrane, pass through sol-gel method fabricated in situ and titanium dioxide/graphene oxide water solution is made, then itself and Aqueous Solutions of Polyethylene Glycol are formed into organic function layer by LBL self-assembly on the surface through highly basic activation ceramic membrane to get the titanium dioxide graphene oxide polyethylene glycol composite ceramics nanofiltration membrane.The present invention by graphene oxide carried titanium dioxide can increase the hydrophilicity of film layer, the flux of film layer is improved, to enhance the contamination resistance of film layer.Under the test condition of room temperature, to the Adlerika of 0.2wt% salt rejection rate with higher, pure water flux is higher.
Description
Technical field
The invention belongs to nanofiltration membrane preparation technical fields, and in particular to a kind of titanium dioxide graphene oxide polyethylene glycol is multiple
Close the preparation method of nanofiltration membrane.
Background technique
Nanofiltration membrane is a kind of novel pressure drive membrane, membrane aperture between ultrafiltration and it is reverse osmosis between, can be used in divalent
The separation of salt and monovalent salt.The main preparation methods of nanofiltration membrane have interfacial polymerization, phase transfer method, lotus electrochemical process and cladding process
Deng.Interfacial polymerization is to prepare the most important method of organic nanofiltration membrane at present, in interfacial polymerization process, need to monomer concentration,
Reaction time, reaction temperature and ambient humidity have more harsh requirement, increase the difficulty of preparation nanofiltration membrane.Therefore using opposite
Simple LBL self-assembly method preparation nanofiltration membrane becomes very promising method.
From nanofiltration membrane in recent years studies have shown that pure inorganic ceramic nanofiltration membrane and pure machine nanofiltration membrane in industrial application
In all there are some problems.Now widely used organic ceramic nanofiltration membrane high temperature resistant, acid-proof alkaline are poor；And inorganic ceramic
Nanofiltration membrane preparation cost is higher, and brittleness is big, processing difficulties.Therefore, either organic nanofiltration membrane or Inorganic Nanofiltration Membranes is in industry
It is all restricted in use, how inorganic material and organic material to be combined, prepare composite ceramics nanofiltration using the advantages of the two
Film has become domestic and international nanofiltration membrane and studies new hot spot.
Summary of the invention
The purpose of the present invention is to provide a kind of systems of titanium dioxide graphene oxide polyethylene glycol composite ceramics nanofiltration membrane
Preparation Method.
Technical scheme is as follows:
A kind of preparation method of titanium dioxide graphene oxide polyethylene glycol composite ceramics nanofiltration membrane, passes through sol-gel
Simultaneously titanium dioxide/graphene oxide water solution is made in method fabricated in situ, then by itself and Aqueous Solutions of Polyethylene Glycol living through highly basic
Change and organic function layer is formed to get the poly- second two of the titanium dioxide graphene oxide by LBL self-assembly on the surface of ceramic membrane
Alcohol composite ceramics nanofiltration membrane, the Kong Jingwei 10-100nm of the inorganic functional layer of above-mentioned ceramic membrane, the material of above-mentioned ceramic membrane are oxygen
Change aluminium, titanium oxide or zirconium oxide.
In a preferred embodiment of the invention, include the following steps:
(1) graphene oxide water solution for being 1-4mg/L with modified Hummers method preparation concentration；
(2) above-mentioned graphene oxide water solution is added dropwise to concentration with 0.8-1.2 drop/s speed is 0.1-5mol/L's
In titanium organic salt alcoholic solution, adds nitric acid or hydrochloric acid carries out dispergation, obtain titanium dioxide/graphene oxide water that pH is 3-5
Solution；
(3) by the ceramic membrane it is sonicated after, be soaked in the strong base solution of 1-10mol/L and be activated,
Then it dries, continues to rinse with cellulose after cooling, then be washed with ethyl alcohol and deionized water, then after drying, obtain
Ceramic membrane after activation；
(4) ceramic membrane after activation is impregnated into 10- with the Aqueous Solutions of Polyethylene Glycol that concentration is 1-20wt% at room temperature
60min is put into RO water and cleans, and is then soaked in above-mentioned titanium dioxide/graphene oxide water solution at room temperature and is reacted,
It is rinsed again to remove the material on the ceramic membrane being not associated with after activation, is repeated the step 2-4 times, most afterwards after air-drying with RO water
It is heat-treated in 50-60 DEG C, to get the titanium dioxide graphene oxide polyethylene glycol composite ceramics nanofiltration membrane after natural cooling.
It is further preferred that the time of the ultrasonic treatment in the step (3) is 5-10h.
It is further preferred that the time of the activation processing in the step (3) is 10-24h.
It is further preferred that the temperature of the drying in the step (3) is 100-150 DEG C, time 10-24h.
It is further preferred that the reaction time at room temperature in the step (4) is 1-15min.
In a preferred embodiment of the invention, the titanium organic salt is tetrabutyl titanate or metatitanic acid isopropyl alcohol ester.
In a preferred embodiment of the invention, the highly basic is sodium hydroxide or potassium hydroxide.
The beneficial effects of the present invention are: the present invention by graphene oxide carried titanium dioxide can increase film layer
Hydrophilicity, improves the flux of film layer, to enhance the contamination resistance of film layer.Under room temperature and the test condition of 0.6MPa,
To the Adlerika of 0.2wt% rejection with higher (95-97%), pure water flux 40-42LHM, and pure poly- second
The flux of glycol is 21.1LHM, flux 26LHM of the Tao Shi commercialization nanofiltration membrane NF-8 at 0.69MPa, to the sulfuric acid of 0.2wt%
The rejection 88-95% of magnesium solution；168h is impregnated at the pH nitric acid solution for being 2 and pH be 12 85 DEG C of sodium hydroxide solution,
Then it is 41-43LHM that its pure water flux is tested under room temperature and the test condition of 0.6MPa, to the Adlerika of 0.2wt%
92-94% is retained, is held essentially constant.
Detailed description of the invention
Fig. 1 is sweeping for titanium dioxide graphene oxide polyethylene glycol composite ceramics nanofiltration membrane prepared by the embodiment of the present invention 1
Retouch electromicroscopic photograph.
Specific embodiment
Technical solution of the present invention is further explained and described below by way of specific embodiment.
Embodiment 1:
1, membrane tube is handled
After the 100nm aluminium oxide ceramics membrane tube ultrasound 5h for being 50cm or so by length after cutting, with 2mol/L sodium hydroxide
It impregnates for 24 hours, 10h is dried at 100 DEG C, uses cellulose to rinse ceramic-film tube after cooling, then successively uses ethyl alcohol and deionized water
It rinses for several times, is put into baking oven with furnace cooling after 100 DEG C of desired temperature dry 12h, acquisition treated membrane tube.
2,1mg/L graphene oxide water solution is prepared using modified Hummers method.It is again that the graphene oxide is water-soluble
Liquid is added dropwise in the tetrabutyl titanate alcoholic solution of 5mol/L with 1 drop/s speed, and the nitric acid or hydrochloric acid for adding 5mol/L carry out
Dispergation, the pH value of solution after dispergation are 3-5, in graphene oxide water solution through sol-gel method in graphene oxide layer
It is in situ to cover upper nano-titania particle, prepare titanium dioxide/graphene oxide water solution；
3, nanofiltration film preparation
Step 1, by treated, membrane tube is soaked in the Aqueous Solutions of Polyethylene Glycol that mass fraction is 1wt%, at room temperature instead
It takes out after answering 10min, is dried with the flushing of RO water.
Membrane tube is soaked in above-mentioned titanium dioxide/graphene oxide water solution again by step 2, is taken after reacting 5min at room temperature
Out, it is dried with the flushing of RO water.
Step 3 repeats step 1 and 2
Step 4, membrane tube is placed air-dry in the cool after be put into 50 DEG C of baking ovens and be heat-treated certain time, it is cold with furnace later
But, complete titanium dioxide graphene oxide polyethylene glycol composite ceramics nanofiltration membrane is prepared.
Membrane tube performance test: under the test condition of room temperature and the pressure of 0.6MPa, pure water flux 42LHM, to 0.2wt%
Adlerika rejection be 95%, and the flux of pure polyethylene glycol is 21.1LHM, and Tao Shi commercialization nanofiltration membrane NF-8 exists
Flux 26LHM under 0.69MPa, to the rejection 88-95% of the Adlerika of 0.2wt%.
Resistance to acid and alkali test: at 85 DEG C, by titanium dioxide graphene oxide polyethylene glycol composite ceramic made from the present embodiment
Porcelain nanofiltration membrane respectively after the sodium hydroxide solution that the pH nitric acid solution for being 2 and pH are 12 impregnates 168h, then in room temperature and
It is 42.8LHM that its pure water flux is tested under the test condition of the pressure of 0.6MPa, to the Adlerika rejection of 0.2wt%
92.5%, it is held essentially constant.And flux of the GE commercialization film DK at 0.76MPa is 27LHM, the pH of acid and alkali-resistance range is 3-9.
Embodiment 2:
1, membrane tube is handled
After the 100nm aluminium oxide ceramics membrane tube ultrasound 5h for being 50cm or so by length after cutting, with 2mol/L sodium hydroxide
It impregnates for 24 hours, 10h is dried at 100 DEG C, uses cellulose to rinse ceramic-film tube after cooling, then successively uses ethyl alcohol and deionized water
It rinses for several times, is put into baking oven with furnace cooling after 100 DEG C of desired temperature dry 12h, acquisition treated membrane tube.2, it uses
Modified Hummers method prepares 4mg/L graphene oxide water solution, then by the graphene oxide water solution with 1 drop/s speed
Degree is added dropwise in the metatitanic acid isopropanol ester solution of 2mol/L, and the nitric acid or hydrochloric acid for adding 5mol/L carry out dispergation, after dispergation
PH value of solution is 3-5, passes through sol-gel method in graphene oxide water solution and covers upper nanometer in situ in graphene oxide layer
TiO 2 particles prepare titanium dioxide/graphene oxide water solution；
3, nanofiltration film preparation
Step 1, by treated, membrane tube is soaked in the Aqueous Solutions of Polyethylene Glycol that mass fraction is 10wt%, at room temperature instead
It takes out after answering 10min, is dried with the flushing of RO water.
Membrane tube is soaked in above-mentioned titanium dioxide/graphene oxide water solution again by step 2, is taken after reacting 15min at room temperature
Out, it is dried with the flushing of RO water.
Step 3 repeats step 1 and 2
Step 4, membrane tube placed at room temperature air-dry in the cool after be put into 50 DEG C of baking ovens and be heat-treated certain time, later
Complete titanium dioxide graphene oxide polyethylene glycol composite ceramics nanofiltration membrane is prepared in furnace cooling.
Membrane tube performance test: under the test condition of room temperature and the pressure of 0.6MPa, pure water flux 40LHM, to 0.2wt%
Adlerika rejection be 97%, and the flux of pure polyethylene glycol is 21.1LHM, and Tao Shi commercialization nanofiltration membrane NF-8 exists
Flux 26LHM under 0.69MPa, to the rejection 88-95% of the Adlerika of 0.2wt%.
Resistance to acid and alkali test: at 85 DEG C, by titanium dioxide graphene oxide polyethylene glycol composite ceramic made from the present embodiment
Porcelain nanofiltration membrane respectively after the sodium hydroxide solution that the pH nitric acid solution for being 2 and pH are 12 impregnates 168h, then in room temperature and
It is 41.2LHM that its pure water flux is tested under the test condition of the pressure of 0.6MPa, to the Adlerika rejection of 0.2wt%
93.8%, it is held essentially constant.And flux of the GE commercialization film DK at 0.76MPa is 27LHM, the pH of acid and alkali-resistance range is 3-9.
The foregoing is only a preferred embodiment of the present invention, the range that the present invention that therefore, it cannot be limited according to is implemented, i.e.,
Equivalent changes and modifications made in accordance with the scope of the invention and the contents of the specification should still be within the scope of the present invention.
Claims (8)
1. a kind of preparation method of titanium dioxide graphene oxide polyethylene glycol composite ceramics nanofiltration membrane, it is characterised in that: pass through
Simultaneously titanium dioxide/graphene oxide water solution is made in sol-gel method fabricated in situ, and then itself and Aqueous Solutions of Polyethylene Glycol exist
Organic function layer is formed to get the titanium dioxide graphite oxide by LBL self-assembly on surface through highly basic activation ceramic membrane
Alkene polyethylene glycol composite ceramics nanofiltration membrane, the Kong Jingwei 10-100nm of the inorganic functional layer of above-mentioned ceramic membrane, above-mentioned ceramic membrane
Material is aluminium oxide, titanium oxide or zirconium oxide.
2. preparation method as described in claim 1, characterized by the following steps:
(1) graphene oxide water solution for being 1-4mg/L with modified Hummers method preparation concentration；
(2) above-mentioned graphene oxide water solution is added dropwise to the titanium that concentration is 0.1-5mol/L with 0.8-1.2 drop/s speed has
In machine salt alcoholic solution, adds nitric acid or hydrochloric acid carries out dispergation, obtain titanium dioxide/graphene oxide water solution that pH is 3-5；
(3) by the ceramic membrane it is sonicated after, be soaked in the strong base solution of 1-10mol/L and be activated, then
Drying continues to rinse, then be washed with ethyl alcohol and deionized water, then after drying, activated after cooling with cellulose
Ceramic membrane afterwards；
(4) ceramic membrane after activation is impregnated into 10-60min with the Aqueous Solutions of Polyethylene Glycol that concentration is 1-20wt% at room temperature,
It is put into RO water and cleans, be then soaked in above-mentioned titanium dioxide/graphene oxide water solution at room temperature and reacted, then use RO
Water is rinsed to remove the material on the ceramic membrane being not associated with after activation, is repeated the step 2-4 times, most afterwards after air-drying in 50-
60 DEG C are heat-treated, to get the titanium dioxide graphene oxide polyethylene glycol composite ceramics nanofiltration membrane after natural cooling.
3. preparation method as claimed in claim 2, it is characterised in that: the time of the ultrasonic treatment in the step (3) is 5-
10h。
4. preparation method as claimed in claim 2, it is characterised in that: the time of the activation processing in the step (3) is 10-
24h。
5. preparation method as claimed in claim 2, it is characterised in that: the temperature of the drying in the step (3) is 100-150
DEG C, time 10-24h.
6. preparation method as claimed in claim 2, it is characterised in that: the reaction time at room temperature in the step (4) is
1-15min。
7. the preparation method as described in any claim in claim 1 to 6, it is characterised in that: the titanium organic salt is titanium
Sour N-butyl or metatitanic acid isopropyl alcohol ester.
8. the preparation method as described in any claim in claim 1 to 6, it is characterised in that: the highly basic is hydroxide
Sodium or potassium hydroxide.
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Cited By (6)
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|---|---|---|---|---|
| CN111420564A (en) * | 2020-03-05 | 2020-07-17 | 浙江美易膜科技有限公司 | Inorganic composite separation membrane containing graphene oxide, and preparation method and application thereof |
| CN114130197A (en) * | 2020-09-04 | 2022-03-04 | 三达膜科技（厦门）有限公司 | Graphene oxide titanium dioxide-dopamine PEI nanofiltration membrane and preparation method thereof |
| CN114130219A (en) * | 2020-09-04 | 2022-03-04 | 三达膜科技（厦门）有限公司 | Titanium dioxide loaded molybdenum disulfide oxide doped piperazine polyamide composite ceramic nanofiltration membrane and preparation method thereof |
| CN114130201A (en) * | 2020-09-04 | 2022-03-04 | 三达膜科技（厦门）有限公司 | Titanium dioxide graphene oxide modified organic ultrafiltration membrane and preparation method thereof |
| CN115368158A (en) * | 2021-05-21 | 2022-11-22 | 三达膜科技（厦门）有限公司 | Preparation method of ultrathin titanium oxide ceramic nanofiltration membrane |
| CN115364689A (en) * | 2021-05-21 | 2022-11-22 | 三达膜科技（厦门）有限公司 | Preparation method of ultrathin zirconium oxide-titanium oxide ceramic composite nanofiltration membrane |
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