CN110743386A - Preparation method of zirconia-titanium oxide composite ultrafiltration membrane - Google Patents
Preparation method of zirconia-titanium oxide composite ultrafiltration membrane Download PDFInfo
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Abstract
The invention discloses a preparation method of a zirconia-titania composite ultrafiltration membrane. The Ti-Zr composite sol prepared by a sol-gel method is used as a precursor, then the precursor is treated by a hydrothermal method, a Ti-Zr composite nano solution with uniform particle size can be obtained by adopting a two-step method, a proper amount of additive is added into the Ti-Zr composite nano solution to directly prepare a coating solution, the coating solution is coated for one time, and the Ti-Zr composite ultrafiltration membrane can be prepared by drying and calcining.
Description
Technical Field
The invention belongs to the technical field of ultrafiltration membrane preparation, and particularly relates to a preparation method of a zirconia-titania composite ultrafiltration membrane.
Background
Membrane separation technology is a separation technology that arose in the 60's of the 20 th century and has developed rapidly over decades. The application field of the membrane separation technology is deep in various aspects of life and production of people, such as chemical industry, environmental protection, electronics, textiles, medicines, foods and the like. Since the industrialization of membrane separation technology, organic polymer membranes have been dominant, and although the advantages of organic membranes are many, with the gradual expansion of membrane separation technology, some disadvantages of polymer separation membranes are gradually exposed, such as poor high temperature resistance, poor chemical resistance, easy pollution, swelling and shrinking in solvents, etc., which limits the application thereof.
Compared with organic membranes, inorganic membranes have many excellent characteristics as emerging separation media, such as good chemical stability, high mechanical strength, high temperature resistance, microbial corrosion resistance, long service life and the like, so that the inorganic membranes become green and environment-friendly materials. Inorganic membrane media are gradually developed into a large class of green and environment-friendly high-tech technology as a separation process. Inorganic separation membranes are classified into two major types, namely dense membranes and porous membranes, from the surface layer structure. The materials can be classified into ceramic membranes, metal membranes, alloy membranes, zeolite membranes, glass membranes and the like, wherein the ceramic membranes mainly comprise alumina, titania, zirconia and silica, and are known for thermal stability and widely applied.
The sol-gel method is the most important method for preparing the ceramic ultrafiltration membrane. The sol-gel method is that alkoxide or non-alkoxide is hydrolyzed and polycondensed in certain solvent to obtain sol with certain grain size distribution, and proper amount of additive is added into the sol to prepare coating liquid with certain viscosity and concentration; and then coating the porous support body with the coating liquid to form a gel membrane, and drying and sintering to form the ultrafiltration membrane. The nano particles prepared by the sol-gel method have high water content, the film layer is easy to crack, and the sol-gel method generally needs repeated coating for many times to ensure the integrity of the film layer; meanwhile, TiO2 and ZrO2 nano particles prepared by a sol-gel method can respectively generate anatase and tetragonal phases at the temperature of 300-400 ℃, and when the sintering temperature is increased to 500 ℃, TiO2 and ZrO2 particles can generate crystal transformation, and the generation of defects and the increase of the aperture can be caused along with the volume change and the growth of crystal grains. To address this problem, researchers have mainly doped the crystal form stabilizer into TiO2 and ZrO2 to raise the crystal form transition temperature of TiO2 and ZrO 2. However, since the crystal stabilizers are expensive and are prone to acidic substance reaction, the acid and alkali resistance of the product needs to be examined.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a zirconia-titania composite ultrafiltration membrane.
The technical scheme of the invention is as follows:
a preparation method of a zirconia-titania composite ultrafiltration membrane comprises the following steps:
(1) adding polyethylene glycol or nitric acid with the weight-average molecular weight of 550-650 serving as a dispersing agent into a mixed solution of organic zirconium alkoxide and organic titanium alkoxide, stirring at 50-65 ℃, dropwise adding ammonia water or sodium hydroxide to adjust the pH value to 9-11, then carrying out heat preservation reaction for 2-3h, then carrying out solid-liquid separation to obtain a solid, drying the solid, then dissolving the solid into water again, adding nitric acid to carry out peptization, and enabling the pH value of the peptized material to be 2-3 to prepare Ti-Zr composite sol; in the mixed solution, the mol ratio of the organic zirconium alkoxide to the organic titanium alkoxide is 0.8-1.2: 0.8-1.2, and the concentration is 0.1-1 mol/L;
(2) putting the Ti-Zr composite sol into a hydrothermal reaction kettle, keeping the filling degree at 50-60%, carrying out heat preservation reaction at the temperature of 200-250 ℃ for 5-10h, and cooling to obtain a Ti-Zr composite nano solution;
(3) adding polyethylene glycol with the weight-average molecular weight of 350-450 serving as a plasticizer and a cellulose compound with the molecular weight of 6000-10000 serving as a binder into the Ti-Zr composite nano solution until the final concentrations are 2-5 wt% and 0.1-0.5 wt%, and uniformly mixing to obtain a coating solution; the cellulose compound is hydroxymethyl cellulose, hydroxyethyl cellulose or hydroxypropyl cellulose;
(4) coating the coating liquid on a porous alumina ceramic membrane support, heating to 120 ℃ at the speed of 1-3 ℃/min, preserving heat, drying for 2-5h, then heating to 700 ℃ at the speed of 1-3 ℃/min, preserving heat, calcining for 2-3h, and cooling to obtain the zirconia-titania composite ultrafiltration membrane.
In a preferred embodiment of the present invention, in the step (1), the dispersant is added in an amount of 1 to 3 wt% of the mixed solution.
In a preferred embodiment of the present invention, in the step (1), the molar ratio of the organozirconium alkoxide to the organotitanium alkoxide is 1: 1.
In a preferred embodiment of the invention, the organozirconium alkoxide is zirconium n-butoxide or zirconium n-propoxide.
In a preferred embodiment of the invention, the organic titanium alkoxide is titanium isopropoxide or titanium tert-butoxide.
In a preferred embodiment of the present invention, in the step (3), polyethylene glycol having a weight average molecular weight of 350-450 as a plasticizer and a cellulose compound as a binder are added to the above Ti — Zr composite nano solution to final concentrations of 2 to 5 wt% and 0.1 to 0.5 wt%, respectively, and after mixing uniformly, a defoaming agent is added to a final concentration of 0.01 to 0.1 wt%, to prepare a coating solution.
Further preferably, the defoaming agent is a silicone defoaming agent.
In a preferred embodiment of the present invention, the porous alumina ceramic membrane support has an average pore size of 0.1 μm.
The invention has the beneficial effects that: the Ti-Zr composite sol prepared by a sol-gel method is used as a precursor, then the precursor is treated by a hydrothermal method, a Ti-Zr composite nano solution with uniform particle size can be obtained by adopting a two-step method, a proper amount of additive is added into the Ti-Zr composite nano solution to directly prepare a coating solution, the coating solution is coated for one time, and the Ti-Zr composite ultrafiltration membrane can be prepared by drying and calcining.
Drawings
FIG. 1 is a scanning electron micrograph of a membrane layer of a zirconia ceramic ultrafiltration membrane prepared in comparative example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of a membrane layer of the titanium oxide ceramic ultrafiltration membrane prepared in comparative example 2 of the present invention.
Fig. 3 is a scanning electron micrograph of a membrane layer of the zirconia-titania composite ultrafiltration membrane prepared in example 1 of the present invention.
Detailed Description
The technical solution of the present invention will be further illustrated and described below with reference to the accompanying drawings by means of specific embodiments.
Comparative example 1
(1) Adding a dispersant polyethylene glycol (PEG 600) into a 0.5moL/L n-butyl zirconium solution to enable the final mass concentration to be 2%, and dropwise adding 0.1moL L sodium hydroxide into the solution under the stirring condition at 60 ℃ to adjust the pH value to be 10; after 2.5h of reaction, carrying out solid-liquid separation, drying the solid part at 60 ℃, dissolving the solid part in water again, adding 0.1M nitric acid to carry out peptization, and enabling the pH value of the peptized solution to be 2 to prepare zirconia sol;
(2) putting the zirconia sol obtained in the step (1) into a hydrothermal reaction kettle with the filling degree of 60%, carrying out heat preservation reaction for 8 hours at the temperature of 200 ℃, and cooling to obtain a zirconia nano solution;
(3) adding PEG-400 and hydroxymethyl cellulose with the molecular weight of 6000-10000 into the zirconia nano solution obtained in the step (2), enabling the final mass concentration of the PEG-400 and the final mass concentration of the hydroxymethyl cellulose to be 3% and 0.3% respectively, stirring uniformly, then adding an organic silicon defoamer Dow Corning DC65 and enabling the final mass concentration to be 0.05%, and uniformly mixing to obtain a coating solution;
(4) coating the coating liquid on a porous alumina ceramic membrane support with the average pore diameter of 0.1 mu m, heating to 120 ℃ according to the heating rate of 2 ℃/min, drying for 3h, then heating to 650 ℃ according to the heating rate of 2 ℃/min, carrying out heat preservation and calcination for 2h, and cooling to obtain the zirconia ceramic ultrafiltration membrane. The average pore diameter of the prepared zirconia ceramic ultrafiltration membrane is 15nm, the retention rate of 2g/L glucan (molecular weight is 15 ten thousand) exceeds 90%, and the integral bubble pressure is more than 0.5MPa through a bubble pressure test. The film layers are shown in figure 1.
Comparative example 2
(1) Adding a dispersant polyethylene glycol (PEG 600) into 0.5moL/L titanium isopropoxide solution to enable the final mass concentration of the polyethylene glycol to be 2%, and dropwise adding 0.1moL L of sodium hydroxide into the solution to adjust the pH value to be 10 under the condition of stirring at 60 ℃; after 2.5h of reaction, carrying out solid-liquid separation, drying the solid part at 60 ℃, dissolving the solid part in water again, adding 0.1M nitric acid to carry out peptization, and enabling the pH value of the peptized solution to be 2 to prepare titanium oxide sol;
(2) putting the titanium oxide sol obtained in the step (1) into a hydrothermal reaction kettle with the filling degree of 60%, carrying out heat preservation reaction for 8 hours at the temperature of 200 ℃, and cooling to obtain a titanium oxide nano solution;
(3) adding PEG-400 and hydroxymethyl cellulose with the molecular weight of 6000-10000 into the titanium oxide nano solution obtained in the step (2), enabling the final mass concentration of the PEG-400 and the final mass concentration of the hydroxymethyl cellulose to be 3% and 0.3% respectively, stirring uniformly, then adding an organic silicon defoamer Dow Corning DC65 and enabling the final mass concentration to be 0.05%, and uniformly mixing to obtain a coating solution;
(4) coating the film coating liquid on a porous alumina ceramic membrane support with the average pore diameter of 0.1 mu m, heating to 120 ℃ according to the heating rate of 2 ℃/min, drying for 3h, then heating to 650 ℃ according to the heating rate of 2 ℃/min, carrying out heat preservation and calcination for 2h, and cooling to obtain the titanium oxide ceramic ultrafiltration membrane. The average pore diameter of the prepared titanium oxide ceramic ultrafiltration membrane is 12nm, the retention rate of 2g/L glucan (with the molecular weight of 10 ten thousand) exceeds 90 percent, and the integral bubble pressure is more than 0.5MPa through a bubble pressure test. The film layers are shown in figure 2.
Example 1
(1) Adding a dispersant polyethylene glycol (PEG 600) into a 0.5moL/L solution (the moL ratio is 1: 1) of zirconium n-butoxide and titanium isopropoxide, and enabling the final mass concentration to be 2%, and dropwise adding 0.1moL L of sodium hydroxide into the solution under the stirring condition at 60 ℃ to adjust the pH value to be 10; after 2.5h of reaction, carrying out solid-liquid separation, drying the solid part at 60 ℃, dissolving the solid part in water again, adding 0.1M nitric acid to carry out peptization, and enabling the pH value of the peptized solution to be 2 to prepare Ti-Zr composite sol;
(2) putting the Ti-Zr composite sol obtained in the step (1) into a hydrothermal reaction kettle with the filling degree of 60%, carrying out heat preservation reaction for 8 hours at the temperature of 200 ℃, and cooling to obtain a Ti-Zr composite nano solution;
(3) adding PEG-400 and hydroxymethyl cellulose with the molecular weight of 6000-10000 into the Ti-Zr composite nano solution obtained in the step (2), enabling the final mass concentration of the PEG-400 and the final mass concentration of the hydroxymethyl cellulose to be 3% and 0.3% respectively, stirring uniformly, then adding an organic silicon defoamer Dow Corning DC65 and enabling the final mass concentration to be 0.05%, and uniformly mixing to obtain a coating solution;
(4) coating the coating liquid on a porous alumina ceramic membrane support with the average pore diameter of 0.1 mu m, heating to 120 ℃ according to the heating rate of 2 ℃/min, drying for 3h, then heating to 650 ℃ according to the heating rate of 2 ℃/min, carrying out heat preservation and calcination for 2h, and cooling to obtain the zirconia-titania composite ultrafiltration membrane. The average pore diameter of the prepared zirconia-titania composite ultrafiltration membrane is 8nm, the retention rate of 2g/L glucan (molecular weight is 4 ten thousand) exceeds 90%, and no defect pore bubbles appear through a bubble pressure test. The film layers are shown in figure 3.
Example 4
(1) Adding a dispersant polyethylene glycol (PEG 600) into a 0.1moL/L solution (the moL ratio is 1: 1) of zirconium n-butoxide and titanium isopropoxide, enabling the final mass concentration to be 2%, and dropwise adding 0.1moL L of sodium hydroxide into the solution under the stirring condition at 60 ℃ to adjust the pH value to be 9; after reacting for 2h, carrying out solid-liquid separation, drying the solid part at 50 ℃, dissolving the solid part in water again, adding 0.1M nitric acid to carry out peptization, and enabling the pH value of the peptized solution to be 3 to prepare Ti-Zr composite sol;
(2) putting the Ti-Zr composite sol obtained in the step (1) into a hydrothermal reaction kettle with the filling degree of 50%, carrying out heat preservation reaction for 10 hours at the temperature of 200 ℃, and cooling to obtain a Ti-Zr composite nano solution;
(3) adding PEG-400 and hydroxymethyl cellulose into the Ti-Zr composite nano solution obtained in the step (2), enabling the final mass concentration of the PEG-400 and the final mass concentration of the hydroxymethyl cellulose to be 2% and 0.1% respectively, stirring uniformly, then adding an organic silicon defoamer Dow Corning DC65 and enabling the final mass concentration to be 0.01%, and uniformly mixing to obtain a coating solution;
(4) the coating liquid is coated on a porous alumina ceramic membrane support body with the average pore diameter of 0.1 mu m, the temperature is raised to 100 ℃ according to the heating rate of 1 ℃/min, the drying is carried out for 3h, then the temperature is raised to 600 ℃ according to the heating rate of 2 ℃/min, the heat preservation and the calcination are carried out for 2h, and the cooling is carried out, so that the zirconia-titania composite ultrafiltration membrane is obtained, the retention rate of 2g/L glucan (with the molecular weight of 4 ten thousand) is more than 90%, and the bubble pressure test shows that no defect pore bubble occurs.
Example 5
(1) Adding a dispersant polyethylene glycol (PEG 600) into lmol/L n-zirconium butanol and titanium isopropoxide solution (the molar ratio is 1: 1) to enable the final mass concentration to be 2%, and dropwise adding 0.1moL of sodium hydroxide into the solution under the stirring condition at 65 ℃ to adjust the pH value to be 11; after reacting for 2h, carrying out solid-liquid separation, drying the solid part at 50 ℃, dissolving the solid part in water again, adding 0.1M nitric acid to carry out peptization, and enabling the pH value of the peptized solution to be 3 to prepare Ti-Zr composite sol;
(2) putting the Ti-Zr composite sol obtained in the step (1) into a hydrothermal reaction kettle with the filling degree of 60%, carrying out heat preservation reaction for 10 hours at the temperature of 200 ℃, and cooling to obtain a Ti-Zr composite nano solution;
(3) adding PEG-400 and hydroxymethyl cellulose with the molecular weight of 6000-10000 into the Ti-Zr composite nano solution obtained in the step (2), enabling the final mass concentration of the PEG-400 and the final mass concentration of the hydroxymethyl cellulose to be 5% and 1% respectively, stirring uniformly, then adding an organic silicon defoamer Dow Corning DC65 and enabling the final mass concentration to be 0.1%, and uniformly mixing to obtain a coating solution;
(4) the coating liquid is coated on a porous alumina ceramic membrane support body with the average pore diameter of 0.1 mu m, the temperature is raised to 120 ℃ according to the heating rate of 1 ℃/min, the drying is carried out for 3h, then the temperature is raised to 700 ℃ according to the heating rate of 2 ℃/min, the heat preservation and the calcination are carried out for 2h, and the cooling is carried out, so that the zirconia-titania composite ultrafiltration membrane is obtained, the retention rate of 2g/L glucan (with the molecular weight of 4 ten thousand) is more than 90%, and no defect pore bubble appears through a bubble pressure test.
The hydroxymethyl cellulose in the above embodiments may also be replaced with hydroxyethyl cellulose or hydroxypropyl cellulose.
TABLE 1
As can be seen from Table 1, in the present invention, the crystal form stabilizer is doped into TiO2And ZrO2The method can reduce the particle size and prepare the ceramic ultrafiltration membrane with smaller pore diameter.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (8)
1. A preparation method of a zirconia-titania composite ultrafiltration membrane is characterized by comprising the following steps: the method comprises the following steps:
(1) adding polyethylene glycol or nitric acid with the weight-average molecular weight of 550-650 serving as a dispersing agent into a mixed solution of organic zirconium alkoxide and organic titanium alkoxide, stirring at 50-65 ℃, dropwise adding ammonia water or sodium hydroxide to adjust the pH value to 9-11, then carrying out heat preservation reaction for 2-3h, then carrying out solid-liquid separation to obtain a solid, drying the solid, then dissolving the solid into water again, adding nitric acid to carry out peptization, and enabling the pH value of the peptized material to be 2-3 to prepare Ti-Zr composite sol; in the mixed solution, the mol ratio of the organic zirconium alkoxide to the organic titanium alkoxide is 0.8-1.2: 0.8-1.2, and the concentration is 0.1-1 mol/L;
(2) putting the Ti-Zr composite sol into a hydrothermal reaction kettle, keeping the filling degree at 50-60%, carrying out heat preservation reaction at the temperature of 200-250 ℃ for 5-10h, and cooling to obtain a Ti-Zr composite nano solution;
(3) adding polyethylene glycol with the weight-average molecular weight of 350-450 serving as a plasticizer and a cellulose compound with the molecular weight of 6000-10000 serving as a binder into the Ti-Zr composite nano solution until the final concentrations are 2-5 wt% and 0.1-0.5 wt%, and uniformly mixing to obtain a coating solution; the cellulose compound is hydroxymethyl cellulose, hydroxyethyl cellulose or hydroxypropyl cellulose;
(4) coating the coating liquid on a porous alumina ceramic membrane support, heating to 120 ℃ at the speed of 1-3 ℃/min, preserving heat, drying for 2-5h, then heating to 700 ℃ at the speed of 1-3 ℃/min, preserving heat, calcining for 2-3h, and cooling to obtain the zirconia-titania composite ultrafiltration membrane.
2. The method of claim 1, wherein: in the step (1), the addition amount of the dispersant is 1-3 wt% of the mixed solution.
3. The method of claim 1, wherein: in the step (1), the molar ratio of the organic zirconium alkoxide to the organic titanium alkoxide is 1: 1.
4. The method of claim 1, wherein: the organic zirconium alkoxide is n-butyl zirconium or n-propyl zirconium.
5. The method of claim 1, wherein: the organic titanium alkoxide is titanium isopropoxide or titanium tert-butoxide.
6. The method of claim 1, wherein: and (3) adding polyethylene glycol with the weight-average molecular weight of 350-450 serving as a plasticizer and a cellulose compound serving as a binder into the Ti-Zr composite nano solution until the final concentrations are respectively 2-5 wt% and 0.1-0.5 wt%, uniformly mixing, and then adding a defoaming agent until the final concentration is 0.01-0.1 wt%, thereby preparing the coating solution.
7. The method of claim 6, wherein: the defoaming agent is an organic silicon defoaming agent.
8. The method of claim 1, wherein: the average pore diameter of the porous alumina ceramic membrane support is 0.1 mu m.
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| WO2021248897A1 (en) * | 2020-06-12 | 2021-12-16 | 三达膜科技（厦门）有限公司 | Preparation method for zirconia ceramic ultrafiltration 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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