CN106512751A - Preparation method of disc-type multi-channel plate ceramic membrane - Google Patents
Preparation method of disc-type multi-channel plate ceramic membrane Download PDFInfo
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- CN106512751A CN106512751A CN201611088839.0A CN201611088839A CN106512751A CN 106512751 A CN106512751 A CN 106512751A CN 201611088839 A CN201611088839 A CN 201611088839A CN 106512751 A CN106512751 A CN 106512751A
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Classifications
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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
- B01D69/06—Flat membranes
-
- 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
-
- 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
-
- 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
-
- 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
Abstract
The invention discloses a preparation method of a disc-type multi-channel plate ceramic membrane. A support body of the disc-type multi-channel plate ceramic membrane is in a circular plate shape, a water through hole is formed in the center of the support body, and a plurality of hole channels are formed in the support body in the radial direction, so that the flowability of a filtrate in the support body is increased; one end of each hole channel is sealed, the other end of the hole channel is communicated with the water through hole, and the plurality of hole channels are arranged on a single layer or multiple layers. The preparation method is simple, low in mold cost, basically pollution-free to the environment, non-damage to operators and high in production efficiency; the formed disc-type multi-channel plate ceramic membrane has high throughput and excellent performance, and can be used for a rotary dynamic filter ceramic membrane component.
Description
Technical field
The invention belongs to ceramic membrane technology field, and in particular to a kind of preparation side of disc type Multi-channel flat plate ceramic membrane
Method.
Background technology
Inorganic ceramic film has excellent strainability, in addition to effective crown_interception, also with high temperature resistant, resistance to molten
The advantages of agent, acid-alkali-corrosive-resisting, high mechanical properties, long-life, high separating efficiency and renewable easy cleaning, it is capable of achieving to sewage depth
Degree purification, deep phosphorous removal denitrogenation.However, the concentration polarization and fouling membrane phenomenon during ceramic membrane filter is caused under permeation flux
Drop, causes the technology play one's part to the full in the field that there is using value the poles such as chemical industry, biochemical process and food processing.
Generally in ceramic membrane filter operation, with the carrying out of filter operation, due to the selective penetrated property of film, filter membrane table
Face constantly has component to be trapped, and is trapped component and accumulates in coating materials liquid side surface, forms cake layer so that mistake in the case of pressurized
Filter membrane resistance increases, and the rate of filtration reduces, and forms concentration polarization.Concentration polarization can increase the concentration that face is trapped material, plus
The generation of fast fouling membrane, causes flux depression, transmembrane pressure to raise, and affects film to produce water efficiency and service life.
Numerous studies show that membrane module rotation can effectively mitigate fouling membrane, delay the decay of membrane flux.This is because film
Component can form shearing force on film surface when rotating, and filter membrane surface is kept than relatively thin cake layer thickness, grasp filtration
Work can keep continuous, stable filtration condition.In recent years, the technology is of increased attention, chemical industry, food,
The aspect such as pharmacy and water process achieves good application effect.
German at present, Japan, Jun You enterprises of U.S. production rotary disc-type Multi-channel flat plate ceramic membrane and its component, and all
There is the application technology of maturation, but the country can produce disc type Multi-channel flat plate ceramic membrane currently without enterprise.
Shaanxi Province modern building design academy is having prepared circle using dry pressuring forming process and solid particles sintering process
Template porous ceramic film support.But there is not collecting channel to be distributed in the middle of its circular Flat Membrane for preparing, its collection water pressure will
Greatly increase, and be not suitable for rotating dynamic filtration ceramic film component.
The content of the invention
It is an object of the invention to provide a kind of preparation method of disc type Multi-channel flat plate ceramic membrane.
Technical scheme is as follows：
A kind of preparation method of disc type Multi-channel flat plate ceramic membrane, the supporter of the disc type Multi-channel flat plate ceramic membrane
Rounded tabular, its center have a hydrops through hole, and which is radially inside provided with some ducts in direction, are being propped up with improving filtrate
Mobility in support body, the duct one end are closed, and the other end is connected with hydrops through hole, and some ducts are that monolayer is arranged or multilamellar
Arrange；
Specifically include following steps：
(1) by 70～90: 2～5: 2～5: 5～10 weight ratio by ceramic aggregate, pore creating material, dispersant and gel injection-moulding
Binding agent 2～4h of mixing and ball milling, obtains mixed-powder, alumina powder, carborundum powder of the above-mentioned ceramic aggregate for 1～200 μm of particle diameter
Or cordierite powder, above-mentioned gel injection-moulding binding agent is avirulence natural polymer colloid；
(2) above-mentioned mixed-powder is mixed with 1～2.5: 1 volume ratio with RO water, is then heated to 40～85 DEG C, ball milling
4～20h, makes finely dispersed slurry；
(3) slurry obtained by step (2) is carried out into froth in vacuum while its temperature is maintained for 40～85 DEG C, be injected into into
In pattern tool, the slurry in mould is made to be gelled and formed in situ by controlling 0～40 DEG C of forming temperature, the demoulding obtains wet
Base, is provided with tubulose or bar molds to form the duct in above-mentioned mould；
(4) by above-mentioned wet base Jing after room temperature dries in the shade 1～5d and 40～100 DEG C of 1～5d of drying, it is incubated in 1000～1700 DEG C
1～4h of sintering, it is 30～70% to obtain porosity, and average pore size is 0.2～50 μm, support of the comprcssive strength in 20-40MPa
Body；
(5) the preparative separation film layer on above-mentioned support external surface, obtains final product the disc type Multi-channel flat plate ceramic membrane.
In a preferred embodiment of the invention, the cross sectional shape in the duct is circular, oval row or polygon.
In a preferred embodiment of the invention, the pore creating material is starch or graphite powder.
In a preferred embodiment of the invention, the dispersant is carboxymethyl cellulose, methylcellulose, poly- second
Enol or Polyethylene Glycol.
In a preferred embodiment of the invention, the gel injection-moulding binding agent is gelatin, agarose, agar, fruit
Sugar, Irish platform glue, shitosan or protein.
In a preferred embodiment of the invention, step (1) is：By 70～90wt%: 2～5wt%: 2～
The percentage by weight of 5wt%: 5～10wt% is by ceramic aggregate, pore creating material, dispersant and gel injection-moulding binding agent mixing and ball milling 2
～4h, obtains mixed-powder.
In a preferred embodiment of the invention, step (5) are：Using soaking paste cladding process, sol-gel
Method, spraying process, the curtain coating or spread coating preparative separation film layer on above-mentioned support external surface, obtains final product the disc type multichannel
Ceramic membrane.
Beneficial effects of the present invention：The present invention preparation method it is simple to operate, die cost is low, to environment substantially without dirt
Dye, to operator's fanout free region, production efficiency is high, the circular multichannel earthenware slab membrane flux height of institute's molding, function admirable, its
Can be used for rotary dynamic filtration ceramic film component, break the production technology ridge of external disc type Multi-channel flat plate ceramic membrane
It is disconnected.
Description of the drawings
Fig. 1 is the structural representation of the supporter of circular multichannel earthenware slab film prepared by the present invention.
Specific embodiment
Accompanying drawing is combined below by way of specific embodiment to be further detailed technical scheme and describe.
The structure of the supporter of circular multichannel earthenware slab film prepared by following embodiments is as shown in figure 1, the disk
The 1 rounded tabular of supporter of formula Multi-channel flat plate ceramic membrane, its center have a hydrops through hole 11, and which is radially inside square
To some ducts 12 are provided with, to improve mobility of the filtrate in supporter 1,12 one end of duct is closed, the other end and hydrops
Through hole 11 is connected, and some ducts 12 are that monolayer is arranged or multilamellar is arranged.
Embodiment 1
(1) by carborundum (150 μm, 90wt%), activated carbon powder (30 μm, 2wt%), PVA powder (molecular weight 2000,
3wt%) with gelatin powder (purity 98%, 5wt%) mixing and ball milling 2h, mixed-powder is obtained；
(2) above-mentioned mixed-powder is mixed with 2.5: 1 volume ratio with RO water, then heating in water bath is to 85 DEG C, ball milling
20h, makes finely dispersed slurry；
(3) slurry obtained by step (2) is carried out into froth in vacuum while its temperature is maintained for 80 DEG C, be injected into shaping mould
In tool, the slurry in mould is made to be gelled and formed in situ by controlling 20 DEG C of forming temperature, the demoulding obtains wet base, above-mentioned
It is provided with tubulose or bar molds to form the duct 12 in mould；
(4) above-mentioned wet base is dried in the shade 48h and 75 DEG C Jing room temperature and is dried after 40h, in 1550 DEG C of heat preservation sintering 2.5h, obtain hole
Gap rate is 68%, and average pore size is 30 μm, and supporter (as shown in Figure 1) of the comprcssive strength in 34MPa, in the pressure of 0.1MPa
Under, the supporter pure water flux is 29m3/m2h；
(5) carbon of the one layer of aperture for 500nm is prepared by suspended nitride dip-coating method on above-mentioned support external surface
SiClx film, obtains final product the disc type Multi-channel flat plate ceramic membrane, under the pressure of 0.1MPa, the disc type Multi-channel flat plate ceramics
Film pure water flux is 10m3/m2h。
Embodiment 2
(1) by cordierite (1 μm, 85wt%), starch (1 μm, 2wt%), PEG powder (molecular weight 1000,3wt%) and fine jade
Rubber powder end (purity 98%, 10wt%) mixing and ball milling 4h, obtains mixed-powder；
(2) above-mentioned mixed-powder is mixed with 1.7: 1 volume ratio with RO water, then heating in water bath is to 45 DEG C, ball milling
20h, makes finely dispersed slurry；
(3) slurry obtained by step (2) is carried out into froth in vacuum while its temperature is maintained for 45 DEG C, be injected into shaping mould
In tool, the slurry in mould is made to be gelled and formed in situ by controlling 15 DEG C of forming temperature, the demoulding obtains wet base, above-mentioned
It is provided with tubulose or bar molds to form the duct in mould；
(4) above-mentioned wet base is dried in the shade 72h and 60 DEG C Jing room temperature and is dried after 120h, in 1150 DEG C of heat preservation sintering 2h, obtain hole
Gap rate is 46%, and average pore size is 0.21 μm, and supporter (as shown in Figure 1) of the comprcssive strength in 29MPa, in the pressure of 0.1MPa
Under, the supporter pure water flux is 17m3/m2h；
(5) silicon carbide film of the one layer of aperture for 50nm is prepared by spraying process on above-mentioned support external surface, obtains final product institute
Disc type Multi-channel flat plate ceramic membrane is stated, under the pressure of 0.1MPa, the disc type Multi-channel flat plate ceramic membrane pure water flux is
2.8m3/m2h。
Embodiment 3
(1) aluminium oxide (100 μm, 95wt%), activated carbon powder (10 μm, 2wt%), MC powder (molecular weight 2800,1wt%)
With agarose powder (purity 98%, 5wt%) mixing and ball milling 3h, mixed-powder is obtained；
(2) above-mentioned mixed-powder is mixed with 2.1: 1 volume ratio with RO water, then heating in water bath is to 70 DEG C, ball milling
20h, makes finely dispersed slurry；
(3) slurry obtained by step (2) is carried out into froth in vacuum while its temperature is maintained for 75 DEG C, be injected into shaping mould
In tool, the slurry in mould is made to be gelled and formed in situ by controlling 25 DEG C of forming temperature, the demoulding obtains wet base, above-mentioned
It is provided with tubulose or bar molds to form the duct in mould；
(4) above-mentioned wet base is dried in the shade 72h and 65 DEG C Jing room temperature and is dried after 40d, in 1550 DEG C of heat preservation sintering 3h, obtain hole
Rate is 67%, and average pore size is 23 μm, supporter (as shown in Figure 1) of the comprcssive strength in 25MPa, under the pressure of 0.1MPa,
The supporter pure water flux is 19m3/m2h；
(5) one layer of aperture of preparation is sent out for the pellumina of 100nm by spraying on above-mentioned support external surface, obtains final product institute
Disc type Multi-channel flat plate ceramic membrane is stated, under the pressure of 0.1MPa, the disc type Multi-channel flat plate ceramic membrane pure water flux is
7.8m3/m2h。
The above, only presently preferred embodiments of the present invention, therefore the scope of present invention enforcement can not be limited according to this, i.e.,
The equivalence changes made according to the scope of the claims of the present invention and description and modification, all still should belong in the range of the present invention covers.
Claims (7)
1. a kind of preparation method of disc type Multi-channel flat plate ceramic membrane, it is characterised in that：The disc type Multi-channel flat plate ceramics
The rounded tabular of supporter of film, its center have a hydrops through hole, and which is radially inside provided with some ducts in direction, to carry
Mobility of the high filtrate in supporter, the duct one end are closed, and the other end is connected with hydrops through hole, and some ducts are monolayer
Arrange or multilamellar is arranged；Specifically include following steps：
(1) ceramic aggregate, pore creating material, dispersant and gel injection-moulding are bondd by 70～90: 2～5: 2～5: 5～10 weight ratio
Agent 2～4h of mixing and ball milling, obtains mixed-powder, and above-mentioned ceramic aggregate is alumina powder, carborundum powder or the violet of 1～200 μm of particle diameter
Bluestone powder, above-mentioned gel injection-moulding binding agent are avirulence natural polymer colloid；
(2) above-mentioned mixed-powder is mixed with 1～2.5: 1 volume ratio with RO water, is then heated to 40～85 DEG C, ball milling 4～
20h, makes finely dispersed slurry；
(3) slurry obtained by step (2) is carried out into froth in vacuum while its temperature is maintained for 40～85 DEG C, be injected into shaping mould
In tool, the slurry in mould is made to be gelled and formed in situ by controlling 0～40 DEG C of forming temperature, the demoulding obtains wet base,
It is provided with tubulose or bar molds to form the duct in above-mentioned mould；
(4) by above-mentioned wet base Jing after room temperature dries in the shade 1～5d and 40～100 DEG C of 1～5d of drying, in 1000～1700 DEG C of heat preservation sinterings
1～4h, it is 30～70% to obtain porosity, and average pore size is 0.2～50 μm, supporter of the comprcssive strength in 20-40MPa；
(5) the preparative separation film layer on above-mentioned support external surface, obtains final product the disc type Multi-channel flat plate ceramic membrane.
2. preparation method as claimed in claim 1, it is characterised in that：The cross sectional shape in the duct for circular, oval row or
Polygon.
3. preparation method as claimed in claim 1, it is characterised in that：The pore creating material is starch or graphite powder.
4. preparation method as claimed in claim 1, it is characterised in that：The dispersant is carboxymethyl cellulose, Methyl cellulose
Element, polyvinyl alcohol or Polyethylene Glycol.
5. preparation method as claimed in claim 1, it is characterised in that：The gel injection-moulding binding agent is gelatin, agarose, fine jade
Glue, Fructose, Irish platform glue, shitosan or protein.
6. preparation method as claimed in claim 1, it is characterised in that：Step (1) is：By 70～90wt%：2～
5wt%：2～5wt%：The percentage by weight of 5～10wt% is by ceramic aggregate, pore creating material, dispersant and gel injection-moulding binding agent
2～4h of mixing and ball milling, obtains mixed-powder.
7. preparation method as claimed in claim 1, it is characterised in that：Step (5) are：Using soaking paste cladding process, colloidal sol-
Gel method, spraying process, the curtain coating or spread coating preparative separation film layer on above-mentioned support external surface, obtains final product the disc type many
Multi-channel plate ceramic membrane.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602091A (en) * | 2017-09-22 | 2018-01-19 | 山东理工大学 | A kind of preparation method of dish-style alumina filter film |
| CN109248566A (en) * | 2018-11-28 | 2019-01-22 | 焦国豪 | A kind of hollow plate type ceramic film of helical duct and preparation method thereof |
| CN110141972A (en) * | 2019-05-29 | 2019-08-20 | 浙江中诚环境研究院有限公司 | The preparation method of disk type flat ceramic filter membrane |
| CN110559872A (en) * | 2019-08-14 | 2019-12-13 | 浙江理工大学 | Preparation method of shaft disc type rotating ceramic membrane |
| CN114053877A (en) * | 2020-08-01 | 2022-02-18 | 常启兵 | Preparation method of disc-type ceramic membrane support and ceramic membrane product thereof |
| CN114249582A (en) * | 2020-09-25 | 2022-03-29 | 三达膜科技（厦门）有限公司 | Internal multi-runner disc type alumina ceramic membrane and preparation method thereof |
| CN114311225A (en) * | 2022-01-18 | 2022-04-12 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane and high-pressure slip casting method thereof |
| CN114452830A (en) * | 2022-01-18 | 2022-05-10 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane and one-step forming method thereof |
| CN114452829A (en) * | 2022-01-18 | 2022-05-10 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane and material distribution method thereof |
| CN114452834A (en) * | 2022-01-18 | 2022-05-10 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602091A (en) * | 2017-09-22 | 2018-01-19 | 山东理工大学 | A kind of preparation method of dish-style alumina filter film |
| CN109248566A (en) * | 2018-11-28 | 2019-01-22 | 焦国豪 | A kind of hollow plate type ceramic film of helical duct and preparation method thereof |
| CN110141972B (en) * | 2019-05-29 | 2022-06-17 | 浙江中诚环境研究院有限公司 | Preparation method of disc type flat ceramic filter membrane |
| CN110141972A (en) * | 2019-05-29 | 2019-08-20 | 浙江中诚环境研究院有限公司 | The preparation method of disk type flat ceramic filter membrane |
| CN110559872A (en) * | 2019-08-14 | 2019-12-13 | 浙江理工大学 | Preparation method of shaft disc type rotating ceramic membrane |
| CN110559872B (en) * | 2019-08-14 | 2022-03-01 | 浙江理工大学 | Preparation method of shaft disc type rotating ceramic membrane |
| CN114053877A (en) * | 2020-08-01 | 2022-02-18 | 常启兵 | Preparation method of disc-type ceramic membrane support and ceramic membrane product thereof |
| CN114053877B (en) * | 2020-08-01 | 2024-01-23 | 常启兵 | Preparation method of disc-type ceramic membrane support and ceramic membrane product thereof |
| CN114249582B (en) * | 2020-09-25 | 2023-01-10 | 三达膜科技（厦门）有限公司 | Internal multi-runner disc type alumina ceramic membrane and preparation method thereof |
| CN114249582A (en) * | 2020-09-25 | 2022-03-29 | 三达膜科技（厦门）有限公司 | Internal multi-runner disc type alumina ceramic membrane and preparation method thereof |
| CN114452829A (en) * | 2022-01-18 | 2022-05-10 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane and material distribution method thereof |
| CN114452834A (en) * | 2022-01-18 | 2022-05-10 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane |
| CN114452830A (en) * | 2022-01-18 | 2022-05-10 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane and one-step forming method thereof |
| CN114311225A (en) * | 2022-01-18 | 2022-04-12 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane and high-pressure slip casting method thereof |
| 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 |
| CN114452834B (en) * | 2022-01-18 | 2023-11-03 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane |
| CN114452829B (en) * | 2022-01-18 | 2023-11-03 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane and distribution method thereof |
| CN114311225B (en) * | 2022-01-18 | 2023-11-03 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane and high-pressure grouting forming method thereof |
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Application publication date: 20170322 |