CN110559872B - Preparation method of shaft disc type rotating ceramic membrane - Google Patents
Preparation method of shaft disc type rotating ceramic membrane Download PDFInfo
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 13
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- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims description 6
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 6
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- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 claims description 5
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- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 5
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- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
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- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 4
- RFRMMZAKBNXNHE-UHFFFAOYSA-N 6-[4,6-dihydroxy-5-(2-hydroxyethoxy)-2-(hydroxymethyl)oxan-3-yl]oxy-2-(hydroxymethyl)-5-(2-hydroxypropoxy)oxane-3,4-diol Chemical compound CC(O)COC1C(O)C(O)C(CO)OC1OC1C(O)C(OCCO)C(O)OC1CO RFRMMZAKBNXNHE-UHFFFAOYSA-N 0.000 claims description 3
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- 230000032683 aging Effects 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
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- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 claims description 2
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
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- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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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
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0041—Inorganic membrane manufacture by agglomeration of particles in the dry state
-
- 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
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0076—Pretreatment of inorganic membrane material prior to membrane formation, e.g. coating of metal powder
-
- 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
-
- 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
- B01D69/10—Supported membranes; Membrane supports
- B01D69/105—Support pretreatment
-
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to the technical field of porous ceramic materials and membrane separation, in particular to a preparation method of a shaft disc type rotating ceramic membrane. The method is mainly characterized in that a microsphere ceramic raw material is used as aggregate of a support body, ceramic fiber is used as a transition layer, beta-silicon carbide is used as a film layer, and the shaft disc type rotating ceramic film is formed by pressing and firing through a hydraulic press and a low-temperature liquid phase method. The preparation method has the characteristics of low sintering temperature, low production energy consumption, simple process method, low equipment requirement, low production cost and investment cost, flexible control, easy molding, suitability for industrial customization and capability of meeting large-scale production. The shaft disc type rotating ceramic membrane prepared by the method has the characteristics of good hydrophilicity, large permeation flux, high porosity, high yield, no need of arranging a diversion trench, good acid and alkali resistance and long service life.
Description
Technical Field
The invention relates to the technical field of inorganic porous materials, in particular to the technical field of inorganic membrane separation materials, and specifically relates to a preparation method of a shaft disc type rotating ceramic membrane.
Background
Compared with the traditional polymer separation membrane material, the ceramic membrane has the advantages of good chemical stability, acid and alkali resistance, organic solvent resistance, high mechanical strength, back flushing capability, strong antimicrobial capability, high temperature resistance, narrow pore size distribution, high separation efficiency and the like, and is widely applied to the fields of food industry, bioengineering, environmental engineering, chemical industry, petrochemical industry, metallurgical industry and the like.
However, the ceramic membrane also has the problem of membrane pollution, which causes a series of disadvantages of low membrane permeation flux, frequent membrane cleaning, high operation cost and the like. In order to alleviate the tendency of fouling of the ceramic membrane, the multichannel tubular ceramic membrane usually adopts a cross-flow filtration mode, and utilizes the shearing force generated by high-speed fluid on the surface of the membrane to eliminate the problem of membrane fouling caused by concentration polarization or a filter cake layer. The operation mode can indeed slow down the reduction of the permeation flux of the membrane and ensure the stable operation of the separation efficiency of the membrane. However, the large membrane surface flow rate needs a large-flow water pump for driving, the energy consumption is high, and the operation cost is high. The flat-plate ceramic membrane generally adopts an immersion dead-end filtration mode, utilizes the suction force generated by a negative pressure pump as the mass transfer power of membrane filtration, and needs to be matched with bubbles generated by the aeration of a blower to wash the surface of the membrane so as to slow down the membrane pollution caused by concentration polarization or a filter cake layer. The filtering mode negative pressure pump has relatively low energy consumption, but the filtering efficiency of the separating membrane is not fully utilized, the energy consumption of the aeration fan is higher, the filling density of the membrane is high, and the investment cost is high.
A shaft disc type rotary ceramic membrane filtering technology adopts shearing force generated when a membrane rotates to slow down concentration polarization or filter cake layers and other pollutants on the surface of the membrane, and adopts a negative pressure suction filtering mode to reduce the energy consumption of membrane filtration and prolong the time of membrane fouling and blocking. The membrane separation technology has the advantages of the two operation modes, avoids the defects, is a brand new filtration mode for thoroughly excavating the filtration potential of the ceramic membrane, and has the advantages of high concentration multiple, low energy consumption, low investment cost, low operation cost and the like. Both patents CN106512751A and CN208694725U disclose and report the preparation method of the multi-channel or multi-channel disk-shaped rotatable ceramic membrane. These patents clearly report that the disc-type ceramic membrane cake is provided with straight or curved water guiding grooves in the middle, which reduces the permeation resistance of the membrane and facilitates the circulation of membrane permeate. However, the design of forming the diversion trench in the middle of the membrane cake greatly increases the difficulty, complexity and cost of the membrane manufacturing process, and leads to extremely low qualification rate of membrane products. Because the process needs two types of moulds, particularly the mould with the diversion trench has high difficulty in demoulding, two biscuit blanks with different thicknesses need to be buckled into a complete round cake, and the buckling part needs to be bonded by high-temperature bonding agent, the nonstandard products are easy to generate, or the leakage risk exists. In addition, the disc-type ceramic membrane is generally prepared by adopting mechanically ground powder, the porous ceramic formed by piling the powder with different specifications has low porosity, the penetration resistance of the support body is large, and the water flux is low.
Disclosure of Invention
The invention aims to solve the problems of complex ceramic membrane manufacturing process, high manufacturing cost and investment cost, high operation energy consumption and operation cost and the like; and the problems of high manufacturing difficulty, low yield, small permeation flux and the like of the disc type ceramic membrane. The manufacturing method has the advantages of simple manufacturing process, low manufacturing cost and investment cost, low sintering temperature, high yield, large permeation flux, flexible control, easy molding, suitability for industrial customization and large-scale production.
One problem to be solved by the present invention is: the existing ceramic membrane production raw material is irregular powder obtained by crushing, grinding and sorting ceramic block raw materials, and then is sintered at high temperature to form a porous ceramic membrane with three-dimensional pores; the ceramic membrane has low porosity, large permeation resistance and high required driving pressure when being used in the process of filtering liquid or gas, thereby generating high operation cost. The method for preparing the porous shaft disc type rotating ceramic membrane by using the silicon dioxide microspheres as the ceramic membrane sintering raw materials and sintering at the temperature of 700-1400 ℃ is provided.
Another problem to be solved by the present invention is: the existing disc type ceramic membrane cake is provided with a linear or curved diversion trench in the middle, and is pressed and formed by a double-mold process, and is bonded into an integral disc-shaped ceramic membrane at high temperature. Complex manufacturing process, high demoulding difficulty, low yield, high investment cost and the like. The method for preparing the large-size thin-wall shaft disc type rotating ceramic membrane has the advantages of simple mold structure, simple manufacturing process, one-time press molding, easy demolding, no cracking and no warping in the firing process and can be used for preparing the large-size thin-wall shaft disc type rotating ceramic membrane.
In order to solve the technical problems in the preparation process of the shaft disc type rotating ceramic membrane, the technical scheme of the invention is as follows:
the preparation method of the shaft disc type rotating ceramic membrane comprises the following raw materials of silicon dioxide microspheres, sintering aids, plasticizers, solvents and release agents, wherein: the particle size of the silicon dioxide microspheres is 1-200 mu m, and the concentration is more than 80%; the sintering aid is composed of silica sol, alumina sol, magnesium carbonate, aluminum dihydrogen phosphate and kaolin, and the sintering aid is prepared from the following components in percentage by mass (35-55 wt%): (10 wt% to 30 wt%): (10 wt% to 25 wt%): (5 wt% -20 wt%): (5 wt% -20 wt%) and the sum of the mass percentages of all the components is 100%, wherein the sintering aid is the technical core of sintering the shaft disc type rotating ceramic support body and the ceramic membrane by a low-temperature liquid phase method, and is used for forming a liquid phase at a high temperature and bonding the silicon dioxide microspheres together; the plasticizer is composed of more than one of methylcellulose, sodium carboxymethylcellulose, hydroxypropyl methylcellulose and polyvinyl alcohol, has certain viscosity after hydrolysis, mainly has the function of endowing barren materials such as silicon dioxide microspheres, sintering aids and the like with certain plasticity at normal temperature, and can be pressed and formed by a press; the solvent is composed of one or more of water, ethanol or mixture of water and ethanol, and is used for hydrolyzing the plasticizer to make it have certain viscosity, and pressing the barren material and sintering aid into round cake shape under the action of press. The release agent is composed of more than one of oleic acid, tung oil, aluminum stearate and graphite, and has the functions of lubrication, convenient separation of a formed round cake and a mould groove and guarantee of forming of a complete biscuit with a flawless round cake shape;
through the combination of the raw materials and the cooperation of a reasonable drying and firing system, the axial disc type rotating ceramic membrane with simple manufacturing process, high porosity and ultra-large permeation flux can be obtained, and the preparation method comprises the following steps:
(1) support preparation
The preparation method comprises the following steps of (1) taking 85 wt% of silicon dioxide microspheres with the particle size range of 1-200 mu m, sintering aid, plasticizer, solvent and release agent according to the mass percentage: (25 wt% to 5 wt%): (1 wt% -5 wt%) (5 wt% -20 wt%): (0.5 wt% -8 wt%) and the sum of the mass percentages of all the components except the solvent and the release agent is 100%; after the silicon dioxide microspheres, the sintering aid and the plastic agent are dry-mixed in a strong mixer for 5-30 min, slowly adding a solvent and a release agent on a granulator until large soybean particles are formed, sealing the wet materials with the prepared particles by using a vacuum bag, and ageing for 12-24 h at the temperature of 20-25 ℃ and the humidity of 50-80%. The mould is processed into a round cake shape with the diameter of 100-500 mm according to design requirements, a round hole with the diameter of 10-100 mm is formed in the center of the mould, and the thickness of the round cake is 3-50 mm. Installing a mould and sleeving the mould at the upper cylinder head and the lower cylinder head of a ceramic powder hydraulic forming machine, uniformly scattering a layer of graphite powder on the surface of a mould groove, adding aged particles into the mould groove, pressing into a biscuit with a shape of a round cake with a hole at the center by a hydraulic press, and transferring the biscuit onto a ceramic supporting plate by a sucking disc for drying. And transferring the ceramic supporting plate together with the biscuit subjected to press forming onto a chain plate of a continuous tunnel microwave ceramic dryer, quickly setting for 1-3 times at the speed of 0.5-5 m/min under the microwave power of 300-850W and the conveyer belt speed, transferring into a hot air resistance drying oven, and drying at the temperature of 100-300 ℃ for 1-12 hours. And transferring the dried biscuit into a high-temperature resistance kiln, a gas shuttle kiln or a tunnel kiln, and sintering at high temperature in an air atmosphere. The firing system is as follows: heating from room temperature to 150 ℃, wherein the heating rate is 20-50 ℃/h, keeping the temperature for 1-3 h, and performing a dehydration procedure; heating from 120 ℃ to 400 ℃, keeping the temperature for 2-4 h at the heating rate of 10-50 ℃/h, and carrying out a degumming procedure; heating from 400 ℃ to 750 ℃, wherein the heating rate is 30-50 ℃/h, and the heating process is simple; heating from 750 ℃ to 1400 ℃, wherein the heating rate is 10-30 ℃/h, preserving heat for 3-5 h, and carrying out an oxidizing firing process; and then naturally cooling to room temperature to obtain the shaft disc type rotary ceramic support.
(2) Preparation of the transition layer
Polycrystalline mullite fiber with the diameter and the length of 1-1000 mu m, a sintering aid, a binder, a dispersant and a solvent are mixed according to the mass percentage (10-1 wt%): (0.1 wt% to 1.5 wt%): (0.1 wt% to 5 wt%): (0.1 wt% to 5 wt%): (80 wt% -95 wt%) and mixing, wherein the sum of the mass percentages of the components is 100%; the sintering aid is the same as the sintering aid in the step (1); the binder is composed of more than one of methylcellulose, sodium carboxymethylcellulose, hydroxypropyl methylcellulose, hydroxyethyl cellulose and polyvinyl alcohol; the dispersant is composed of more than one of sodium stearate, polyacrylic acid, ammonium polyacrylate, polyethyleneimine and polyethylene glycol; the solvent is one or more of water, ethanol or a mixture of water and ethanol; and (2) uniformly mixing the raw materials in proportion, carrying out ball milling for 1-12 h to obtain slurry with uniform dispersion and good tape-casting property, uniformly coating the prepared slurry on the support prepared in the step (1) by adopting a spraying or dip-coating process, transferring the support to a box-type microwave dryer, and obtaining the mullite fiber-coated reel-type rotary ceramic support with the microwave power of 300-850W and the microwave time of 1-3 h.
(3) Film preparation
Mixing beta-silicon carbide powder with a medium particle size of 0.05-5 mu m with a sintering aid, a binder, a dispersant and a solvent according to the mass percentage (30-10 wt%): (1 wt% -3 wt%): (0.5 wt% to 5 wt%): (0.1 wt% to 5 wt%): (50 wt% -80 wt%) and mixing, wherein the sum of the mass percentages of the components is 100%; the sintering aid, the binder, the dispersant and the solvent are the same as those in the step (2); and (3) uniformly mixing the raw materials in proportion, performing ball milling for 1-12 hours to obtain slurry with uniform dispersion and good curtain coating property, uniformly coating the prepared slurry on the mullite fiber-coated reel-to-reel rotary ceramic support prepared in the step (2) by adopting a spraying or dip-coating process, transferring the mullite fiber-coated reel-to-reel rotary ceramic support into a box-type microwave dryer, and performing microwave drying for 1-3 hours at a microwave power of 300-850W to obtain the silicon carbide powder-coated reel-to-reel rotary ceramic support.
(4) Firing of the film
And (4) transferring the shaft disc type rotary ceramic support body coated with the silicon carbide powder prepared in the step (3) into a high-temperature resistance kiln, a gas shuttle kiln or a tunnel kiln, and sintering in an air atmosphere. The sintering system is as follows: heating from room temperature to 150 ℃, keeping the temperature for 1-3 h at the heating rate of 15-30 ℃/min, and dehydrating; heating from 150 ℃ to 400 ℃, keeping the temperature at the heating rate of 10-25 ℃/min for 1-3 h, and carrying out a degumming procedure; heating from 400 ℃ to 1300 ℃, wherein the heating rate is 20-50 ℃/min, and keeping the temperature for 1-2 h; and naturally cooling to room temperature to obtain the shaft disc type rotating ceramic membrane.
Preferably, the preparation method of the shaft disc type rotating ceramic membrane is characterized by comprising the following steps: the filter layer is prepared from polycrystalline mullite fibers with the diameter and the length of 1-1000 mu m, a sintering aid, a binder, a dispersing agent and a solvent according to the mass percentage (10-1 wt%): (0.1 wt% to 1.5 wt%): (0.1 wt% to 5 wt%): (0.1 wt% to 5 wt%): (80 wt% -95 wt%) and the sum of the mass percentages of all the components is 100%.
Preferably, the preparation method of the shaft disc type rotating ceramic membrane is characterized by comprising the following steps: the sintering aid comprises the following raw materials in percentage by mass: (10 wt% to 20 wt%): (10 wt% to 20 wt%): (5 wt% -10 wt%): (15 wt% -20 wt%) and the sum of the mass percentages of all the components is 100%.
Preferably, the preparation method of the shaft disc type rotating ceramic membrane comprises the following steps of mixing beta-silicon carbide powder with a medium particle size of 0.05-5 mu m, a sintering aid, a binder, a dispersing agent and a solvent according to mass percentage (30-20%): (2 wt% -3 wt%): (2.5 wt% -5 wt%): (2 wt% -3 wt%): (60 wt% -70 wt%) and the sum of the mass percentages of all the components is 100%.
Preferably, the preparation method of the shaft disc type rotating ceramic membrane is characterized by comprising the following steps: the transition layer and the film layer drying system is as follows: the microwave drying is carried out in a microwave dryer, the microwave power is 500-650W, and the microwave time is 2 h.
Preferably, the preparation method of the shaft disc type rotating ceramic membrane is characterized by comprising the following steps: the transition layer and the film layer are sintered according to the following schedule: heating from room temperature to 150 ℃, keeping the temperature for 2h at the heating rate of 15-30 ℃/min, and dehydrating; heating from 150 ℃ to 400 ℃, keeping the temperature for 2h at the heating rate of 10-25 ℃/min, and carrying out a degumming procedure; heating from 400 ℃ to 1300 ℃, wherein the heating rate is 20-50 ℃/min, and keeping the temperature for 1-2 h; then naturally cooling to room temperature.
Preferably, the preparation method of the shaft disc type rotating ceramic membrane is characterized by comprising the following steps: the binder is composed of more than one of methylcellulose, sodium carboxymethylcellulose, hydroxypropyl methylcellulose, hydroxyethyl cellulose and polyvinyl alcohol.
Preferably, the preparation method of the shaft disc type rotating ceramic membrane is characterized by comprising the following steps: the dispersant is composed of more than one of sodium stearate, polyacrylic acid, ammonium polyacrylate, polyethyleneimine and polyethylene glycol.
The technical scheme of the preparation method of the shaft disc type rotating ceramic membrane has the following beneficial effects:
1. the main raw material components of the shaft disc type rotating ceramic membrane are silicon dioxide microspheres, silicate sintering aids and silicon carbide coating powder, and the materials can form rich silanol bonds in an aqueous solution and can generate hydrogen bond action with water molecules, so that the hydrophilicity is good, and a shaft disc type rotating ceramic support prepared from the material has good hydrophilicity and contamination resistance.
2. The aggregate of the support body of the shaft disc type rotating ceramic membrane is very regular microspheres, and the microspheres are stacked to form a developed three-dimensional pore structure, so that the support body can realize the effect of high permeation flux without a diversion trench in the middle of a round cake.
3. The support body of the shaft disc type rotating ceramic membrane is pressed into a round cake shape at one time by a hydraulic press, a diversion trench is not required to be reserved in the middle of the round cake, and half round cakes are not required to be bonded into a whole round cake by a high-temperature bonding agent, so that the manufacturing process is simple, the yield is high, and products with large sizes and thin walls can be pressed.
4. The transition layer of the shaft disc type rotating ceramic membrane adopts disordered accumulation of polycrystalline mullite fibers, has high porosity and almost no resistance to fluid permeation, and effectively prevents fine solid particles in coating liquid of the membrane layer from blocking holes of a support body.
5. The film layer of the shaft disc type rotating ceramic film adopts the accumulation of beta-silicon carbide powder on the surface of the transition layer; the crystal form of the beta-silicon carbide is cubic phase, the particles are round and smooth, and the oxidation resistance is good; the raw material is used as a film layer and has the advantages of good hydrophilicity, good pollution resistance, acid and alkali corrosion resistance, large permeation flux and the like.
6. The shaft disc type rotating ceramic membrane is sintered by strong oxidizing flame below 1400 ℃ in air atmosphere, so that the method has the advantages of low sintering temperature, low production energy consumption, simple process method, low equipment requirement, low production cost and low investment cost.
7. The shaft disc type rotating ceramic membrane has wide application field, can be used for special separation in the industries of chemical industry, biological fermentation, papermaking, food and beverage, mineral processing and the like, can also be used for the links of tap water purification, sewage upgrading reconstruction, wastewater treatment, useful substance recovery, reclaimed water reuse and the like, and can also be applied to gas purification such as automobile exhaust purification, coal chemical crude gas filtration, high-temperature flue gas treatment and the like.
Drawings
FIG. 1 is a schematic cross-sectional view of a rotating ceramic disk.
Fig. 2 is a top view of a rotating ceramic disk.
The specific implementation mode is as follows:
the invention is further illustrated by the following examples, which are not intended to limit the scope of the present disclosure in any way.
Example 1
Mixing silica microspheres with a medium particle size of 45 mu m, hydroxypropyl methylcellulose and a sintering aid (45 wt% of silica sol, 20 wt% of aluminum sol, 15 wt% of magnesium carbonate, 10 wt% of aluminum dihydrogen phosphate and 10 wt% of kaolin) according to the mass percentage of 85: 2: 13, mixing, wherein the silicon dioxide microspheres, the hydroxypropyl methyl cellulose, the magnesium carbonate, the aluminum dihydrogen phosphate and the kaolin are firstly mixed in a powerful mixer for 15min, and then liquid silica sol and aluminum sol are added in proportion; transferring the mixed raw materials to a granulator, slowly adding water and tung oil which respectively account for 10 wt% and 4.5 wt% of the total weight of the silicon dioxide microspheres, the hydroxypropyl methylcellulose and the sintering aid until large soybean particles are formed, sealing the wet materials of the prepared particles by using a vacuum bag, and ageing for 24 hours at the temperature of 20-25 ℃ and the humidity of 50-80%; adding aged wet material particles into a groove of a mold which is scattered with a layer of graphite powder, wherein the size of the mold is a segmental annular cake with the inner diameter of 50mm, the outer diameter of 200mm and the thickness of 6mm, pressing the segmental annular cake into a spinning ceramic biscuit under a 400-ton hydraulic press, transferring the spinning ceramic biscuit onto a ceramic supporting plate by adopting a sucking disc, transferring the ceramic supporting plate and the pressed biscuit onto a chain plate of a continuous tunnel microwave ceramic dryer together, quickly setting for 2 times, transferring the ceramic supporting plate and the pressed biscuit into a hot air resistance drying box, and drying for 4 hours at the temperature of 110 ℃; transferring the dried biscuit into a natural gas shuttle kiln, sintering at high temperature in air atmosphere, and firing according to the following system: heating from room temperature to 150 ℃, keeping the temperature for 3h at the heating rate of 30 ℃/h, and dehydrating; heating from 120 ℃ to 400 ℃, keeping the temperature at the heating rate of 20 ℃/h for 3h, and carrying out a degumming procedure; heating from 400 ℃ to 750 ℃, wherein the heating rate is 50 ℃/h, and the heating process is simple; heating from 750 ℃ to 1320 ℃, wherein the heating rate is 15 ℃/h, keeping the temperature for 3h, and carrying out an oxidizing firing process; and then naturally cooling to room temperature to obtain the shaft disc type rotary ceramic support.
Polycrystalline mullite fiber with the diameter of 10 mu m and the length of 500 mu m, sintering aid (45 wt% of silica sol, 20 wt% of alumina sol, 15 wt% of magnesium carbonate, 10 wt% of aluminum dihydrogen phosphate and 10 wt% of kaolin), methyl cellulose, ammonium polyacrylate and water according to the mass percentage of 7 wt%: 1 wt%: 1 wt%: 1 wt%: mixing 90 wt%; the raw materials are uniformly mixed according to a proportion and then are subjected to ball milling for 6 hours to obtain slurry which is uniformly dispersed and has good tape-casting property, then the prepared slurry is uniformly coated on the prepared support body by adopting a spraying process, and the support body is transferred into a box-type microwave dryer, wherein the microwave power is 600W, and the microwave time is 2 hours, so that the shaft disc type rotary ceramic support body coated with the mullite fiber can be obtained.
Mixing beta-silicon carbide powder with a medium particle size of 1 mu m with a sintering aid (45 wt% of silica sol, 20 wt% of aluminum sol, 15 wt% of magnesium carbonate, 10 wt% of aluminum dihydrogen phosphate and 10 wt% of kaolin), methylcellulose, sodium stearate and water according to the mass percentage of 20 wt%: 1 wt%: 1 wt%: 0.5 wt%: 77.5 wt% mixing; the raw materials are uniformly mixed according to a proportion and then are subjected to ball milling for 10 hours to obtain slurry with uniform dispersion and good tape-casting property, then the prepared slurry is uniformly coated on a shaft disc type rotary ceramic support body coated with mullite fiber by adopting a spraying process, and the shaft disc type rotary ceramic support body coated with silicon carbide powder can be obtained by transferring the shaft disc type rotary ceramic support body to a box type microwave dryer with the microwave power of 600W and the microwave time of 2 hours.
And transferring the shaft disc type rotating ceramic support body coated with the silicon carbide powder into a natural gas shuttle kiln, and sintering in an air atmosphere. The sintering system is as follows: heating from room temperature to 150 ℃, keeping the temperature for 2h at the heating rate of 25 ℃/min, and dehydrating; heating from 150 ℃ to 400 ℃, keeping the temperature for 3h at the heating rate of 15 ℃/min, and carrying out a degumming procedure; heating from 400 ℃ to 1280 ℃, wherein the heating rate is 30 ℃/min, and keeping the temperature for 1 h; and naturally cooling to room temperature to obtain the shaft disc type rotating ceramic membrane, and performing various performance tests.
Example 2
Except that the medium particle size of the film-sprayed beta-silicon carbide powder was changed to 0.5 μm, and the other operation steps, the addition amount and the control parameters were the same as those of example 1.
Example 3
Except that the medium particle size of the film-sprayed beta-silicon carbide powder was changed to 1.5 μm, and the other operation steps, the addition amount and the control parameters were the same as those of example 1.
Example 4
Except that the medium particle size of the film-sprayed beta-silicon carbide powder was changed to 2.0. mu.m, and the other operation steps, addition amounts and control parameters were the same as those of example 1.
The performance evaluation method of the porous silicon carbide ceramic film prepared by the invention is shown in the following table 1:
table 2 porous silicon carbide ceramic film performance testing in the above examples:
the above description is only a preferred embodiment of the present invention, and should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (4)
1. A preparation method of a shaft disc type rotating ceramic membrane is characterized by comprising the following steps: the used raw materials comprise silicon dioxide microspheres, polycrystalline mullite fibers, beta-silicon carbide, sintering aids, plasticizers, solvents and release agents, wherein: the particle size of the silicon dioxide microspheres is 1-200 mu m, and the concentration is more than 80%; the sintering aid is composed of silica sol, alumina sol, magnesium carbonate, aluminum dihydrogen phosphate and kaolin, and the sintering aid is prepared from the following components in percentage by mass (35-55 wt%): (10 wt% to 30 wt%): (10 wt% to 25 wt%): (5 wt% -20 wt%): (5 wt% -20 wt%) and mixing, wherein the sum of the mass percentages of the components is 100%; the plastic agent is composed of more than one of methylcellulose, sodium carboxymethylcellulose, hydroxypropyl methylcellulose and polyvinyl alcohol; the solvent is water, ethanol or a mixture of water and ethanol; the release agent is composed of more than one of oleic acid, tung oil, aluminum stearate and graphite; the preparation method comprises the following specific steps:
(1) support preparation
The preparation method comprises the following steps of (1) taking 85 wt% of silicon dioxide microspheres with the particle size range of 1-200 mu m, sintering aid, plasticizer, solvent and release agent according to the mass percentage: 13 wt%: 2 wt%: 10 wt%: 4.5 wt% of the components except the solvent and the release agent, wherein the sum of the mass percentages of the components is 100%; carrying out the material manufacturing, drying and firing treatment; during the preparation of the support, the material is prepared by dry mixing the silicon dioxide microspheres, the sintering aid and the plasticizer in a strong mixer for 5-30 min, slowly adding a solvent and a release agent in a granulator until large soybean particles are formed, sealing the prepared wet material with a vacuum bag, and ageing at the temperature of 20-25 ℃ and the humidity of 50-80% for 12-24 h;
the support body is dried and fired in the preparation process, a round cake-shaped mold with the diameter of 100-500 mm is firstly processed, a round hole with the diameter of 10-100 mm is formed in the center of the mold, and the thickness of the round cake is 3-50 mm; mounting a mold and sleeving the mold at the upper cylinder head and the lower cylinder head of a ceramic powder hydraulic forming machine, uniformly scattering a layer of graphite powder on the surface of a mold groove, adding aged particles into the mold groove, pressing into a biscuit with a round cake shape with a hole at the center by a hydraulic press, and transferring the biscuit onto a ceramic supporting plate by a sucking disc for drying; transferring the ceramic supporting plate together with the biscuit subjected to press forming onto a chain plate of a continuous tunnel microwave ceramic dryer, quickly setting for 1-3 times at the speed of 0.5-5 m/min under the microwave power of 300-850W and the conveyer belt speed, transferring into a hot air resistance drying oven, and drying at 100-300 ℃ for 1-12 hours; transferring the dried biscuit into a high-temperature resistance kiln, a gas shuttle kiln or a tunnel kiln, and sintering at high temperature in an air atmosphere; the firing system is as follows: heating from room temperature to 150 ℃, wherein the heating rate is 20-50 ℃/h, keeping the temperature for 1-3 h, and performing a dehydration procedure; heating from 150 ℃ to 400 ℃, keeping the temperature for 2-4 h at the heating rate of 10-50 ℃/h, and carrying out a degumming procedure; heating from 400 ℃ to 750 ℃, wherein the heating rate is 30-50 ℃/h, and the heating process is simple; heating from 750 ℃ to 1400 ℃, wherein the heating rate is 10-30 ℃/h, preserving heat for 3-5 h, and carrying out an oxidizing firing process; then naturally cooling to room temperature to obtain the shaft disc type rotating ceramic support body;
(2) preparation of the transition layer
Polycrystalline mullite fiber with the diameter and the length of 1-1000 mu m, a sintering aid, a binder, a dispersant and a solvent are mixed according to the mass percentage (10-1 wt%): (0.1 wt% to 1.5 wt%): (0.1 wt% to 5 wt%): (0.1 wt% to 5 wt%): (80 wt% -95 wt%) and mixing, wherein the sum of the mass percentages of the components is 100%; the binder is composed of more than one of methylcellulose, sodium carboxymethylcellulose, hydroxypropyl methylcellulose, hydroxyethyl cellulose and polyvinyl alcohol; the dispersant is composed of more than one of sodium stearate, polyacrylic acid, ammonium polyacrylate, polyethyleneimine and polyethylene glycol; coating on the support prepared in the step (1);
(3) film preparation
Mixing beta-silicon carbide powder with a medium particle size of 0.05-5 mu m with a sintering aid, a binder, a dispersant and a solvent according to the mass percentage of 20 wt%: 1 wt%: 1 wt%: 0.5 wt%: 77.5 wt% and the sum of the mass percentages of the components is 100%; the sintering aid, the binder, the dispersant and the solvent are the same as those in the step (2); uniformly coating the slurry on the product prepared in the step (2);
(4) firing of the film
And (4) carrying out high-temperature sintering on the shaft disc type rotating ceramic support body coated with the silicon carbide powder prepared in the step (3) to obtain the shaft disc type rotating ceramic membrane.
2. The method according to claim 1, wherein the method comprises the steps of: in the preparation process of the transition layer, the mixed material liquid is uniformly mixed according to a proportion and then is subjected to ball milling for 1-12 hours to obtain slurry which is uniformly dispersed and has good tape-casting property, then the prepared slurry is uniformly coated on the support body prepared in the step (1) by adopting a spraying or dip-coating process, and the support body is transferred into a box-type microwave dryer, the microwave power is 300-850W, and the microwave time is 1-3 hours, so that the shaft disc type rotary ceramic support body coated with the mullite fiber can be obtained.
3. The method according to claim 1, wherein the method comprises the steps of: in the preparation process of the film layer, the slurry is uniformly mixed according to a proportion and then is subjected to ball milling for 1-12 hours, and the slurry which is uniformly dispersed and has good tape-casting property can be obtained; and (3) uniformly coating the prepared slurry on the shaft disc type rotary ceramic support body coated with the mullite fiber prepared in the step (2) by adopting a spraying or dip-coating process, and transferring the shaft disc type rotary ceramic support body into a box type microwave dryer, wherein the microwave power is 300-850W, and the microwave time is 1-3 h, so that the shaft disc type rotary ceramic support body coated with the silicon carbide powder can be obtained.
4. The method according to claim 1, wherein the method comprises the steps of: in the film layer firing process, transferring the product obtained in the step (3) into a high-temperature resistance kiln, a gas shuttle kiln or a tunnel kiln, and sintering in an air atmosphere; the sintering system is as follows: heating from room temperature to 150 ℃, keeping the temperature for 1-3 h at the heating rate of 15-30 ℃/min, and dehydrating; heating from 150 ℃ to 400 ℃, keeping the temperature at the heating rate of 10-25 ℃/min for 1-3 h, and carrying out a degumming procedure; heating from 400 ℃ to 1300 ℃, wherein the heating rate is 20-50 ℃/min, and keeping the temperature for 1-2 h; then naturally cooling to room temperature.
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| CN107915475A (en) * | 2017-11-02 | 2018-04-17 | 武汉理工大学 | A kind of gradient pore high temperature filtration ceramic tube and preparation method thereof |
| CN108704492A (en) * | 2018-04-27 | 2018-10-26 | 台州利欧环保新材料有限公司 | A kind of preparation method of porous silicon carbide ceramic membrane |
| CN108421414A (en) * | 2018-06-08 | 2018-08-21 | 山东铭创环境工程有限公司 | Disc type pottery membrane microfiltration device |
| CN208771220U (en) * | 2018-06-08 | 2019-04-23 | 山东铭创环境工程有限公司 | Disc type ceramic film component and its disc type ceramic membrane ultrafitration purifier |
| CN111499361A (en) * | 2020-04-26 | 2020-08-07 | 山东泰禾环保科技股份有限公司 | Preparation method of composite ceramic membrane |
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