CN108479421B - Manufacturing method of efficient inorganic membrane filter plate for water treatment - Google Patents
Manufacturing method of efficient inorganic membrane filter plate for water treatment Download PDFInfo
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- CN108479421B CN108479421B CN201810504238.6A CN201810504238A CN108479421B CN 108479421 B CN108479421 B CN 108479421B CN 201810504238 A CN201810504238 A CN 201810504238A CN 108479421 B CN108479421 B CN 108479421B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D67/0039—Inorganic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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Abstract
The invention discloses a method for manufacturing a water treatment high-efficiency inorganic membrane filter plate, which comprises the steps of firstly, corundum sand, Suzhou soil and α -Al2O3Titanium aluminium carbide, feldspar, methyl cellulose, dextrin, lepidolite, bentonite, talcum powder and oleic acid, stirring according to a certain proportion, ageing, mechanically pressing and forming, drying and shaping, spraying a layer of zeolite slurry film on the plate-shaped surface, primary sintering, coating film slurry consisting of corundum sand, Suzhou soil, feldspar, titanium oxide sol, fiber, talcum powder, bentonite, dextrin, lepidolite and sodium humate, naturally drying, secondary sintering, cooling, discharging from a furnace, assembling, inspecting, packaging and warehousing. The high-efficiency inorganic membrane filter plate is widely used for the water removal treatment of industrial waste such as chemical industry, food, medicine, fertilizer, metallurgy, papermaking, printing and dyeing and the like, and has the advantages of high filtering efficiency, strong dirt interception capability, good effluent quality, long service life and low operation cost.
Description
Technical Field
The invention relates to solid-liquid separation of wastewater in the field of environmental protection, and aims to provide a manufacturing method of a high-efficiency inorganic membrane filter plate with high efficiency, wide adaptability and low price.
Background
In the process of removing SS and oil in wastewater, activated carbon adsorption, modified bentonite adsorption and macroporous resin adsorption are commonly used as the most representative in the traditional technology, and the principle is that the solid adsorbent has good physical adsorption and surface chemical activity due to large specific surface area, high porosity, strong polarity and charged polarity of particles, and has good adsorption capacity on various pollutants in the wastewater, so that the purpose of purifying the water body is achieved. However, the traditional filtering technology has the defects of high price, single function, high investment cost, poor backwashing effect and the like.
The inorganic membrane filtration is a new technology developed in recent years, can complete separation, concentration and purification, and has the characteristics of energy conservation, environmental protection, easy operation and control and the like. Inorganic membranes are classified into ceramic membranes and metal membranes according to the type of membrane material. The ceramic membrane is an asymmetric inorganic membrane formed by preparing an inorganic ceramic material through a special process. The ceramic membrane is a permeable membrane with a separation function and takes a porous ceramic material as a medium carrier and a microporous ceramic membrane as a filter layer. The ceramic film is mainly an aluminum oxide film, a cobalt oxide film, a silicon oxide film, a silicic acid film, a silicon carbide film, a titanium oxide film, a zirconium oxide film, or the like. According to market research, the current inorganic ceramic membrane, especially the inorganic ceramic membrane plate, has the following problems in practical use: firstly, because the thickness of the ceramic membrane plate is generally 8-15 mm, the area is 1-3 square meters, the strength of the ceramic membrane plate is not high, the brittleness is large, and the ceramic membrane plate is easy to crack after working for a period of time under severe conditions, so that the filtering efficiency is reduced; secondly, the surface film-hanging adsorbability of the ceramic plate carrier is not high, and the film layer can locally fall off and separate, so that the filtering effect is influenced; thirdly, the membrane flux of the membrane layer is not high enough, the sizes of membrane pores are not uniformly dispersed, the membrane pores are easy to block, the backwashing difficulty is increased, and the filtration cost is increased. Ceramic membranes are mainly classified into two types, tubular ceramic membranes and flat ceramic membranes. The tube wall of the tubular ceramic membrane is densely distributed with micropores, under the action of pressure, the raw material liquid flows in the membrane tube or outside the membrane, small molecular substances (or liquid) permeate the membrane, and large molecular substances (or solid) are intercepted by the membrane, so that the purposes of separation, concentration, purification, environmental protection and the like are achieved. The plate surface of the flat ceramic membrane is densely distributed with micropores, according to the fact that the permeability is different when the diameters of molecules of permeated substances are different within a certain membrane aperture range, the pressure difference between two sides of the membrane is used as a driving force, the membrane is used as a filtering medium, and under the action of a certain pressure, when feed liquid flows through the surface of the membrane, only water, inorganic salt and small molecular substances are allowed to permeate through the membrane, and macromolecular substances such as suspended matters, glue, microorganisms and the like in the water are prevented from passing through the membrane. Compared with organic membranes, the ceramic membrane has the advantages of high separation efficiency, stable effect, good chemical stability, acid and alkali resistance, organic solvent resistance, bacteria resistance, high temperature resistance, pollution resistance, high mechanical strength, good regeneration performance, simple separation process, low energy consumption, simple and convenient operation and maintenance, long service life and the like, is successfully applied to various fields of food, beverage, plant (medicine) deep processing, biomedicine, fermentation, fine chemical industry and the like, and can be used for separation, clarification, purification, concentration, sterilization, desalination and the like in the technical process.
Disclosure of Invention
Aiming at the problems of the ceramic membrane plate in the prior art in practical use, the invention provides the manufacturing method of the water treatment high-efficiency inorganic membrane filter plate with the ceramic carrier, which has high mechanical strength, good impact resistance, strong membrane-hanging capability of surface adsorption and large membrane flux.
The manufacturing method of the water treatment high-efficiency inorganic membrane filter plate comprises the following steps:
a. 60-80 meshes of 50-60wt% of corundum, 20-30wt% of Suzhou soil and 5-10wt% of α -Al2O3The raw materials of 3-5wt% of titanium aluminum carbide, 0.5-1wt% of feldspar, 5.2-10.5wt% of methyl cellulose, 0.5-1wt% of dextrin, 0.3-0.8wt% of lepidolite, 0.3-1wt% of bentonite, 0.3-1wt% of talcum powder and 0.5-1wt% of oleic acid are firstly mixed according to the proportion2O3The Suzhou soil, the feldspar, the dextrin, the lepidolite, the bentonite, the talcum powder and the oleic acid are put into a stirrer to be stirred for 15 minutes, and then the methyl cellulose which is well proportioned is put into the stirrer to be stirred to prepare a mixture;
b. putting the mixture into a closed space for ageing for 15-20 hours, putting the aged mixture into a hydraulic press for pressing into a plate-shaped green body, and naturally drying the plate-shaped green body for 1-2 days;
c. drying and shaping the naturally dried plate-shaped blank in a dryer at the drying temperature of 30-60 ℃, cooling to normal temperature, spraying a layer of zeolite slurry film on the surface of the plate,
d. c, placing the plate-shaped blank in the step c into a shuttle kiln, preserving heat for 3-5 hours at 1300-1500 ℃, performing primary sintering, cooling along with the furnace, and discharging to obtain a high-efficiency inorganic membrane filter plate carrier;
e. putting 200-mesh 300-mesh corundum sand 60-80wt%, Suzhou soil 5-15wt%, feldspar 0.1-0.3wt%, titania sol 5-10wt%, fiber 5-10wt%, talcum powder 0.1-0.3wt%, bentonite 0.1-0.3wt%, dextrin 0.3-0.5wt%, lepidolite 0.3-0.5wt%, sodium humate 0.01-0.03wt%, dolomite 0.01-0.03wt%, glass water 0.05-0.15wt%, soda 0.01-0.03wt%, defoaming agent 0.2-0.3wt%, polypropylene 0.1-0.3wt% and water in a ball mill for ball milling, filtering and preparing film-forming slurry;
f. coating the high-efficiency inorganic membrane filter plate carrier block by using a soft brush, and naturally drying the coated filter plate for 2-3 days at normal temperature;
g. placing the filter plate coated with the membrane material and dried into a shuttle kiln for secondary sintering at the sintering temperature of 1400 ℃ and 1550 ℃ and keeping the temperature for 3-5 h;
h. assembling: and sealing the external thread connector and the reserved holes of the high-efficiency inorganic membrane filter plates by using glue, inspecting each high-efficiency inorganic membrane filter plate, and packaging and warehousing after the high-efficiency inorganic membrane filter plates are qualified.
The technological features of the present invention are that corundum sand is used as main material to form the skeleton of the substrate in the ceramic plate as the carrier for producing ceramic film plate, and certain amount of α -Al is added2O3And titanium aluminum carbide (TiAl), α -Al in the ceramic plate in one sintering oxidation process2O3The crystal grains are dispersed to the interface of the skeleton to make the skeleton become stable, so that the strength of the matrix is raised and the brittleness of the matrix is lowered.
The invention has the technical characteristics that: secondly, thick slurry (the viscosity is 800-900 mpa.s) prepared by dissolving and mixing the zeolite powder with the particle size of 200-300 meshes and ethanol is sprayed on the surface of the ceramic plate, so that an adsorption hanging membrane layer is arranged on the surface of the ceramic plate, the adsorption hanging membrane layer can be well, uniformly dispersed, tightly and firmly adsorbed, and the filtration membrane layer is not easy to fall off and separate and is more resistant to scouring.
The invention has the technical characteristics that: and thirdly, in order to form a filtering membrane layer which has large membrane flux, is not easy to block and is convenient for backwashing, titanium oxide sol and polypropylene are added into the membrane slurry, so that the strength of the ceramic membrane plate can be improved, the membrane flux of the filtering membrane layer of the ceramic membrane plate can be improved, the filtering membrane layer has a self-cleaning function, the membrane hole blocking is reduced, and the membrane pollution is reduced.
The titanium oxide sol is prepared by a gel method in the prior art or purchased in a chemical industry market.
The Suzhou clay is medium-low temperature hydrothermal alteration residual kaolin, is produced in Yangshan area of Suzhou of Jiangsu of China, is white in appearance, fine and smooth in texture, has the whiteness of more than 90% after burning, mainly comprises tubular halloysite and platy kaolinite, the content of alumina is 37-39%, the content of silicon dioxide is 46-48%, the refractoriness is 1730 ℃, and the plasticity is low. The oleic acid is vegetable oleic acid, such as linolenic acid, coconut oil acid, palmitoleic acid, etc.
The inorganic ceramic membrane filter plate has a membrane layer thickness of 50-60 μm, a membrane pore diameter of 0.01-0.08 μm, a porosity of 50-70%, a filtration tolerance pressure of 0.5-1MPa, a backwashing pressure of 0.3-0.5MPa, and a membrane flux of 80-100l/m2H, the retention rate is more than 85 percent, the recovery rate of membrane flux is 80-90 percent, and the plate bearing load (the thickness is 10-15mm) is 1500-2。
The high-efficiency inorganic membrane filter plate is widely used for the water removal treatment of industrial waste such as chemical industry, food, medicine, fertilizer, metallurgy, papermaking, printing and dyeing and the like, and has the advantages of high filtering efficiency, strong dirt interception capability, good effluent quality, long service life and low operation cost.
Detailed Description
Example 1, the manufacturing method of the water treatment high-efficiency inorganic membrane filter plate of the invention comprises the following steps:
a. 60-80 meshes of 55wt% of corundum, 21.5wt% of Suzhou soil and 8wt% of α -Al2O3The raw materials of 4wt% of titanium aluminum carbide, 1wt% of feldspar, 7.5wt% of methyl cellulose, 0.5wt% of dextrin, 0.5wt% of lepidolite, 0.5wt% of bentonite, 0.5wt% of talcum powder and 1wt% of oleic acid are firstly mixed according to the proportion2O3The Suzhou soil, the feldspar, the dextrin, the lepidolite, the bentonite, the talcum powder and the oleic acid are put into a stirrer to be stirred for 15 minutes, and then the prepared methyl cellulose is put into the stirrer to be stirred to prepare a mixture;
b. putting the mixture into a closed space for ageing for 20 hours, putting the aged mixture into a hydraulic press for pressing into a plate-shaped green body, and naturally drying the plate-shaped green body for 1 day;
c. drying and shaping the naturally dried plate-shaped blank in a dryer at the drying temperature of 45-60 ℃, cooling to normal temperature, spraying a layer of zeolite slurry film on the surface of the plate,
d. c, placing the plate-shaped blank body in the step c into a shuttle kiln, preserving heat for 3.5 hours at 1400 ℃, performing primary sintering, cooling along with the furnace, and discharging to obtain a high-efficiency inorganic membrane filter plate carrier;
e. putting 200 meshes of corundum sand 70wt%, suzhou soil 10wt%, feldspar 0.2wt%, titanium oxide sol 8wt%, fiber 8wt%, talcum powder 0.2wt%, bentonite 0.2wt%, dextrin 0.4wt%, lepidolite 0.4wt%, sodium humate 0.02wt%, dolomite 0.02wt%, glass water 0.1wt%, soda 0.02wt%, defoaming agent 0.3wt%, polypropylene 0.2wt% and water in a ball mill for ball milling, and filtering to prepare film-forming slurry;
f. coating the high-efficiency inorganic membrane filter plate carrier block by using a soft brush, and naturally drying the coated filter plate for 2-3 days at normal temperature;
g. placing the coated material and the dried filter plate into a shuttle kiln for secondary sintering at 1450 ℃ and keeping the temperature for 4 hours;
h. assembling: and sealing the external thread connector and the reserved holes of the high-efficiency inorganic membrane filter plates by using glue, inspecting each high-efficiency inorganic membrane filter plate, and packaging and warehousing after the high-efficiency inorganic membrane filter plates are qualified.
The inorganic membrane filter plate prepared in example 1 has a membrane layer thickness of 50-60 μm, a membrane pore diameter of 0.02-0.05 μm, a porosity of 60.5%, a filtration tolerance pressure of 0.5-0.8MPa, a backwash pressure of 0.45MPa, and a membrane flux of 88.5l/m2H, the rejection rate is 89%, the membrane flux recovery rate is 88%, and the plate bearing load (thickness 10mm) is 1680Kg/m2。
Example 2, the manufacturing method of the water treatment high-efficiency inorganic membrane filter plate of the invention comprises the following steps:
a. 60-80 meshes, 52wt% of corundum, 26wt% of Suzhou soil and 6wt% of α -Al2O33.5wt% of titanium aluminum carbide, 0.8wt% of feldspar, 8.4wt% of methyl cellulose, 1wt% of dextrin, 0.7wt% of lepidolite, 0.8wt% of bentonite, 0.3wt% of talcum powder and 0.5wt% of oleic acid, wherein corundum, titanium aluminum carbide and α -Al are mixed according to the proportion2O3The Suzhou soil, the feldspar, the dextrin, the lepidolite, the bentonite, the talcum powder and the oleic acid are put into a stirrer to be stirred for 15 minutes, and then the prepared methyl cellulose is put into the stirrer to be stirred to prepare a mixture;
b. putting the mixture into a closed space for ageing for 20 hours, putting the aged mixture into a hydraulic press for pressing into a plate-shaped green body, and naturally drying the plate-shaped green body for 1 day;
c. drying and shaping the naturally dried plate-shaped blank in a dryer at the drying temperature of 45-60 ℃, cooling to normal temperature, spraying a layer of zeolite slurry film on the surface of the plate,
d. c, placing the plate-shaped blank body in the step c into a shuttle kiln, preserving heat for 3.5 hours at 1400 ℃, performing primary sintering, cooling along with the furnace, and discharging to obtain a high-efficiency inorganic membrane filter plate carrier;
e. putting 200 meshes of 65wt% corundum sand, 12wt% Suzhou soil, 0.3wt% feldspar, 8wt% titanium oxide sol, 8wt% fiber, 0.2wt% talcum powder, 0.2wt% bentonite, 0.4wt% dextrin, 0.4wt% lepidolite, 0.02wt% sodium humate, 0.02wt% dolomite, 0.1wt% glass water, 0.02wt% soda ash, 0.3% defoamer, 0.2wt% polypropylene and the balance of water into a ball mill for ball milling, and filtering to prepare film-forming slurry;
f. coating the high-efficiency inorganic membrane filter plate carrier by using a soft brush for the membrane slurry, and naturally drying the coated filter plate for 2-3 days at normal temperature;
g. placing the coated membrane material and the dried filter plate into a shuttle kiln for secondary sintering, wherein the sintering temperature is 1450 ℃, and the temperature is kept for 4 hours;
h. assembling: and sealing the external thread connector and the reserved holes of the high-efficiency inorganic membrane filter plates by using glue, inspecting each high-efficiency inorganic membrane filter plate, and packaging and warehousing after the high-efficiency inorganic membrane filter plates are qualified.
The inorganic membrane filter plate prepared in example 2 has a membrane layer thickness of 50-60 μm, a membrane pore size of 0.02-0.05 μm, a porosity of 63.5%, a filtration tolerance pressure of 0.5-0.8MPa, a backwash pressure of 0.45MPa, and a membrane flux of 90.1l/m2H, retention rate 88.7%, recovery rate of membrane flux 89.5%, plate bearing load (thickness 10mm) 1785Kg/m2。
Claims (2)
1. A manufacturing method of a water treatment high-efficiency inorganic membrane filter plate comprises the following steps: the method is characterized in that: the method comprises the following steps:
a. 60-80 meshes, 50-60wt% of corundum sand and 20-30wt% of corundum sandSuzhou earth, 5-10wt% α -Al2O3The raw materials of 3-5wt% of titanium aluminum carbide, 0.5-1wt% of feldspar, 5.2-10.5wt% of methyl cellulose, 0.5-1wt% of dextrin, 0.3-0.8wt% of lepidolite, 0.3-1wt% of bentonite, 0.3-1wt% of talcum powder and 0.5-1wt% of oleic acid are firstly mixed according to the proportion2O3The Suzhou soil, the feldspar, the dextrin, the lepidolite, the bentonite, the talcum powder and the oleic acid are put into a stirrer to be stirred for 15 minutes, and then the methyl cellulose which is well proportioned is put into the stirrer to be stirred to prepare a mixture;
b. putting the mixture into a closed space for ageing for 15-20 hours, putting the aged mixture into a hydraulic press for pressing into a plate-shaped green body, and naturally drying the plate-shaped green body for 1-2 days;
c. drying and shaping the naturally dried plate-shaped blank in a dryer at the drying temperature of 30-60 ℃, cooling to normal temperature, spraying a layer of zeolite slurry film on the surface of the plate,
d. c, placing the plate-shaped blank in the step c into a shuttle kiln, preserving heat for 3-5 hours at 1300-1500 ℃, performing primary sintering, cooling along with the furnace, and discharging to obtain a high-efficiency inorganic membrane filter plate carrier;
e. putting 200-mesh 300-mesh corundum sand 60-80wt%, Suzhou soil 5-15wt%, feldspar 0.1-0.3wt%, titania sol 5-10wt%, fiber 5-10wt%, talcum powder 0.1-0.3wt%, bentonite 0.1-0.3wt%, dextrin 0.3-0.5wt%, lepidolite 0.3-0.5wt%, sodium humate 0.01-0.03wt%, dolomite 0.01-0.03wt%, glass water 0.05-0.15wt%, soda 0.01-0.03wt%, defoaming agent 0.2-0.3wt%, polypropylene 0.1-0.3wt% and water in a ball mill for ball milling, filtering and preparing film-forming slurry;
f. coating the high-efficiency inorganic membrane filter plate carriers block by using a soft brush, and naturally drying the coated filter plates for 2-3 days at normal temperature;
g. placing the filter plate coated with the membrane material and dried into a shuttle kiln for secondary sintering at the sintering temperature of 1400 ℃ and 1550 ℃ and keeping the temperature for 3-5 h;
h. assembling: and sealing the external thread connector and the reserved holes of the high-efficiency inorganic membrane filter plates by using glue, inspecting each high-efficiency inorganic membrane filter plate, and packaging and warehousing after the high-efficiency inorganic membrane filter plates are qualified.
2. The manufacturing method of the water treatment high-efficiency inorganic membrane filter plate according to claim 1: the method is characterized in that: the oleic acid is vegetable oleic acid, and the vegetable oleic acid is linolenic acid, coco oleic acid or palmitoleic acid.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003078672A1 (en) * | 2002-03-13 | 2003-09-25 | Ceramem Corporation | Reaction bonded alumina filter and membrane support |
| CN1843629A (en) * | 2006-04-18 | 2006-10-11 | 天津大学 | Method for preparing catalyst with micron-grade zeolite molecular sieve coated on carrier |
| CN101970717A (en) * | 2008-03-12 | 2011-02-09 | 钴碳化钨硬质合金公司 | Body coated with hard material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003078672A1 (en) * | 2002-03-13 | 2003-09-25 | Ceramem Corporation | Reaction bonded alumina filter and membrane support |
| CN1843629A (en) * | 2006-04-18 | 2006-10-11 | 天津大学 | Method for preparing catalyst with micron-grade zeolite molecular sieve coated on carrier |
| CN101970717A (en) * | 2008-03-12 | 2011-02-09 | 钴碳化钨硬质合金公司 | Body coated with hard material |
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