CN110523296B - Preparation method of tubular zeolite membrane applied to reverse osmosis water treatment - Google Patents
Preparation method of tubular zeolite membrane applied to reverse osmosis water treatment Download PDFInfo
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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
- B01D61/025—Reverse osmosis; Hyperfiltration
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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
- B01D67/0093—Chemical modification
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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
- B01D69/02—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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- 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
- B01D69/04—Tubular membranes
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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
- B01D71/028—Molecular sieves
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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
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/02—Non-contaminated water, e.g. for industrial water supply
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
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Abstract
The invention provides a preparation method of a tubular zeolite membrane applied to reverse osmosis water treatment, which is characterized in that the tubular zeolite membrane is prepared by a traditional secondary growth method and is repaired after being roasted at high temperature, wherein the repair is carried out by sequentially introducing a water phase solution containing polyamine and an organic phase solution containing acyl chloride into the inner side and the outer side of the tubular membrane, so that the two phase solutions are reflected and crosslinked at defect holes to form polyamide to repair the defect holes. The repair method provided by the invention combines the advantages of the zeolite membrane and the polyamide membrane, improves the desalination rate of the membrane and keeps the water flux in a higher range.
Description
Technical Field
The invention relates to a preparation method of a membrane, in particular to a preparation method of a tubular zeolite membrane applied to reverse osmosis water treatment.
Background
Reverse osmosis is a membrane separation technique that uses pressure as a driving force by virtue of the function of a permselective (semi-permeable) membrane, when the pressure applied in the system is greater than the osmotic pressure of an inlet water solution, water molecules continuously permeate the membrane, flow into a central tube through a water production flow channel, then impurities in outlet water at one end, such as ions, organic matters, bacteria, viruses and the like, are trapped at the inlet side of the membrane, and then flow out at the outlet end of concentrated water, thereby achieving the purpose of separation and purification. Nowadays, reverse osmosis is widely applied in the fields of pure water and ultrapure water preparation, wastewater treatment, seawater desalination and the like.
At present, the membrane for reverse osmosis mainly comprises organic membranes such as cellulose acetate membrane, aromatic polyamide membrane and the like, wherein the polyamide membrane is common. However, polyamide reverse osmosis membranes have relatively poor salt rejection, poor fouling resistance, short life, and high water demand. The zeolite membrane has the characteristics of small and uniform pore diameter, so that the zeolite membrane becomes a potential ideal reverse osmosis membrane material. Since the beginning of this century, different zeolite membranes were gradually applied in reverse osmosis water treatment, such as ZK-4 type, LTA type, MFI type, and FAU type. The MFI type zeolite has a three-dimensional pore channel structure, the effective pore diameter of the MFI type zeolite is about 0.55 nm, the rule ratio of the MFI type zeolite is adjustable, and the MFI type zeolite is an inorganic reverse osmosis membrane type which is researched more. However, for the MFI zeolite membrane, a template agent is required to be adopted in the preparation process, so that the MFI zeolite membrane needs to be calcined at a high temperature after being subjected to hydrothermal synthesis to remove the template agent. Therefore, cracks and other defects often occur during the high-temperature baking process. In addition, intergranular defects such as pinholes also occur during the film preparation process. The above-mentioned drawbacks result in a low salt rejection of the membrane in reverse osmosis water treatment. Therefore, a method for preparing a zeolite membrane for reverse osmosis water treatment is urgently needed.
Disclosure of Invention
In view of the above problems, the present invention provides a method for preparing a tubular zeolite membrane for reverse osmosis water treatment, wherein the tubular zeolite membrane is a ZSM-5 zeolite membrane supported on a tubular carrier, and the method comprises the following steps:
(a) pretreating a tubular carrier, and then soaking the tubular carrier into a ZSM-5-containing zeolite solution for seed crystal loading;
(b) placing the tubular carrier loaded with the seed crystal into a membrane casting solution, wherein the membrane casting solution contains a template agent TPAOH, a silicon source, an aluminum source, sodium hydroxide and water for hydrothermal synthesis, the synthesis temperature is 120-180 ℃, and the synthesis time is 12-48 h;
(c) roasting the zeolite membrane synthesized in the step (b) at the temperature of 400-500 ℃ for 4-6h, wherein the heating and cooling rates are 1-2 ℃/min;
(d) soaking the zeolite membrane in deionized water for 12-24h, and drying at 50-80 deg.C for 6-8 h;
(e) putting the zeolite membrane into a tubular membrane component, and carrying out vacuum degassing treatment on the zeolite membrane for 1-3 h;
(f) passing an aqueous phase solution containing a polyamine through the inside of the tubular zeolite membrane at a rate of 0.2-2mL/min for a first contact time of 10-20s;
(g) passing deionized water through the inside/outside of the tubular zeolite membrane at a rate of 0.05-0.5ml/min for a second contact time of 2-4s;
(h) passing the organic phase solution containing the polyacyl chloride through the outer side of the tubular zeolite membrane at the speed of 0.5-2ml/min, wherein the third contact time is 10-20s;
(i) repeating steps (f) - (h) 2-6 times;
(j) taking out the zeolite membrane from the tubular membrane module, and drying at 60-100 deg.C for 5-20 min.
Preferably, the tubular support has an internal diameter of 5 to 12 mm.
Preferably, in the tubular membrane module, the distance between the zeolite membrane and the inner wall of the tubular membrane module is 3-8 mm.
Preferably, the polyamine is one or more of m-phenylenediamine, p-phenylenediamine, xylylenediamine and 2, 4-diaminotoluene.
Preferably, the acyl chloride solution is one or more of phthaloyl chloride, terephthaloyl chloride, isophthaloyl chloride and trimesoyl chloride.
Preferably, the organic solvent in the organic phase solution is one or more of cyclohexane, heptane, octane, naphtha, ISOPARE or mineral oil.
Preferably, the concentration of the polyamine in the aqueous phase solution is 1% -5%, and the concentration of the acyl chloride in the organic phase solution is 0.05-0.5%.
The invention also provides a tubular zeolite membrane applied to reverse osmosis water treatment, which is prepared according to the method.
The invention also provides an application of the tubular zeolite membrane in reverse osmosis water treatment, which comprises wastewater treatment, seawater desalination, pure water preparation and the like.
The invention adopts the traditional secondary growth method to prepare the zeolite membrane, and adopts the mode of generating polyamide by interfacial polymerization to repair the defects of the zeolite membrane, and concretely, the inner side of the tubular zeolite membrane is firstly introduced with aqueous phase solution containing polyamine, the aqueous phase solution can permeate into the defect holes in the flowing process, ZSM-5 zeolite containing aluminum has hydrophilicity and the adsorption performance of the zeolite is adsorbed by the zeolite surface at the defect holes, and then deionized water is slowly introduced into the inner part and the outer part of the tubular zeolite membrane, so that the aqueous phase solution at the inner side and the outer side of the tubular zeolite membrane is removed to avoid amidation of other subsequent organic phases at the inner side and the outer side of the tubular zeolite membrane. Then, an organic phase solution containing acyl chloride is introduced to the outer side of the zeolite membrane, and the organic phase solution enters the defect hole and reacts with the water phase solution adsorbed at the defect hole to crosslink into polyamide so as to fill the defect hole.
The invention has the beneficial effects that: the invention fills polyamide in the defect of the zeolite membrane applied to reverse osmosis water treatment, and the repaired zeolite membrane combines the advantages of high desalination rate of the zeolite membrane and large flux of the polyamide membrane because the polyamide is provided with pores, and the compactness of the polyamide can be adjusted by adjusting the repairing times so as to meet different requirements. The reverse osmosis membrane prepared by the invention is applied to 0.1mol NaCL, the desalination rate can reach 84-92% and the flux can reach 1.1-1.3 Kg/(m) at 25 ℃, the pH value is 7.5 and the pressure is 2.75MPa2.h)。
Detailed Description
Example 1
A tubular zeolite membrane for reverse osmosis water treatment was prepared as follows.
(a) Pretreating a tubular carrier, and then soaking the tubular carrier into a ZSM-5-containing zeolite solution (1%) to carry out seed crystal loading;
(b) placing a tubular carrier loaded with seed crystals in a casting solution, wherein the casting solution contains a template agent TPAOH, a silicon source, an aluminum source and water for hydrothermal synthesis, the synthesis temperature is 150 ℃, and the synthesis time is 24 hours, wherein the silicon source is TEOS, and the aluminum source is sodium metaaluminate;
(c) roasting the zeolite membrane synthesized in the step (b) at the temperature of 450 ℃ for 4h, wherein the heating and cooling rates are both 1 ℃/min;
(d) soaking the zeolite membrane to be repaired in deionized water for a whole day, and drying at 60 ℃ for 6 h;
(e) putting the zeolite membrane into a tubular membrane module, and carrying out vacuum degassing treatment on the zeolite membrane for 3 hours;
(f) passing an aqueous phase solution containing 3% m-phenylenediamine through the inside of the tubular zeolite membrane at a rate of 1mL/min for a first contact time of 20s; herein, the contact time is defined as the time during which the aqueous/organic phase solution is contacted at a point inside/outside the tubular support;
(g) passing deionized water through the inside/outside of the tubular zeolite membrane at a rate of 0.1ml/min for a second contact time of 2s;
(h) passing an organic phase solution containing 0.5% phthaloyl chloride through the outside of the tubular zeolite membrane at a rate of 1ml/min for a third contact time of 10s;
(i) repeating steps (f) - (h) 2 times;
(j) the zeolite membrane was removed from the tubular membrane module and dried at 100 ℃ for 10 min.
Example 2
A tubular zeolite membrane for reverse osmosis water treatment was prepared as follows.
(b) Pretreating a tubular carrier, and then soaking the tubular carrier into a ZSM-5-containing zeolite solution (1%) to carry out seed crystal loading;
(b) placing a tubular carrier loaded with seed crystals in a casting solution, wherein the casting solution contains a template agent TPAOH, a silicon source, an aluminum source and water for hydrothermal synthesis, the synthesis temperature is 150 ℃, and the synthesis time is 24 hours, wherein the silicon source is TEOS, and the aluminum source is sodium metaaluminate;
(c) roasting the zeolite membrane synthesized in the step (b) at the temperature of 450 ℃ for 4h, wherein the heating and cooling rates are both 1 ℃/min;
(d) soaking the zeolite membrane to be repaired in deionized water for a whole day, and drying at 60 ℃ for 6 h;
(e) putting the zeolite membrane into a tubular membrane module, and carrying out vacuum degassing treatment on the zeolite membrane for 3 hours;
(f) passing an aqueous phase solution containing 3% m-phenylenediamine through the inside of the tubular zeolite membrane at a rate of 1mL/min for a first contact time of 20s; herein, the contact time is defined as the time during which the aqueous/organic phase solution is contacted at a point inside/outside the tubular support;
(g) passing deionized water through the inside/outside of the tubular zeolite membrane at a rate of 0.1ml/min for a second contact time of 2s;
(h) passing an organic phase solution containing 0.5% phthaloyl chloride through the outside of the tubular zeolite membrane at a rate of 1ml/min for a third contact time of 10s;
(i) repeating steps (f) - (h) 4 times;
(j) the zeolite membrane was removed from the tubular membrane module and dried at 100 ℃ for 10 min.
Example 3
A tubular zeolite membrane for reverse osmosis water treatment was prepared as follows.
(c) Pretreating a tubular carrier, and then soaking the tubular carrier into a ZSM-5-containing zeolite solution (1%) to carry out seed crystal loading;
(b) placing a tubular carrier loaded with seed crystals in a casting solution, wherein the casting solution contains a template agent TPAOH, a silicon source, an aluminum source and water for hydrothermal synthesis, the synthesis temperature is 150 ℃, and the synthesis time is 24 hours, wherein the silicon source is TEOS, and the aluminum source is sodium metaaluminate;
(c) roasting the zeolite membrane synthesized in the step (b) at the temperature of 450 ℃ for 4h, wherein the heating and cooling rates are both 1 ℃/min;
(d) soaking the zeolite membrane to be repaired in deionized water for a whole day, and drying at 60 ℃ for 6 h;
(e) putting the zeolite membrane into a tubular membrane module, and carrying out vacuum degassing treatment on the zeolite membrane for 3 hours;
(f) passing an aqueous phase solution containing 3% m-phenylenediamine through the inside of the tubular zeolite membrane at a rate of 1mL/min for a first contact time of 20s; herein, the contact time is defined as the time during which the aqueous/organic phase solution is contacted at a point inside/outside the tubular support;
(g) passing deionized water through the inside/outside of the tubular zeolite membrane at a rate of 0.1ml/min for a second contact time of 2s;
(h) passing an organic phase solution containing 0.5% phthaloyl chloride through the outside of the tubular zeolite membrane at a rate of 1ml/min for a third contact time of 10s;
(i) repeating steps (f) - (h) 6 times;
(j) the zeolite membrane was removed from the tubular membrane module and dried at 100 ℃ for 10 min.
Comparative example 1
A tubular zeolite membrane for reverse osmosis water treatment was prepared as follows.
(d) Pretreating a tubular carrier, and then soaking the tubular carrier into a ZSM-5-containing zeolite solution (1%) to carry out seed crystal loading;
(b) placing a tubular carrier loaded with seed crystals in a casting solution, wherein the casting solution contains a template agent TPAOH, a silicon source, an aluminum source and water for hydrothermal synthesis, the synthesis temperature is 150 ℃, and the synthesis time is 24 hours, wherein the silicon source is TEOS, and the aluminum source is sodium metaaluminate;
(c) roasting the zeolite membrane synthesized in the step (b) at the temperature of 450 ℃ for 4h, wherein the heating and cooling rates are both 1 ℃/min;
comparative example 2
A tubular zeolite membrane for reverse osmosis water treatment was prepared as follows.
(e) Pretreating a tubular carrier, and then soaking the tubular carrier into a ZSM-5-containing zeolite solution (1%) to carry out seed crystal loading;
(b) placing a tubular carrier loaded with seed crystals in a casting solution, wherein the casting solution contains a template agent TPAOH, a silicon source, an aluminum source and water for hydrothermal synthesis, the synthesis temperature is 150 ℃, and the synthesis time is 24 hours, wherein the silicon source is TEOS, and the aluminum source is sodium metaaluminate;
(c) roasting the zeolite membrane synthesized in the step (b) at the temperature of 450 ℃ for 4h, wherein the heating and cooling rates are both 1 ℃/min;
(d) soaking the zeolite membrane to be repaired in deionized water for a whole day, and drying at 60 ℃ for 6 h;
(e) putting the zeolite membrane into a tubular membrane module, and carrying out vacuum degassing treatment on the zeolite membrane for 3 hours;
(f) passing an aqueous phase solution containing 3% m-phenylenediamine through the inside of the tubular zeolite membrane at a rate of 1mL/min for a first contact time of 20s; herein, the contact time is defined as the time during which the aqueous/organic phase solution is contacted at a point inside/outside the tubular support;
(g) passing an organic phase solution containing 0.5% phthaloyl chloride through the outside of the tubular zeolite membrane at a rate of 1ml/min for a third contact time of 10s;
(h) repeating steps (f) - (g) 4 times;
(i) the zeolite membrane was removed from the tubular membrane module and dried at 100 ℃ for 10 min.
The membranes repaired in the comparative examples and examples were placed in a 0.1M NaCl solution and subjected to desalting test at 25 ℃ at pH 7.5 and pressure 2.75MPa, and the results are shown in Table I.
Watch 1
| Sample (I) | Salt rejection | Flux (Kg/(m)2.h)） |
| Example 1 | 84.1% | 1.27 |
| Example 2 | 90.4% | 1.20 |
| Example 3 | 91.8% | 1.13 |
| Comparative example 1 | 37.1% | 2.4 |
| Comparative example 2 | 91.7% | 0.78 |
As can be seen from the above table, the membrane after firing has a poor salt rejection and a high flux due to defective pores generated during the firing or membrane preparation. After the method adopted by the invention is adopted for repairing, the desalination rate of the membrane is greatly improved, the flux of the membrane is also kept in a higher range, and the desalination rate and the water flux of the membrane can be adjusted in a certain range according to different repairing times.
Claims (7)
1. A preparation method of a tubular zeolite membrane applied to reverse osmosis water treatment, wherein the tubular zeolite membrane is loaded on a ZSM-5 zeolite membrane on a tubular carrier, and is characterized by comprising the following steps:
(a) pretreating a tubular carrier, and then soaking the tubular carrier into a ZSM-5-containing zeolite solution for seed crystal loading;
(b) placing the tubular carrier loaded with the seed crystal into a membrane casting solution, wherein the membrane casting solution contains a template agent TPAOH, a silicon source, an aluminum source, sodium hydroxide and water for hydrothermal synthesis, the synthesis temperature is 120-180 ℃, and the synthesis time is 12-48 h;
(c) roasting the zeolite membrane synthesized in the step (b) at the temperature of 400-500 ℃ for 4-6h, wherein the heating and cooling rates are 1-2 ℃/min;
(d) soaking the calcined zeolite membrane in deionized water for 12-24h, and drying at 50-80 deg.C for 6-8 h;
(e) putting the zeolite membrane into a tubular membrane component, and carrying out vacuum degassing treatment on the zeolite membrane for 1-3 h;
(f) passing an aqueous phase solution containing a polyamine through the inside of the tubular zeolite membrane at a rate of 0.2-2mL/min for a first contact time of 10-20s;
(g) passing deionized water through the inner/outer side of the tubular zeolite membrane at a speed of 0.05-0.5mL/min for a second contact time of 2-4s;
(h) passing the organic phase solution containing the polyacyl chloride through the outer side of the tubular zeolite membrane at the speed of 0.5-2mL/min, wherein the third contact time is 10-20s;
(i) repeating steps (f) - (h) 2-6 times;
(j) taking out the zeolite membrane from the tubular membrane module, drying at 60-100 ℃ for 5-20min to repair the defects of the zeolite membrane by adopting a mode of generating polyamide by interfacial polymerization; the inner diameter of the tubular carrier is 5-12 mm; in the tubular membrane component, the distance between the zeolite membrane and the inner wall of the tubular membrane component is 3-8 mm.
2. The method of claim 1, wherein the polyamine is one or more of m-phenylenediamine, p-phenylenediamine, xylylenediamine, and 2, 4-diaminotoluene.
3. The method according to claim 1, wherein the acid chloride solution is one or more of phthaloyl chloride, terephthaloyl chloride, isophthaloyl chloride, and trimesoyl chloride.
4. The method according to claim 1, wherein the organic solvent in the organic phase solution is one or more of cyclohexane, heptane, octane, naphtha, ISOPARE or mineral oil.
5. The method according to claim 1, wherein the concentration of polyamine in the aqueous phase solution is 1% to 5% and the concentration of acid chloride in the organic phase solution is 0.05 to 0.5%.
6. A tubular zeolite membrane for reverse osmosis water treatment prepared according to the method of any one of claims 1 to 5.
7. Use of the tubular zeolite membrane of claim 6 in reverse osmosis water treatment, including wastewater treatment, desalination of sea water, pure water production.
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| US12040517B2 (en) | 2022-11-15 | 2024-07-16 | Rahul S. Nana | Reverse electrodialysis or pressure-retarded osmosis cell and methods of use thereof |
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| US11502322B1 (en) | 2022-05-09 | 2022-11-15 | Rahul S Nana | Reverse electrodialysis cell with heat pump |
| US11502323B1 (en) | 2022-05-09 | 2022-11-15 | Rahul S Nana | Reverse electrodialysis cell and methods of use thereof |
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