CN107362586B - The preparation method and application of super-hydrophobic super-oleophylic water-oil separating cork filter membrane - Google Patents
The preparation method and application of super-hydrophobic super-oleophylic water-oil separating cork filter membrane Download PDFInfo
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- CN107362586B CN107362586B CN201710565096.XA CN201710565096A CN107362586B CN 107362586 B CN107362586 B CN 107362586B CN 201710565096 A CN201710565096 A CN 201710565096A CN 107362586 B CN107362586 B CN 107362586B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/08—Thickening liquid suspensions by filtration
- B01D17/085—Thickening liquid suspensions by filtration with membranes
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Abstract
The invention belongs to remove oil type water-oil separating material technical field, more particularly to a kind of preparation method and application of super-hydrophobic super-oleophylic water-oil separating cork filter membrane, it is modified including raw material drying, surface oxidation and surface, the cork filter membrane of preparation and the contact angle of water are more than 150 °, contact angle with oil is 0 °, and the roll angle of water is less than 10 °, and the cork filter membrane of preparation is used for the separating treatment of oil water mixture, cork raw material convenient material drawing, renewable, the filter membrane of preparation has the advantages that separative efficiency is high.
Description
Technical field
The invention belongs to remove oil type water-oil separating material technical field more particularly to a kind of super-hydrophobic super-oleophylic water-oil separating
The preparation method and application of cork filter membrane.
Background technology
With the development of science and technology, the living environment of the mankind receives the pollution at more and more pollutions, especially water source, often
The water pollution seen includes water pollution caused by oil exploitation, marine transportation oil accident and factories and miness, enterprise's oil-containing（It is molten
Agent）The discharge in violation of regulations of sewage, the sewage siltation of generation can block the pipeline of enterprise, and serious dirt can be caused by being directly discharged to environment
Dye, causes ecological environment potentially hazardous, and is possible to jeopardize the health of the mankind.Usual oil-water separation method includes weight
Force method, centrifugal process, absorption method, floatation and chemical method etc., but these methods are limited due to high costs and inefficiency
Its application, additionally is able to the oil adsorbent overwhelming majority non-degradable of absorption oil, will also result in secondary pollution.In order to detach
It during oil water mixture and emulsion, improves water-oil separating efficiency, reduce cost and energy consumption, start exploration in recent years and use filter membrane
Handle oily wastewater.But grease filter membrane now（And sorbing material）Multi-purpose copper mesh, steel mesh, filter paper, fiber, ceramics, polymer, fibre
Prepared by dimension element, and modify other substances with special wetability, but these bionical separation materials are non-renewable, and repeatedly makes
It is difficult to degrade after, secondary pollution is caused to environment.
Invention content
The object of the present invention is to provide a kind of convenient material drawing, the super-hydrophobic super-oleophylic greases point that renewable, separative efficiency is high
Preparation method and application from cork filter membrane.
In order to achieve the above objectives, the technical solution adopted by the present invention is：
A kind of preparation method of super-hydrophobic super-oleophylic water-oil separating cork filter membrane, comprises the steps of：
（1）It is dry：First, softwood trees crust is placed in baking oven and is dried for the first time, drying temperature is 40~80 DEG C, dry
Time is 1~3 week, obtains primary drying softwood trees crust, then primary drying softwood trees crust is placed in boiling in 100 DEG C of boiling water
1.0~1.5h obtains smooth softwood trees crust, and smooth softwood trees crust, which is then placed in baking oven second, dries, and two
The temperature of secondary drying is 40~80 DEG C, and the time of redrying is 1~3 week, redrying softwood trees crust is obtained, finally, by two
Secondary dry softwood trees crust handle thickness be 0.5~2.5mm cork filter membrane；
（2）Oxidation：It is 10~30% H to use mass concentration at ambient temperature2O220~40min is aoxidized to cork filter membrane,
It is washed with distilled water 3 times, is placed in oven and dried after oxidation, dry temperature is 40~80 DEG C, and drying time 2h must be aoxidized
Handle filter membrane；
（3）It is modified：Cork filter membrane after oxidation is placed in the closed container equipped with mixed solution and is modified, to container constant temperature
Heating, heating temperature are 60 DEG C, and heating time is for 24 hours, after filter membrane taking-up ethyl alcohol and distilled water are washed three times respectively, then right
Cork filter membrane is dried, and drying temperature is 60 DEG C, and the time of redrying is 2h.
Further, the step（1）In cork be cork oak and quercus suber tree crust.
Further, the step（3）In mixed solution be made of alkyl triethoxysilane, distilled water and methanol,
And the volume ratio of alkyl triethoxysilane, distilled water and methanol is 1: 2: 10~1: 7: 30 in mixed solution.
Further, the step（3）In mixed solution be made of alkyl triethoxysilane and methanol, and mix it is molten
The volume ratio of alkyl triethoxysilane and methanol is 1: 10~1: 30 in liquid.
Further, the alkyl triethoxysilane is 1H, 1H, 2H, 2H- perfluoro decyl trichlorosilanes, 13
At least one of fluorine octyltri-ethoxysilane, octadecyltriethoxy silane, dodecyl triethoxysilane.
Further, the cork filter membrane prepared using the preparation method of super-hydrophobic super-oleophylic water-oil separating cork filter membrane,
It is characterized in that：The contact angle of the cork filter membrane and water is more than 150 °, and the contact angle with oil is 0 °, and the roll angle of water is less than 10 °.
Further, the application of super-hydrophobic super-oleophylic water-oil separating cork filter membrane, uses it for the separation of oil water mixture
It handles, the oil in oil water mixture is n-hexane, dimethylbenzene, hexamethylene, petroleum ether, diesel oil, gasoline, kerosene, dichloromethane, three
At least one of chloromethanes, carbon tetrachloride, 1,2- dichloromethane and nitrobenzene.
Present invention has the advantage that：
1. cork filter membrane itself rough surface provided by the invention, after surface modification by mixed solution, the silicon on surface
Alkane chain has hydrophobicity, reduces the free energy of filter membrane surface, filter membrane obtains good lipophile and hydrophobicity, makes filter membrane
With good oil and water separation capability；
2. cork filter membrane preparation method provided by the invention is simple, vegetable cork used is rich and easy to get, it is of low cost, can be again
It is raw, degradable.
Description of the drawings
Fig. 1 is super-hydrophobic super-oleophylic cork filter membrane SEM figures prepared by the embodiment of the present invention 1；
Fig. 2 is the water and n-hexane wetting figure of super-hydrophobic super-oleophylic cork filter membrane prepared by the embodiment of the present invention 1；
Fig. 3 is water wetting and the n-hexane process of osmosis of super-hydrophobic super-oleophylic cork filter membrane prepared by the embodiment of the present invention 1
Figure；
Fig. 4 is that super-hydrophobic super-oleophylic cork filter membrane prepared by the embodiment of the present invention 1 divides the grease of different oil water mixtures
From efficiency chart；
Fig. 5 is the water-oil separating efficiency and water contact angle of super-hydrophobic super-oleophylic cork filter membrane prepared by the embodiment of the present invention 1
With the separation increased variation diagram of number.
Specific implementation mode
Embodiment 1
As shown in Figs. 1-5, cork oak and quercus suber tree crust are peeled using axe, softwood trees crust is put into baking oven
Dry for the first time, drying temperature is 60 DEG C, and drying time is 2 weeks, obtains primary drying softwood trees crust, then by primary drying cork
Tree crust is placed in boiling 1.0h in 100 DEG C of boiling water, obtains smooth softwood trees crust, is then placed in smooth softwood trees crust
The temperature of second of drying in baking oven, redrying is 60 DEG C, and the time of redrying is 2 weeks, is obtained outside redrying softwood trees
Redrying softwood trees crust is finally sawn into the cork filter membrane that thickness is 2.0mm by skin using wood saw；Use quality hundred
It is 20% H to divide specific concentration2O230min is aoxidized to cork filter membrane at ambient temperature, is washed with distilled water after oxidation, is put after washing
It is 60 DEG C to enter temperature dry in baking oven, dry, and drying time 2h obtains oxidation processes filter membrane；By the cork filter membrane after oxidation
It is put into and 1H, 1H, 2H is housed, it is modified in the closed container of 2H- perfluoro decyl trichlorosilanes, distilled water and methanol, wherein 1H,
1H, 2H, 2H- perfluoro decyl trichlorosilane, distilled water and methanol volume ratio are 1: 5: 15, to container heated at constant temperature, heating temperature
Degree is 60 DEG C, and heating time is for 24 hours, after filter membrane taking-up ethyl alcohol and distilled water are washed three times respectively, then to be done to cork filter membrane
Dry, drying temperature is 60 DEG C, and the dry time is 2h to get super-hydrophobic super-oleophylic cork filter membrane.
Using super-hydrophobic super-oleophylic water-oil separating cork filter membrane preparation method prepare cork filter membrane, the cork filter membrane with
The contact angle of water is more than 150 °, and the contact angle with oil is 0 °, and the roll angle of water is less than 10 °.
The application of super-hydrophobic super-oleophylic water-oil separating cork filter membrane, uses it for the separating treatment of oil water mixture, grease
Oil in mixture is n-hexane, dimethylbenzene, hexamethylene, petroleum ether, diesel oil, gasoline, kerosene, dichloromethane, chloroform, four
At least one of chlorination carbon, 1,2- dichloromethane and nitrobenzene.
Embodiment 2
Embodiment 2 is differed only in embodiment 1：Cork bark first time drying temperature is 80 DEG C, drying time 1
In week, the time of boiling is 1.5h in boiling water, and the temperature of redrying is 80 DEG C, and the time of redrying is 1 week, will be secondary dry
Cork is sawn into the cork filter membrane that thickness is 2.5mm by dry softwood trees crust using wood saw, and use quality percent concentration is 30%
H2O220min is aoxidized to cork filter membrane at ambient temperature, is washed with distilled water after oxidation, is placed in oven and dried after washing, is done
Dry temperature is 60 DEG C, drying time 2h, and the cork filter membrane after oxidation is put into equipped with octadecyltriethoxy silane, is steamed
It is modified in the closed container of distilled water and methanol, wherein octadecyltriethoxy silane, distilled water and methanol volume ratio are 1: 2:
10。
Embodiment 3
Embodiment 3 is differed only in embodiment 1：Cork bark first time drying temperature is 40 DEG C, drying time 3
In week, the time of boiling is 1.5h in boiling water, and the temperature of redrying is 40 DEG C, and the time of redrying is 3 weeks, will be secondary dry
Cork is sawn into the cork filter membrane that thickness is 1.5mm by dry softwood trees crust using wood saw, and use quality percent concentration is 15%
H2O235min is aoxidized to cork filter membrane at ambient temperature, is washed with distilled water after oxidation, drying in baking oven is put in after washed,
Dry temperature is 40 DEG C, drying time 2h, and the cork filter membrane after oxidation is placed in equipped with ten trifluoro octyl triethoxysilicanes
It is modified in the closed container of alkane, distilled water and methanol, wherein octadecyltriethoxy silane, distilled water and methanol volume ratio
It is 1: 7: 30.
Embodiment 4
Embodiment 4 is differed only in embodiment 1：Cork bark first time drying temperature is 50 DEG C, and drying time is
2.5 weeks, the time of boiling was 1.5h in boiling water, and the temperature of redrying is 50 DEG C, and the time of redrying is 2.5 weeks, will
Cork is sawn into the cork filter membrane that thickness is 1.0mm, use quality percent concentration by redrying softwood trees crust using wood saw
For 10% H2O240min is aoxidized to cork filter membrane at ambient temperature, is washed with distilled water after oxidation, is put in baking oven after washing
Dry, dry temperature is 60 DEG C, drying time 2h, and the cork filter membrane after oxidation is placed in equipped with dodecyl triethoxy
It is modified in the closed container of silane and methanol, wherein dodecyl triethoxysilane and methanol volume ratio are 1: 10.
Embodiment 5
Embodiment 5 is differed only in embodiment 1：Cork bark first time drying temperature is 70 DEG C, and drying time is
1.5 weeks, the time of boiling was 1.5h in boiling water, and the temperature of redrying is 70 DEG C, and the time of redrying is 1.5 weeks, will
Cork is sawn into the cork filter membrane that thickness is 0.5mm, use quality percent concentration by redrying softwood trees crust using wood saw
For 10% H2O240min is aoxidized to cork filter membrane at ambient temperature, is washed with distilled water after oxidation, is put in baking oven after washing
Dry, dry temperature is 60 DEG C, drying time 2h, and the cork filter membrane after oxidation is placed in equipped with dodecyl triethoxy
It is modified in the closed container of silane and methanol, wherein dodecyl triethoxysilane and methanol volume ratio are 1: 30.
Claims (5)
1. a kind of preparation method of super-hydrophobic super-oleophylic water-oil separating cork filter membrane, which is characterized in that comprise the steps of：
（1）It is dry：First, softwood trees crust is placed in baking oven and is dried for the first time, drying temperature is 40~70 DEG C, drying time
Be 1~3 week, obtain primary drying softwood trees crust, then by primary drying softwood trees crust be placed in boiling 1.0 in 100 DEG C of boiling water~
1.5h obtains smooth softwood trees crust, and smooth softwood trees crust is then placed in baking oven second of dry, redrying
Temperature be 40~70 DEG C, time of redrying is 1~3 week, redrying softwood trees crust is obtained, finally, by redrying
Softwood trees crust is sawn into the cork filter membrane that thickness is 0.5~2.5mm using wood saw；
（2）Oxidation：It is 10~30% H to use mass concentration at ambient temperature2O220~40min, oxidation are aoxidized to cork filter membrane
After be washed with distilled water 3 times, be placed in oven and dried, dry temperature be 40~60 DEG C, drying time 2h obtains oxidation processes
Filter membrane；
（3）It is modified：Cork filter membrane after oxidation is placed in the closed container equipped with mixed solution and is modified, container constant temperature is added
Heat, heating temperature are 60 DEG C, and heating time is for 24 hours, after filter membrane taking-up ethyl alcohol and distilled water are washed three times respectively, then to soft
The wooden filter membrane drying, drying temperature are 60 DEG C, and the dry time is 2h；The mixed solution is by alkyl triethoxysilane, distillation
Water and methanol composition, and the volume ratio of alkyl triethoxysilane, distilled water and methanol is 1: 2: 10~1: 7 in mixed solution:
30；Or the mixed solution is made of alkyl triethoxysilane and methanol, and in mixed solution alkyl triethoxysilane and
The volume ratio of methanol is 1: 10~1: 30.
2. the preparation method of super-hydrophobic super-oleophylic water-oil separating cork filter membrane as described in claim 1, it is characterised in that：It is described
Step（1）In cork be cork oak and quercus suber tree crust.
3. the preparation method of super-hydrophobic super-oleophylic water-oil separating cork filter membrane as described in claim 1, it is characterised in that：It is described
Alkyl triethoxysilane be tridecafluoro-n-octyltriethoxysilane, octadecyltriethoxy silane, three second of dodecyl
At least one of oxysilane.
4. being prepared using the preparation method of any super-hydrophobic super-oleophylic water-oil separating cork filter membranes of claim 1-3 soft
The wooden filter membrane, it is characterised in that：The contact angle of the cork filter membrane and water is more than 150 °, and the contact angle with oil is 0 °, the rolling of water
Angle is less than 10 °.
5. the application of super-hydrophobic super-oleophylic water-oil separating cork filter membrane as claimed in claim 4, it is characterised in that：It uses it for
The separating treatment of oil water mixture, the oil in oil water mixture be n-hexane, dimethylbenzene, hexamethylene, petroleum ether, diesel oil, gasoline,
At least one of kerosene, dichloromethane, chloroform, carbon tetrachloride, 1,2- dichloromethane and nitrobenzene.
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| CN109248570B (en) * | 2018-09-28 | 2021-02-23 | 刘青 | Preparation method of PAN/PAMS/ZnO oil-water separation membrane |
| CN111330457B (en) * | 2020-02-21 | 2022-03-18 | 平顶山学院 | Preparation and application of pH-responsive natural plant oil-water separation filter membrane |
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| US6738815B1 (en) * | 1998-07-01 | 2004-05-18 | Telcordia Technologies, Inc. | Systems and methods for utilizing a communications network for providing mobile users access to legacy systems |
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