CN110559876B - Novel ceramic membrane - Google Patents
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- CN110559876B CN110559876B CN201910897313.4A CN201910897313A CN110559876B CN 110559876 B CN110559876 B CN 110559876B CN 201910897313 A CN201910897313 A CN 201910897313A CN 110559876 B CN110559876 B CN 110559876B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
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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
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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
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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
- 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
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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
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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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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/04—Backflushing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/16—Use of chemical agents
- B01D2321/168—Use of other chemical agents
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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
- B01D2325/24—Mechanical properties, e.g. strength
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention provides a novel ceramic membrane which is of a multilayer structure and comprises a supporting layer, wherein a transition layer and a membrane separation layer are sequentially loaded on the supporting layer, the thickness of each membrane unit is in gradient distribution increasing from bottom to top, and a large-flux membrane structure is adopted, so that the filtering efficiency can be ensured, the blocking phenomenon can be reduced, and the membrane can be conveniently cleaned; the central hole is provided with a support column, and the rigidity of the membrane is enhanced.
Description
Technical Field
The invention relates to the field of ceramic membranes, in particular to a novel ceramic membrane.
Background
In order to meet the technical challenges brought by the health risks of drinking water quality, the membrane separation technology has gradually become a hot spot of research in the field of drinking water treatment, the membrane technology currently widely researched and applied in drinking water treatment is mainly based on an organic membrane, and although the preparation cost is relatively low, the membrane technology has limitations such as poor corrosion resistance, poor oxidation resistance, difficult cleaning, low mechanical strength, short service life and the like, and the above disadvantages severely limit the potential application value of the organic membrane for treating sewage in harsh conditions.
Ceramic membranes have significant material performance advantages over organic membranes. The ceramic membrane filtration system is a precise super filtration and purification device which can be widely applied to various fields. The ceramic membrane of the core component has excellent thermal stability and pore stability, high strength, chemical corrosion resistance and good cleaning and regenerating performance, and has the double advantages of efficient filtration and precise filtration.
The ceramic membrane can be used for treating various domestic water and process water, purifying industrial wastewater (coking water, turbid circulating water and the like), is suitable for oil-containing wastewater treatment in production and industry, industrial water treatment in the water treatment industry, industrial circulating cooling water purification and high-purity process water purification, pre-filtration before production water treatment, ultrafiltration, reverse osmosis, electrodialysis and ion exchange resin, reclaimed water recycling treatment, equipment refrigeration, cooling circulating water filtration, industrial wastewater filtration and purification, and precise filtration of river water, well water, lake water and the like, but the ceramic membranes sold in the market at present have different defects of high cost, easy blockage and the like.
In order to solve the above technical problems, the present invention provides a novel ceramic film.
Disclosure of Invention
In order to solve the technical problems and improve the sewage treatment effect, the invention provides a novel ceramic membrane.
The invention is realized by the following technical scheme:
the invention provides a novel ceramic membrane which is of a multilayer structure and comprises a supporting layer, wherein a transition layer and a membrane separation layer are sequentially loaded on the supporting layer.
Further, the supporting layer is a special-shaped filter hole ceramic membrane.
Furthermore, the main structure of the special-shaped filter hole ceramic membrane is a multi-hole similar circular support structure, the number of the holes can be 5-9, preferably 7, the holes are numbered from top to bottom by 1-7, wherein the number 1,2,6 and 7 holes are non-barrier holes, the inner diameter of the highest position of each hole is 1mm, and a support structure is arranged on every two similar circular hole structures on the number 3,4 and 5 holes.
Furthermore, the special-shaped filter hole ceramic membrane contains a novel chain compound with the structural formula shown in the specification
Further, the preparation method of the special-shaped filter hole ceramic membrane comprises the following steps:
step one, Ca (OH) with the molar ratio of 1.672And H and3PO4mixing well, preparing HAP powder by wet chemical precipitation method, maintaining reaction environment at pH11-12 during synthesis, then oven drying the synthesized HAP at 80 ℃ and calcining at 800 ℃, then powdering and storing HAP for further use;
step two, preparing the novel chain compound. Specifically, 3.25mL, 31mmol, 6 equivalents of thionyl chloride was added to 60mL of 1, 2-propanediol, and the reaction was carried out at 0 ℃ for 20 minutes; 20mmol of L-Gln was added to the mixture, and the mixture was left at room temperatureStirring for 178 hours in a magnetic stirrer, taking the product, performing thin layer chromatography, and verifying that the amino acid is completely absorbed to obtain a novel chain compound with the structural formula as
Dispersing the HAP powder prepared in the step one in water by using Dolapix, then adding polyethylene glycol and hydroxyethyl cellulose, stirring the solution until no bubbles exist to obtain a solution one, mixing the solution one with the novel chain compound with the same volume, drying the mixture to be in a powder state, air-drying the powder overnight, and sintering the powder, the clay, the alumina, the pore-forming agent and the deflocculant at a heating rate of 3 ℃/min at a mass ratio of 65:20:12:3:1 at 650 ℃ to obtain the special-shaped filter pore ceramic membrane;
washing the special-shaped filter hole ceramic membrane by using boiling water, washing the special-shaped filter hole ceramic membrane by using acetone, carrying out ultrasonic treatment, removing oily and granular substances from the pore channel, and finally drying and blowing the special-shaped filter hole ceramic membrane to remove dust particles.
Further, the preparation method of the novel ceramic membrane comprises the steps of extending hydroxyethyl cellulose and graphene oxide fibers with equal mass ratio along the inner wall of the special-shaped filter hole ceramic membrane after polyacrylamide is crosslinked and solidified, placing the special-shaped filter hole ceramic membrane in an electric arc furnace for sintering, gradually heating to 880 plus materials and 900 ℃, firing for 1.5 hours, then heating to 920 plus materials and 1120 ℃, firing for 0.5 hours, finally cooling to 850-870 ℃, preserving heat for 2 hours, and cooling to obtain a secondary special-shaped filter hole ceramic membrane; the membrane separation layer is coated with nano silver ions (purchased from Dalian and Jian science and technology development Co., Ltd.), the nano silver ions are solidified on the transition layer through polyacrylamide crosslinking, and the temperature is kept for 3h at 120 ℃ to form the filter layer.
The invention has the following beneficial effects: the invention discloses a ceramic membrane sintered in a layered manner, wherein the thickness of each membrane unit is in gradient distribution increasing from bottom to top, a membrane structure with large flux is adopted, the filtration efficiency can be ensured, the blocking phenomenon can be reduced, and the membrane can be conveniently cleaned; the support column is arranged in the central hole, and the rigidity of the membrane is enhanced; the preparation method is simple and convenient, and the success rate of sintering is improved by adopting a layered sintering method.
Drawings
Fig. 1 is a schematic cross-sectional view of the novel ceramic membrane of the present invention.
Fig. 2 is a schematic diagram of the layered structure of the novel ceramic membrane according to the present invention, wherein 111-support layer, 112-transition layer, and 113-separation layer.
Fig. 3 shows a ceramic membrane filter according to the present invention, wherein 1-a ceramic membrane body, 2-a first detachable connector, 3-a second detachable connector, 11-a novel ceramic membrane, 12-a first sealing ring, 13-a second sealing ring, 14-a cleaning port, 21-a third sealing ring, 22-a water outlet, 31-a third sealing ring, and 32-a water outlet.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings.
Example 1:
materials: hydroxyethyl cellulose (from Sigma, viscosity 80-125cp), acetone (from Sigma, concentration 99.5%), polyethylene glycol (from Merck, Mw-285-.
Step one, Ca (OH) with the molar ratio of 1.672And H and3PO4mixing well, preparing HAP powder by wet chemical precipitation method, maintaining the reaction environment at pH11-12 during synthesis, then oven drying the synthesized HAP at 80 ℃ and calcining at 800 ℃, after which the HAP is powdered and stored for further use.
Step two, preparing the novel chain compound. Specifically, 3.25mL, 31mmol, 6 equivalents of thionyl chloride was added to 60mL of 1, 2-propanediol, and the reaction was carried out at 0 ℃ for 20 minutes; adding 20mmol L-Gln into the mixture, stirring in a magnetic stirrer at room temperature for 178 hours, taking the product, performing thin layer chromatography, and verifying that the amino acid is completely absorbed to obtain the new amino acidA chain type compound with the structural formula
And step three, dispersing the HAP powder (4 wt%) prepared in the step one in water (33 wt%) by using Dolapix (1.5 wt%), adding polyethylene glycol (5 wt%) and hydroxyethyl cellulose (5 wt%), stirring the solution until no bubbles exist to obtain a solution one, mixing the solution one with the novel chain compound with the same volume, drying the solution one to be in a powder state, air-drying the powder overnight, and sintering the powder with clay, alumina, a pore-forming agent and an anti-flocculating agent at a heating rate of 3 ℃/min at a heating rate of 650 ℃ according to a mass ratio of 65:20:12:3:1 to obtain the special-shaped filter pore ceramic membrane.
Washing the special-shaped filter hole ceramic membrane by using boiling water, washing the special-shaped filter hole ceramic membrane by using acetone, carrying out ultrasonic treatment, removing oily and granular substances from the pore channel, and finally drying and blowing the special-shaped filter hole ceramic membrane to remove dust particles.
The special-shaped filter hole ceramic membrane is shown in figure 1, the main structure of the special-shaped filter hole ceramic membrane is a multi-pore-channel circular-like support structure, the number of pore channels can be 5-9, preferably 7, the number of the pore channels is 1-7 from top to bottom, wherein the number 1,2,6 and 7 pore channels are non-barrier pore channels, the inner diameter of the highest position of each pore channel is 1mm, and a support structure is arranged on every two circular-like hole structures on the number 3,4 and 5 pore channels.
Example 2:
taking the special-shaped filter hole ceramic membrane as a basic structure for further preparation, as shown in fig. 3, taking the special-shaped filter hole ceramic membrane as a supporting layer, and loading a transition layer and a membrane separation layer on the supporting layer, specifically, extending hydroxyethyl cellulose and graphene oxide fibers with equal mass ratio along the inner wall of the special-shaped filter hole ceramic membrane after polyacrylamide crosslinking and curing, placing the special-shaped filter hole ceramic membrane in an electric arc furnace for sintering, gradually heating to 880-900 ℃, firing for 1.5h, then heating to 920-1120 ℃, firing for 0.5h, finally cooling to 850-870 ℃, preserving heat for 2h, and cooling to obtain a secondary special-shaped filter hole ceramic membrane; the membrane separation layer is coated with nano silver ions (purchased from Dalian and Jian science and technology development Co., Ltd.), the nano silver ions are solidified on the transition layer through polyacrylamide crosslinking, and the temperature is kept at 120 ℃ for 3 hours to obtain the novel ceramic membrane.
Example 3:
in order to realize the replaceable performance of the ceramic membrane and the seamless butt joint with other purification elements, the invention also provides a ceramic membrane filter, the structure of which is shown in fig. 3, and the ceramic membrane filter comprises a ceramic membrane body 1, a first detachable connector 2 and a second detachable connector 3, wherein the ceramic membrane body 1 comprises a novel ceramic membrane 11, a first sealing ring 12, a second sealing ring 13 and a cleaning opening 14, the first detachable connector 2 comprises a third sealing ring 21 and a water outlet 22, and the second detachable connector 3 comprises a third sealing ring 31 and a water outlet 32. Ceramic membrane body 1, first detachable joint 2, the detachable joint of second 3 adopt conventional mode to connect, including but not limited to threaded connection, splined connection, interference connection, riveting.
The ceramic membrane filter prepared by the embodiment is used for carrying out a chemical wastewater bench test, and the printing and dyeing wastewater with the flux of 2.0kg per hour is filtered; after the ceramic membrane filter is used for 20 minutes, COD of inlet and outlet water is measured, and the result shows that the removal rate of organic matters of the ceramic membrane filter can reach 97.88 percent, the salt content of raw water is 4.98 percent, and the outlet water can be reduced to 0.23 percent. After filtering for 7 days, backwashing the ceramic membrane by using inorganic salt and alcohol solution with equal proportion, recovering the primary color of the ceramic membrane after washing for 30m, and detecting to show that the surface has no organic matter residue basically, which shows that the ceramic membrane has strong self-cleaning function, the ceramic membrane filter provided by the invention has higher filtering precision (the filtering precision can reach 10 nanometers at most) and filtering speed, good cleaning and regenerating performance, is suitable for precise filtering of various media, the surface of the ceramic membrane is nontoxic, tasteless, has good antimicrobial erosion capability, the oil removal rate reaches 95.12-97.88%, and the removal rate of suspended matters with the particle size larger than 0.5 mu m reaches more than 99%.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of the appended claims.
Claims (2)
1. The utility model provides a novel ceramic membrane, its characterized in that, the ceramic membrane is multilayer structure, the ceramic membrane includes the supporting layer, has transition layer and membrane separation layer to load in proper order on the supporting layer, the supporting layer is heterotypic filtration pore ceramic membrane, heterotypic filtration pore ceramic membrane major structure is the circular bearing structure of porous class, and the pore quantity is 7, pore top-down serial number 1-7, wherein 1,2,6, No. 7 pore are for not having the hindrance pore, and every pore highest department internal diameter is 1mm, and 3,4,5 pore are provided with a bearing structure every two kinds of circular pore structures, the preparation method of heterotypic filtration pore ceramic membrane does:
step one, Ca (OH) with the molar ratio of 1.672And H and3PO4mixing well, preparing HAP powder by wet chemical precipitation method, maintaining reaction environment at pH11-12 during synthesis, then oven drying the synthesized HAP at 80 ℃ and calcining at 800 ℃, then powdering and storing HAP for further use;
step two, preparing a chain compound, specifically, adding 3.25mL of 31mmol of 6 equivalent of thionyl chloride into 60mL of 1, 2-propylene glycol, and reacting for 20 minutes at 0 ℃; adding 20mmol L-Gln into the mixture, stirring in a magnetic stirrer at room temperature for 178 hr, collecting the product, performing thin layer chromatography, and verifying that the amino acid is completely absorbed to obtain a chain compound with a structural formula of
Dispersing the HAP powder prepared in the step one in water by using Dolapix, then adding polyethylene glycol and hydroxyethyl cellulose, stirring the solution until no bubbles exist to obtain a solution one, mixing the solution one with a chain compound with the same volume, drying the mixture to be in a powder state, air-drying the powder overnight, and sintering the powder, the clay, the alumina, the pore-forming agent and the deflocculant at a heating rate of 3 ℃/min at a mass ratio of 65:20:12:3:1 at 650 ℃ to obtain the special-shaped filter pore ceramic membrane;
washing the special-shaped filter hole ceramic membrane by using boiling water, washing the special-shaped filter hole ceramic membrane by using acetone, carrying out ultrasonic treatment, removing oily and granular substances from the pore channel, and finally drying and blowing the special-shaped filter hole ceramic membrane to remove dust particles.
2. The ceramic membrane of claim 1, wherein the novel ceramic membrane is prepared by extending hydroxyethyl cellulose and graphene oxide fibers with equal mass ratio along the inner wall of the special-shaped filter hole ceramic membrane after cross-linking and curing polyacrylamide, placing the special-shaped filter hole ceramic membrane in an electric arc furnace for sintering, gradually heating to 880-900 ℃, firing for 1.5h, then heating to 920-1120 ℃, firing for 0.5h, finally cooling to 850-870 ℃, preserving heat for 2h, and cooling to obtain a secondary special-shaped filter hole ceramic membrane; the membrane separation layer is coated with nano silver ions, the nano silver ions are solidified on the transition layer through polyacrylamide crosslinking, and the temperature is kept at 120 ℃ for 3 hours to form a filter layer.
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| JP7004042B1 (en) * | 2020-08-21 | 2022-02-10 | 株式会社明電舎 | Ceramic flat membrane |
| CN114452834B (en) * | 2022-01-18 | 2023-11-03 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane |
| CN114452830B (en) * | 2022-01-18 | 2023-11-03 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane and one-step forming method thereof |
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| US4880772A (en) * | 1988-06-09 | 1989-11-14 | Battelle Memorial Institute | Preparation of thin ceramic films via an aqueous solution route |
| EP1595551B1 (en) * | 2000-08-22 | 2009-11-18 | GFE Patent A/S | Concept for slurry separation and biogas production. |
| CN106747346B (en) * | 2016-11-15 | 2019-06-21 | 中国科学院过程工程研究所 | A kind of porous ceramic film and preparation method |
| CN107663088B (en) * | 2017-08-03 | 2020-11-10 | 浙江理工大学 | Preparation method of low-temperature sintered acid-alkali-resistant porous silicon carbide ceramic membrane |
| CN108329033A (en) * | 2018-01-26 | 2018-07-27 | 山东理工大学 | Liquid-phase sintering multichannel silicon carbide ceramics membrane component and preparation method thereof |
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Effective date of registration: 20210811 Address after: 317527 Room 101, building 2, Wenling science and technology business incubator, Wenqiao Town, Wenling City, Taizhou City, Zhejiang Province Applicant after: Zhejiang Kyocera precision tools Co.,Ltd. Address before: 310004 No. 155 Dongxin Road, Xiacheng District, Hangzhou City, Zhejiang Province Applicant before: Zhang Junjie |
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Denomination of invention: A new type of Ceramic membrane Effective date of registration: 20230608 Granted publication date: 20210827 Pledgee: Zhejiang Wenling Rural Commercial Bank Co.,Ltd. Pledgor: Zhejiang Kyocera precision tools Co.,Ltd. Registration number: Y2023980043231 |