CN107670511B - Flexible anti-pollution ceramic membrane and preparation method thereof - Google Patents
Flexible anti-pollution ceramic membrane and preparation method thereof Download PDFInfo
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- CN107670511B CN107670511B CN201710899083.6A CN201710899083A CN107670511B CN 107670511 B CN107670511 B CN 107670511B CN 201710899083 A CN201710899083 A CN 201710899083A CN 107670511 B CN107670511 B CN 107670511B
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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
- 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
- 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
- B01D71/02—Inorganic material
- B01D71/024—Oxides
- B01D71/025—Aluminium oxide
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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
- B01D71/027—Silicium oxide
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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
- B01D71/24—Rubbers
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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
- B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
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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
- B01D2325/36—Hydrophilic membranes
Abstract
The invention discloses a flexible anti-pollution ceramic membrane which is prepared from the following components in percentage by mass through a blending-die pressing forming method: 39-55% of coupling agent modified inorganic nano material, 40-52% of elastomer material, 3-8% of pore-forming agent and 2-7% of cross-linking agent; according to the membrane, the hydrophilic elastic material is added into the inorganic raw material, so that the softening and hydrophilic properties of the ceramic membrane are greatly enhanced, and the mechanical strength and the pollution resistance of the membrane are improved; the preparation process of the flexible anti-pollution ceramic membrane is simple and easy to control, high-temperature sintering is not needed, and the preparation cost is greatly reduced.
Description
Technical Field
The invention belongs to the technical field of membrane separation, and particularly relates to a flexible anti-pollution ceramic membrane and a preparation method thereof.
Background
Ceramic membrane separation technology is one of the most advanced membrane separation technologies in the world in recent years. The ceramic film is one of solid films, mainly made of Al2O3、ZrO2、TiO2And the like. The ceramic membrane is a product formed by uniformly mixing inorganic raw materials with additives, reacting, molding and then calcining at high temperature, and the ceramic membrane contains a large number of pores which are mutually communicated, the porosity is more than 30%, and the average pore diameter is generally 1-10 mu m. Due to the advantages of good chemical stability, acid resistance, alkali resistance, strong oxidant resistance and organic solvent resistance, good anti-microbial corrosion capability and biochemical compatibility, narrow pore size distribution, high separation precision and the like, the method is widely applied to separation of impurities in liquid in the industries of chemical industry, food, medicine, environmental protection and the like, and shows unique advantages and broad prospects.
Chinese patent application CN101337808 discloses a process for preparing a ceramic membrane support body by using alpha-alumina powder; the manufacturing process comprises the following steps: screening and removing impurities from alumina raw material, adding composite mineralizer, mixing to obtain alumina mixture, placing the alumina mixture in high-temperature furnace, high-temperature calcining to obtain alumina powderThe phase inversion temperature is 1500-1700 ℃. The ceramic membrane prepared by the method has uniform pore size distribution and good corrosion resistance after high-temperature calcination. However, in this method, the porous ceramic membrane is often made of alumina (. alpha. -A1)2O3Not less than 99 wt.) is used as a raw material, the raw material is expensive, high-temperature treatment is required in each step of preparation, parameters required to be controlled for coating a film layer are more, the process is complicated, the production period is longer, the cost is higher, and the quality of a finished product cannot be ensured. Expensive raw materials and high sintering cost keep the sale price of the ceramic membrane high, and the application of the ceramic membrane in large-scale industrial production is severely limited. Meanwhile, in order to improve the porosity of the porous ceramic membrane, a common method is to add an inorganic or organic pore-forming material which can be burned out at high temperature when preparing powder, and the method is used for improving the porosity and usually sacrifices the mechanical strength of the ceramic membrane; the prepared ceramic membrane is often fragile and easy to damage, and the use of the ceramic membrane is seriously influenced.
Chinese patent application 201310368448.4 discloses a method for preparing an organic-inorganic hybrid separation membrane; firstly, carrying out surface modification on inorganic nanoparticles to reduce the surface energy of the inorganic nanoparticles and enhance the compatibility with a polymer membrane material; then mixing the surface modified inorganic nano particles, the polymer film material, the additive and the solvent to obtain a membrane casting solution, and preparing a flat plate or a hollow fiber organic-inorganic hybrid separation membrane by a traditional phase conversion method. Compared with the prior art, the method obviously inhibits the agglomeration phenomenon of the inorganic nano particles, improves the dispersibility of the inorganic nano particles in the casting solution, and has better film-making repeatability. However, the membrane prepared by the method has low degree of uniform pore size distribution and difficult guarantee of the mechanical strength of the membrane; in the process of treating the feed liquid, certain components in the treated feed liquid are adsorbed and deposited on the membrane surface or enter membrane pores, and even the membrane pores are blocked, so that the osmotic resistance of the membrane is greatly increased; in the case of membrane separation processes, membrane fouling begins as soon as the feed contacts the membrane; after the operation is started, concentration difference polarization phenomenon is generated, and particularly under the conditions of low flow rate and high solute concentration, when the membrane surface reaches or exceeds the saturation solubility of the solute, gel layer is formed, so that the membrane flux does not depend on the applied pressure, and the membrane flux is rapidly reduced.
The use and development of the ceramic membrane are seriously influenced by various defects of high manufacturing cost, high brittleness, easy pollution and the like of the ceramic membrane.
Disclosure of Invention
In order to solve the problems, the invention provides a flexible anti-pollution ceramic membrane, which is characterized in that a hydrophilic elastic material is added into an inorganic raw material, so that the softening and the hydrophilic performance of the ceramic membrane are greatly enhanced, and the mechanical strength and the anti-pollution performance of the membrane are improved.
The flexible anti-pollution ceramic membrane is prepared from the following components in percentage by mass through a blending-die pressing forming method: 39-55% of coupling agent modified inorganic nano material, 40-52% of elastomer material, 3-8% of pore-forming agent and 2-7% of cross-linking agent.
The preparation process of the coupling agent modified inorganic nano material comprises the following steps: ultrasonically hydrolyzing the coupling agent in an ethanol solution with the pH value of 3-5 and the volume concentration of 95% for 20-45 min to obtain hydrolysate of the coupling agent; then adding the inorganic nano particles into coupling agent hydrolysate, reacting at 50-150 ℃, filtering, drying the solid, and scattering to obtain the coupling agent modified inorganic nano material; wherein the dosage of the coupling agent is 5-15% of the total mass of the coupling agent and the inorganic nano particles, and the dosage of the inorganic nano particles is 85-95% of the total mass of the coupling agent and the inorganic nano particles.
The inorganic nano particles are nano Al2O3Nano SiO2Nano ZrO 22TiO 2 nanoparticles2One kind of (1).
The elastomer material is ethylene-vinyl acetate copolymer, ethylene propylene rubber or hydrophilic thermoplastic elastomer material.
The pore-forming agent is one of sodium bicarbonate, urea, PVP, PEG and PVA.
The cross-linking agent is one of triallyl isocyanurate, triallyl cyanurate, tricarboxymethyl propane trimethacrylate, tripropylene glycol diacrylate, ethyl trisilicate and methyl methacrylate.
The coupling agent is one or more of aluminate coupling agent, titanate coupling agent, rare earth coupling agent and silane coupling agent.
The preparation method of the flexible anti-pollution ceramic membrane comprises the following steps:
(1) mixing the inorganic nano material modified by the coupling agent and the elastomer material in a mixing roll for 20-30min at 100-150 ℃;
(2) mixing the mixture obtained in the step (1), a pore-forming agent and a crosslinking agent in a mixing roll for 10-30 min at 100-200 ℃ to obtain a casting film mixture;
(3) putting the casting film blend obtained in the step (2) into a mould press, and pressing at 100-200 ℃ to form a mould; and cooling the prepared membrane to room temperature, and soaking in an ethanol-water solution for 12-24 hours to obtain the flexible anti-pollution ceramic membrane.
The ethanol-water solution is prepared from ethanol and water according to the volume ratio of 1: 1-1: 2.
The method has the advantages and the technical effects that:
(1) high hydrophilic performance and strong anti-pollution capability
The hydrophilic elastomer material is introduced, so that the hydrophilic performance of the ceramic membrane is greatly improved; in the mass transfer process of filtration, pollutants such as colloid, oil, protein and the like are agglomerated on the surface of the membrane into a spherical aggregate, the spherical aggregate is easy to separate from the surface of the membrane and can be cleaned by simple backwashing, the hydrophilic membrane has low operation pressure and low chemical cleaning frequency, and the service cycle of the ceramic membrane is prolonged;
(2) soft texture, excellent mechanical property, uneasy damage
By controlling the amount of the elastomer material and the cross-linking agent, ceramic membranes with different strengths are prepared, so that the application range is wide, and the service life is long;
(3) the process is simple and easy to control, high-temperature sintering is not needed, and the preparation cost is greatly reduced.
Detailed Description
The technical solution of the present invention is further described below with reference to specific examples, but the scope of the present invention is not limited to the description.
Example 1: the flexible anti-pollution ceramic membrane is prepared from the following components in percentage by mass through a blending-die pressing forming method: coupling agent modified nano Al2O3 45 percent of ethylene-vinyl acetate copolymer, 46 percent of sodium bicarbonate and 3 percent of triallyl isocyanurate;
the coupling agent modified nano Al2O3Ultrasonically hydrolyzing an aluminate coupling agent in an ethanol solution with the pH value of 3 and the volume concentration of 95 percent for 25min to obtain hydrolysate of aluminate; then adding nano Al2O3Mixing the powders, reacting at 120 deg.C for 30min, filtering, oven drying the solid, and scattering to obtain modified nanometer Al2O3Powder; wherein the usage amount of the aluminate is aluminate and nano Al2O38% of total mass, nano Al2O3The dosage of the aluminum acid ester and the nano Al2O392% of the total mass.
The preparation method of the flexible anti-pollution ceramic membrane comprises the following steps:
(1) nano Al modified by coupling agent at 120 deg.C2O3Mixing with ethylene-vinyl acetate copolymer (vinyl acetate content of 28 wt.%) in a mixer for 20 min;
(2) mixing the mixture obtained in the step (1) with sodium bicarbonate and triallyl isocyanurate in a mixing roll for 20min at 100 ℃ to obtain a casting film mixture;
(3) putting the casting film blend obtained in the step (2) into a mould press, and pressing and forming at 150 ℃; and cooling the prepared membrane to room temperature, and soaking in an ethanol-water solution for 24 hours to obtain the flexible anti-pollution ceramic membrane, wherein the ethanol-water solution is prepared from ethanol and water according to the volume ratio of 1: 1.
In this example, the film was subjected to a mechanical property test and a contact angle test. Through determination, the tensile strength of the prepared flexible anti-pollution ceramic membrane is 22.8MPa, and the impact strength is 38.68 J.m-1(ii) a The contact angle is 39.53 degrees, the hydrophilicity is excellent, and the pollution resistance is excellent; and the result of the experiment on the removal effect of the particulate matters in the well water is shown in the table 1.
TABLE 1 results on removal of particulate matter from well water
As can be seen from Table 1, the content of the well water suspended matter is 165-403 mg/L, and the particle size distribution is 2.3-2.8 μm; after being filtered by the ceramic membrane, the content of suspended matters in the effluent is less than 3mg/L, the particle size is less than 2 mu m, the water quality is greatly improved, the filtering effect of the ceramic membrane is excellent, and the performance is stable.
Example 2: the flexible anti-pollution ceramic membrane is prepared from the following components in percentage by mass through a blending-die pressing forming method: coupling agent modified nano SiO240%, ethylene-vinyl acetate copolymer (vinyl acetate content 40 wt.%), 50%, PVA 4%, triallyl cyanurate 6%;
the coupling agent modified nano SiO2 is prepared by ultrasonically hydrolyzing titanate coupling agent in 95% ethanol solution with pH of 3.5 for 30min to obtain titanate hydrolysate; then adding nano SiO2Uniformly mixing, reacting at 100 ℃ for 30min, drying and scattering to obtain the modified nano SiO2Powder; wherein the dosage of the titanate coupling agent is the coupling agent and the nano SiO210% of total mass, nano SiO2The dosage of the coupling agent and the nano SiO290 percent of the total mass.
The preparation method of the flexible anti-pollution ceramic membrane comprises the following steps:
(1) at 130 ℃, modifying titanate coupling agent into nano SiO2Mixing the powder with ethylene-vinyl acetate copolymer (vinyl acetate content of 40 wt.%) in a mixer for 25 min;
(2) mixing the material obtained in the step (1) with PVA and triallyl cyanurate in a mixing roll for 15min at 120 ℃ to obtain a flexible anti-pollution ceramic membrane casting film mixture;
(3) putting the casting film blend obtained in the step (2) into a mould press, and pressing at 120 ℃ to form a mould; and cooling the prepared membrane to room temperature, and soaking in an ethanol-water solution for 20 hours to obtain the flexible anti-pollution ceramic membrane, wherein the ethanol-water solution is prepared from ethanol and water according to the volume ratio of 1: 2.
In this example, the film was subjected to mechanical property test and contact angle test. Through measurement, the tensile strength of the prepared flexible anti-pollution ceramic membrane is 20.1MPa, and the impact strength is 30.56 J.m-1(ii) a The contact angle is 37.92 degrees, the hydrophilicity is excellent, and the pollution resistance is excellent; and the tea soup filtration experiment was carried out, and the results are shown in table 2.
TABLE 2 interception of tea soup contents by Flexible anti-pollution ceramic Membrane
The results show that the ceramic membrane can retain chemical components in the tea soup, wherein protein is one of the known important factors causing the problem of tea beverage sedimentation, the ceramic membrane can retain the protein as high as 51.6 percent, and the quality of the tea soup is greatly improved. Meanwhile, the retention rate of 3 substances of tea polyphenol, amino acid and caffeine is relatively low, the 3 substances are the most main quality components in the tea soup, most of the 3 substances are remained in the tea soup, and the tea beverage is beneficial to maintaining the flavor of the tea beverage.
Example 3: the flexible anti-pollution ceramic membrane is prepared from the following components in percentage by mass through a blending-die pressing forming method: coupling agent modified nano TiO255 percent of ethylene propylene rubber, 40 percent of PEG 3 percent and 2 percent of tricarboxymethyl propane trimethacrylate;
the coupling agent modified nano TiO2Ultrasonically hydrolyzing a silane coupling agent in an ethanol solution with the pH value of 4.2 and the volume concentration of 95 percent for 30min to obtain hydrolysate of the silane coupling agent; then adding nano TiO2Mixing the powders, reacting at 100 deg.C for 30min, oven drying, and scattering to obtain modified nanometer TiO2Powder; wherein the dosage of the silane coupling agent is the coupling agent and the nano TiO215% of total mass, nano TiO2The dosage of the coupling agent and the nano TiO285% of the total mass;
the preparation method of the flexible anti-pollution ceramic membrane comprises the following steps:
(1) modifying coupling agent modified nano TiO at 140 DEG C2Mixing with ethylene propylene rubber in a mixing roll for 20 min;
(2) mixing the mixture obtained in the step (1) with PEG and tricarboxymethyl propane trimethacrylate in a mixing roll for 30min at 110 ℃ to obtain a casting film mixture;
(3) putting the casting film blend obtained in the step (2) into a mould press, and pressing and forming at 150 ℃; and cooling the prepared membrane to room temperature, and soaking in an ethanol-water solution for 12 hours to obtain the flexible anti-pollution ceramic membrane, wherein the ethanol-water solution is prepared from ethanol and water according to the volume ratio of 1: 2.
In this example, the membrane was subjected to mechanical property test and contact angle test, and the tensile strength and impact strength of the prepared flexible anti-pollution ceramic membrane were measured to be 30.2MPa and 42.53J · m-1(ii) a The contact angle is 40.05 degrees, the good hydrophilic performance is shown, and the pollution resistance is excellent; and a citric acid mother liquor filtration experiment, the test results are shown in the following table 3:
TABLE 3 filtration test results of citric acid mother liquor
The result shows that the ceramic membrane has excellent treatment effect on the citric acid mother liquor. After 3 times of filtration, the light transmittance is increased from 63.5 percent to 85.1 percent, the turbidity is reduced from 67.7NTU to 1.96NTU, and the quality of the citric acid mother liquor is greatly improved.
Claims (6)
1. The flexible anti-pollution ceramic membrane is characterized by being prepared from the following components in percentage by mass through a blending-die pressing forming method: 39-55% of coupling agent modified inorganic nano material, 40-52% of elastomer material, 3-8% of pore-forming agent and 2-7% of cross-linking agent;
the preparation process of the coupling agent modified inorganic nano material comprises the following steps: ultrasonically hydrolyzing the coupling agent in an ethanol solution with the pH value of 3-5 and the volume concentration of 95% for 20-45 min to obtain hydrolysate of the coupling agent; then adding the inorganic nano particles into coupling agent hydrolysate, reacting at 50-150 ℃, filtering, drying the solid, and scattering to obtain the coupling agent modified inorganic nano material; wherein the dosage of the coupling agent is 5-15% of the total mass of the coupling agent and the inorganic nano particles, and the dosage of the inorganic nano particles is 85-95% of the total mass of the coupling agent and the inorganic nano particles;
the inorganic nano particles are nano Al2O3Nano SiO2Nano ZrO 22TiO 2 nanoparticles2One of (1);
the elastomer material is ethylene-vinyl acetate copolymer, ethylene propylene rubber or hydrophilic thermoplastic elastomer material.
2. The flexible anti-contamination ceramic membrane of claim 1, wherein: the pore-forming agent is one of sodium bicarbonate, urea, PVP, PEG and PVA.
3. The flexible anti-contamination ceramic membrane of claim 1, wherein: the cross-linking agent is one of triallyl isocyanurate, triallyl cyanurate, tricarboxymethyl propane trimethacrylate, tripropylene glycol diacrylate, ethyl trisilicate and methyl methacrylate.
4. The flexible anti-contamination ceramic membrane of claim 1, wherein: the coupling agent is one or more of aluminate coupling agent, titanate coupling agent, rare earth coupling agent and silane coupling agent.
5. The method for preparing a flexible anti-contamination ceramic membrane according to claim 1, comprising the following steps:
(1) mixing the inorganic nano material modified by the coupling agent and the elastomer material in a mixing roll for 20-30min at 120-150 ℃;
(2) mixing the mixture obtained in the step (1), a pore-forming agent and a crosslinking agent in a mixing roll for 10-30 min at 100-150 ℃ to obtain a casting film mixture;
(3) putting the casting film blend obtained in the step (2) into a mould press, and pressing at 100-150 ℃ to form a mould; and cooling the prepared membrane to room temperature, and soaking in an ethanol-water solution for 12-24 hours to obtain the flexible anti-pollution ceramic membrane.
6. The method for preparing a flexible anti-contamination ceramic membrane according to claim 5, wherein: the ethanol-water solution is prepared from ethanol and water according to the volume ratio of 1: 1-1: 2.
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| CN105542400A (en) * | 2016-01-12 | 2016-05-04 | 扬州大学 | Nucleation modification method of polyester elastomer for optical cable loose tube |
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| 陶瓷膜制备及在水处理中的应用;万昱堃等;《净水技术》;20160425;第35卷(第2期);第2节 * |
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