CN106390767A - Honeycomb ceramic composite membrane and method for preparing same - Google Patents
Honeycomb ceramic composite membrane and method for preparing same Download PDFInfo
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- CN106390767A CN106390767A CN201610980441.1A CN201610980441A CN106390767A CN 106390767 A CN106390767 A CN 106390767A CN 201610980441 A CN201610980441 A CN 201610980441A CN 106390767 A CN106390767 A CN 106390767A
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- Prior art keywords
- composite membrane
- honey comb
- ceramic honey
- membrane
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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
- B01D69/12—Composite membranes; Ultra-thin 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
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
-
- 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
-
- 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
- B01D71/06—Organic material
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/22—Thermal or heat-resistance properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/30—Chemical resistance
Abstract
The invention discloses a honeycomb ceramic composite membrane and a method for preparing the same. The method includes steps of (1), adding organic polymeric membrane materials into organic solvents, adding pore-forming agents into the organic solvents, uniformly stirring and mixing the organic polymeric membrane materials, the organic solvents and the pore-forming agents, completely dissolving the organic polymeric membrane materials to form membrane casting solution, heating the membrane casting solution by water bath and removing bubble; (2), soaking honeycomb ceramics with clean surfaces in the prepared membrane casting solution, lifting the honeycomb ceramics and forming the honeycomb ceramic composite membrane by means of heat treatment. The honeycomb ceramic composite membrane and the method have the advantages that the method includes simple processes, the honeycomb ceramic composite membrane has large membrane areas in unit volume as compared with single-tube ceramic membranes, the shortcomings of low filter precision of common honeycomb ceramics and low flux of the single-tube ceramic membranes can be effectively overcome, and the honeycomb ceramic composite membrane and the method can be widely applied to the fields of sewage and drinking water treatment, petrochemical engineering and papermaking printing and dyeing.
Description
Technical field
The present invention relates to composite separating film preparing technical field is and in particular to a kind of ceramic honey comb composite membrane and its preparation side
Method.
Background technology
Water is one of base substance condition that human society is depended on for existence and development, even if present people have very high section
About use the consciousness of water, but the present situation of hydropenia is increasingly severe.Entangling its reason has following three points：（One）Although the earth more than seventy percent
Area awash, but be mostly wherein the sea water that not directly utilizes, and in the fresh water of remaining only a few,
Glacial water account for greatly；（Two）The development of modern industrial and agricultural production and the surge of urban population density, the mankind provide to water
The consuming in source and demand sharply increase；（Three）Offshore production oil, transfer oil, the steel-making row such as oil refining industry and food processing
Industry creates substantial amounts of oily waste water, has not only had a strong impact on the health of the mankind, also exacerbates the same water resource of social development demand
The not enough contradiction of supply.So the high efficiency of waste water is purified be increasingly becoming put thorny in current one of water process scientist
Thing, have the advantages that efficient, inexpensive membrane separation technique is arisen at the historic moment.
Ceramic membrane has been successfully applied to the neck such as food, beverage, medicine, environmental conservation, biotechnology, fermentation engineering at present
Domain.But one of main problem that present membrane technology faces is：The effective area of unit volume inner membrance is little.Although currently also having one
Large-scale membrane treatment appts a bit, but equipment volume is big, price is high.The advantage in specific surface area due to ceramic honey comb in recent years,
The air pollutants such as denitrification, sulfide can efficiently be gone by supported catalyst, be widely used in purification
In room air or process vehicle exhaust.Patent CN 105312043A discloses one kind and is used for processing PTA tail gas high intensity honeycomb
The preparation method of ceramic catalyst, by the coat on ceramic honey comb surface so that water resistant ability strengthens, increased catalyst
Life-span.Patent CN 105126797A is disclosed one kind and using sol method, nano titanium oxide is supported on honeycomb ceramic carrier,
Catalyst surface area in unit volume is increased, considerably increases the time that gas is contacted with catalyst, improve light quantum
Efficiency, exhaust purification efficiency is up to 98%.
There is presently no and see the report developing in water treatment field with regard to ceramic honey comb film.Hence with honeycomb pottery
Porcelain film unit volume intimal surface amasss big advantage and applies it to water treatment field, has very big development prospect.
Although ceramic honey comb film considerably increases in unit volume Intimal area compared with single hose ceramic membrane, but due to
When being used alone, normal cellular ceramic surface aperture is larger, and filtering accuracy is relatively low, significantly limit it in water treatment field
Application.So by being modified using active layer on its surface, not only making membrane area not change, and improve filtration
Precision, this considerably increases the scope of application.
Content of the invention
The present invention is directed to the shortcoming of prior art, proposes a kind of ceramic honey comb composite membrane and preparation method thereof.
The ceramic honey comb composite membrane that the present invention prepares has the advantages that membrane flux is high, rejection is good, good mechanical property.
The present invention is achieved through the following technical solutions.
A kind of preparation method of ceramic honey comb composite membrane, comprises the steps：
（1）Prepare casting solution：Organic polymer membrane material is added in organic solvent, adds pore creating material, stirring mixing under room temperature
Uniformly, organic polymer membrane material is made to be completely dissolved formation casting solution, heating in water bath removes bubble；
（2）The ceramic honey comb of clean surface is immersed in the casting solution of preparation, lifting, heat treatment film forming, obtains described honeycomb
Ceramic composite membrane.
Further, step（1）In, described organic polymer membrane material is that Kynoar, polyvinyl alcohol and acetic acid are fine
One of plain membrane material of dimension.
Further, step（1）In, described organic solvent is N-N dimethyl acetylamide, N-N dimethylformamide, acetone
One of with dimethyl sulfoxide.
Further, step（1）In, described pore creating material is lithium chloride.
Further, step（1）In, described organic polymer membrane material is 8 ~ 12 with the solid-liquid ratio of organic solvent:88~
92g/mL.
Further, step（1）In, described organic polymer membrane material is 8 ~ 12 with the mass ratio of pore creating material:1~3g/g.
Further, step（2）In, the material of described ceramic honey comb is one of cordierite, mullite and aluminium titanates
More than.
Further, step（2）In, the time of described immersion is 20-30s.
Further, step（2）In, the temperature of described heat treatment is 60-90 DEG C, and heat treatment time is 4 ~ 8h.
Further, repeat step（2）1-3 time, obtain described ceramic honey comb composite membrane.
The ceramic honey comb composite membrane that preparation method described in any of the above-described is obtained, the aperture of described ceramic honey comb composite membrane
Uniformly, the supporting layer of ceramic honey comb composite membrane is ceramic honey comb film, forms organic high molecular layer stratum disjunctum in support layer surface.
Compared with prior art, the invention has the advantages that：
（1）In the inventive method, the ceramic honey comb composite membrane of preparation, with inorganic ceramic honey comb film as material of main part, is made pottery with single hose
Porcelain film is compared, and in unit volume, ceramic honey comb film has bigger membrane area, and the ceramic honey comb composite membrane of preparation equally has
Bigger membrane area, so that membrane treatment appts equipment volume greatly reduces under equal conditions.
（2）The ceramic honey comb composite membrane of the inventive method preparation has supporting layer and stratum disjunctum, the inventive method preparation
Ceramic honey comb composite membrane has the features such as membrane flux is high, rejection is good, is widely used in steel machinery factory, sewage and potable water
The fields such as reason, food processing, petrochemical industry and papermaking printing and dyeing.
（3）In the present invention, ceramic honey comb used is provided that a supporting layer well, and heat stability is high, hydrolysis, with
Can there is very strong adhesion between organic high molecular layer, also not interfere with membrane flux.
Specific embodiment
For more fully understanding the present invention, with reference to embodiment, the present invention is further illustrated, but the reality of the present invention
Mode of applying does not limit so.
Embodiment 1
（1）Prepare casting solution：Precise 8.0g Kynoar, 92.0mlN-N dimethyl acetylamide, the lithium chloride of 3.0g；
Weighed solid and liquid charging stock are added to mix homogeneously in round-bottomed flask, stirring at normal temperatures makes Kynoar complete
Dissolving, casting solution heating in water bath makes its complete froth breaking；
（2）The clean ceramic honey comb of dry tack free is immersed in after 30s lifting once in casting solution, is placed in 80 DEG C of air dry oven
Heat treatment 4h film forming；
（3）Repeat step（2）Twice, obtain ceramic honey comb composite membrane.
Tested with the oily waste water of 100mg/L by ceramic honey comb composite membrane manufactured in the present embodiment, in 0.1MPa
Under, flux reaches 118.2L/m2•h；After purifying through ceramic honey comb composite membrane, oil concentration is less than the national oily waste water row of 10mg/L
Put standard, can directly discharge；And the flux that single hose ceramic membrane is tested under these conditions is 76.4 L/m2•h；The honeybee of preparation
Nest Ceramic Composite membrane flux is significantly higher.
In unit volume, the membrane area of the ceramic honey comb film used in this embodiment is 12 m2, and single hose pottery
The membrane area of porcelain film is only 4 m2；Compared to single hose ceramic membrane, the membrane area in ceramic honey comb film unit volume is significantly larger.
Embodiment 2
（1）Prepare casting solution：Precise 8.0g cellulose acetate, 91.0ml acetone, the lithium chloride of 1.0g；Will be weighed solid
Body and liquid charging stock are added to mix homogeneously in round-bottomed flask, and stirring at normal temperatures makes cellulose acetate be completely dissolved, casting solution
Heating in water bath makes its complete froth breaking；
（2）The clean ceramic honey comb supporting layer of dry tack free is immersed in after 20s lifting once in casting solution, is placed in forced air drying
70 DEG C of heat treatment 8h film forming of case, obtain ceramic honey comb composite membrane.
Tested with the oily waste water of 100mg/L by ceramic honey comb composite membrane manufactured in the present embodiment, in 0.1MPa
Under, flux reaches 63.8L/m2•h；After purifying through ceramic honey comb composite membrane, oil concentration is less than the national oily waste water row of 10mg/L
Put standard, can directly discharge；And the flux that single hose ceramic membrane is tested under these conditions is 39.6 L/m2•h；The honeybee of preparation
The flux of nest ceramic composite membrane is significantly higher.
In unit volume, the membrane area of the ceramic honey comb film used in this embodiment is 12 m2, and single hose pottery
The membrane area of porcelain film is only 4 m2；Compared to single hose ceramic membrane, the membrane area in ceramic honey comb film unit volume is significantly larger.
Embodiment 3
（1）Prepare casting solution：Precise 12.0g Kynoar, 88.0mlN-N dimethylformamide, the lithium chloride of 3.0g；
Weighed solid and liquid charging stock are added to mix homogeneously in round-bottomed flask, stirring at normal temperatures makes Kynoar complete
Dissolving, casting solution heating in water bath makes its complete froth breaking；
（2）Clean for dry tack free ceramic honey comb supporting layer is immersed in after 20s lifting once in casting solution, is placed in air blast and does
Dry 60 DEG C of heat treatment 6h film forming of case；
（3）Repeat step（2）Twice, obtain ceramic honey comb composite membrane.
Tested with the oily waste water of 100mg/L by ceramic honey comb composite membrane manufactured in the present embodiment, in 0.1MPa
Under, flux reaches 84.3L/m2•h；After purifying through ceramic honey comb composite membrane, oil concentration is less than the national oily waste water row of 10mg/L
Put standard, can directly discharge；And the flux that single hose ceramic membrane is tested under these conditions is 54.6 L/m2•h；The honeybee of preparation
The flux of nest ceramic composite membrane is significantly higher.
In unit volume, the membrane area of the ceramic honey comb film used in this embodiment is 12 m2, and single hose pottery
The membrane area of porcelain film is only 4 m2；Compared to single hose ceramic membrane, the membrane area in ceramic honey comb film unit volume is significantly larger.
Embodiment 4
（1）Prepare casting solution：Precise 10.0g polyvinyl alcohol, 90.0ml dimethyl sulfoxide, the lithium chloride of 2.0g；Will be alleged
The solid of amount and liquid charging stock are added to mix homogeneously in round-bottomed flask, and stirring at normal temperatures makes polyvinyl alcohol be completely dissolved, casting
Film liquid heating in water bath makes its complete froth breaking；
（2）The clean ceramic honey comb supporting layer of dry tack free is immersed in after 20s lifting once in casting solution, is placed in forced air drying
90 DEG C of heat treatment 6h film forming of case, obtain ceramic honey comb composite membrane.
Tested with the oily waste water of 100mg/L by ceramic honey comb composite membrane manufactured in the present embodiment, in 0.1MPa
Under, flux reaches 86.9 L/m2•h；After purifying through ceramic honey comb composite membrane, oil concentration is less than the national oily waste water row of 10mg/L
Put standard, can directly discharge；And the flux that single hose ceramic membrane is tested under these conditions is 56.3L/m2•h；The honeycomb of preparation
The flux of ceramic composite membrane is significantly higher.
In unit volume, the membrane area of the ceramic honey comb film used in this embodiment is 12 m2, and single hose pottery
The membrane area of porcelain film is only 4 m2；Compared to single hose ceramic membrane, the membrane area in ceramic honey comb film unit volume is substantially more
Greatly.
Embodiment 5
（1）Prepare casting solution：Precise 12.0g Kynoar, 88.0mlN-N dimethyl acetylamide, the chlorination of 1.0g
Lithium；Weighed solid and liquid charging stock are added to mix homogeneously in round-bottomed flask, stirring at normal temperatures makes Kynoar
It is completely dissolved, casting solution heating in water bath makes its complete froth breaking；
（2）The clean ceramic honey comb supporting layer of dry tack free is immersed in after 30s lifting once in casting solution, is placed in forced air drying
80 DEG C of heat treatment 4h film forming of case；
（3）Repeat step（2）Twice, obtain ceramic honey comb composite membrane.
Tested with the oily waste water of 100mg/L by ceramic honey comb composite membrane manufactured in the present embodiment, in 0.1MPa
Under, flux reaches 69.2L/m2•h；After purifying through ceramic honey comb composite membrane, oil concentration is less than the national oily waste water row of 10mg/L
Put standard, can directly discharge；And the flux that single hose ceramic membrane is tested under these conditions is 43.1 L/m2•h；The honeybee of preparation
The flux of nest ceramic composite membrane is significantly higher.
In unit volume, the membrane area of the ceramic honey comb film used in this embodiment is 12 m2, and single hose pottery
The membrane area of porcelain film is only 4m2；Compared to single hose ceramic membrane, the membrane area in ceramic honey comb film unit volume is substantially more
Greatly.
It should be appreciated that for those skilled in the art, being improved according to the above description or be converted, and
All these modifications and variations all should belong to the protection domain of claims of the present invention.
Claims (10)
1. a kind of preparation method of ceramic honey comb composite membrane is it is characterised in that comprise the steps：
（1）Prepare casting solution：Organic polymer membrane material is added in organic solvent, adds pore creating material, stirring mixing under room temperature
Uniformly, organic polymer membrane material is made to be completely dissolved formation casting solution, heating in water bath removes bubble；
（2）The ceramic honey comb of clean surface is immersed in the casting solution of preparation, lifting, heat treatment film forming, obtains described honeycomb
Ceramic composite membrane.
2. a kind of preparation method of ceramic honey comb composite membrane according to claim 1 is it is characterised in that step（1）In, institute
Stating organic polymer membrane material is one of Kynoar, polyvinyl alcohol and cellulose acetate membrane material material.
3. a kind of preparation method of ceramic honey comb composite membrane according to claim 1 is it is characterised in that step（1）In, institute
Stating organic solvent is one of N-N dimethyl acetylamide, N-N dimethylformamide, acetone and dimethyl sulfoxide.
4. a kind of preparation method of ceramic honey comb composite membrane according to claim 1 is it is characterised in that step（1）In, institute
Stating pore creating material is lithium chloride.
5. a kind of preparation method of ceramic honey comb composite membrane according to claim 1 is it is characterised in that step（1）In, institute
The solid-liquid ratio stating organic polymer membrane material with organic solvent is 8 ~ 12:88~92g/mL；Described organic polymer membrane material with make
The mass ratio of hole agent is 8 ~ 12:1~3g/g.
6. a kind of preparation method of ceramic honey comb composite membrane according to claim 1 is it is characterised in that step（2）In, institute
The material stating ceramic honey comb is one or more of cordierite, mullite and aluminium titanates.
7. a kind of preparation method of ceramic honey comb composite membrane according to claim 1 is it is characterised in that step（2）In, institute
The time stating immersion is 20-30s.
8. a kind of preparation method of ceramic honey comb composite membrane according to claim 1 is it is characterised in that step（2）In, institute
The temperature stating heat treatment is 60-90 DEG C, and heat treatment time is 4 ~ 8h.
9. a kind of preparation method of ceramic honey comb composite membrane according to claim 1 is it is characterised in that repeat step（2）
1-3 time, obtain described ceramic honey comb composite membrane.
10. the ceramic honey comb composite membrane that preparation method described in any one of claim 1-9 is obtained is it is characterised in that described honeybee
The uniform pore diameter of nest ceramic composite membrane, the supporting layer of ceramic honey comb composite membrane is ceramic honey comb film, is formed with support layer surface
Organic polymeric membrane stratum disjunctum.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610980441.1A CN106390767A (en) | 2016-11-08 | 2016-11-08 | Honeycomb ceramic composite membrane and method for preparing same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610980441.1A CN106390767A (en) | 2016-11-08 | 2016-11-08 | Honeycomb ceramic composite membrane and method for preparing same |
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| CN201610980441.1A Pending CN106390767A (en) | 2016-11-08 | 2016-11-08 | Honeycomb ceramic composite membrane and method for preparing same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114471511A (en) * | 2022-02-18 | 2022-05-13 | 大连理工大学 | Preparation method of high-flux visible-light-responsive nanowire catalytic ceramic membrane |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007077646A1 (en) * | 2005-12-28 | 2007-07-12 | Asahi Kasei Chemicals Corporation | Process for producing composite membrane |
| CN103521095A (en) * | 2013-10-31 | 2014-01-22 | 上海赛奥分离技术工程有限公司 | Method for preparing tubular ceramic membrane for oil-water separation |
| CN105000871A (en) * | 2015-07-08 | 2015-10-28 | 深圳中清环境科技有限公司 | Multi-functional flat-sheet ceramic film and preparation process thereof |
-
2016
- 2016-11-08 CN CN201610980441.1A patent/CN106390767A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007077646A1 (en) * | 2005-12-28 | 2007-07-12 | Asahi Kasei Chemicals Corporation | Process for producing composite membrane |
| CN103521095A (en) * | 2013-10-31 | 2014-01-22 | 上海赛奥分离技术工程有限公司 | Method for preparing tubular ceramic membrane for oil-water separation |
| CN105000871A (en) * | 2015-07-08 | 2015-10-28 | 深圳中清环境科技有限公司 | Multi-functional flat-sheet ceramic film and preparation process thereof |
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|---|
| 张明: "《纳米与新材料专辑 5》", 25 November 2005, 材料报道社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114471511A (en) * | 2022-02-18 | 2022-05-13 | 大连理工大学 | Preparation method of high-flux visible-light-responsive nanowire catalytic ceramic membrane |
| CN114471511B (en) * | 2022-02-18 | 2023-01-13 | 大连理工大学 | Preparation method of high-flux visible-light-responsive nanowire catalytic ceramic membrane |
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Application publication date: 20170215 |