CN107261862A - A kind of bat calcium alginate gel compound is modified the preparation method and its usage of composite membrane - Google Patents
A kind of bat calcium alginate gel compound is modified the preparation method and its usage of composite membrane Download PDFInfo
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- CN107261862A CN107261862A CN201710404830.4A CN201710404830A CN107261862A CN 107261862 A CN107261862 A CN 107261862A CN 201710404830 A CN201710404830 A CN 201710404830A CN 107261862 A CN107261862 A CN 107261862A
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- composite membrane
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- calcium alginate
- alginate gel
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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
- B01D71/06—Organic material
- B01D71/08—Polysaccharides
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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
-
- 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
- B01D69/12—Composite membranes; Ultra-thin membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
Abstract
The invention provides the preparation method that a kind of bat calcium alginate gel compound is modified composite membrane, step is as follows：Step 1, configuration sodium alginate soln, add silicon ball and galapectite, and ultrasound is mixed, and obtains mixed liquor；Step 2, stainless (steel) wire impregnated in the mixed liquor, after the completion of dipping, rinsed, dried with distilled water；Step 3, step 2 is dried after sample impregnated in calcium chloride solution, after the completion of dipping, rinsed with distilled water, dry；The operation of step 4, repeat step 2 and step 3, obtains bat calcium alginate gel compound and is modified composite membrane.The present invention is by simply impregnating, sol-gal process, and SH CA gels are coated into stainless (steel) wire surface, coarse structure is constructed by organic inorganic hybridization.The method operating process is simple, and raw material is easy to get pollution-free.
Description
Technical field
The present invention relates to the preparation method and its usage that a kind of bat-calcium alginate gel compound is modified composite membrane, category
Technical field of environment function material preparation.
Background technology
From the point of view of universe, the earth is the celestial body of a sky blue, and its 72% area is covered with water.But in fact, the earth
Upper 97.5%
Water be salt water, the water that utilize of directly being produced and be lived by people is pitiably little, only 2.5% fresh water.Water
It is Source of life, is the necessity needed for human being's production life, but the oils and organic of human industry and life discharge
Pollutant seriously threatens water resource originally deficient on the earth, and this pollution mainly includes industry oil pollution and life greasy dirt
Dye.Industry oil pollution refers to the pollution of the oils and organic solvent that occur in the industrial production to water resource, it is well known that with
It is industrial to continue to develop, it is continuously increased needed for each industrial process with oil, these iundustrial oils have lubricating oil, oil emulsion, combustion
Oil etc. is expected, because the phenomenon such as run, drip, leak of iundustrial oil happens occasionally caused by miscarriage in use.2010
The petrochina Dalian Sea Area contamination accident in July in year, causes about 430 square kilometres of marine site oily wastewater pollutions of Dalian Bay, to the marine site
Seawer quality, the ecosystem and marine organisms all generate serious threat and influence.Life oily pollution refers to people daily
Discarded edible oil is dealt with improperly in life, the pollution caused in water is emitted into.Either industry oil pollution or life oil
Pollution, nowadays all seriously threatens the Nature ecological environment and the existence of the mankind.How oils and organic solvent efficiently handled
Pollution to water resource has caused social many-sided extensive concern.
The method of traditional processing oily wastewater pollution includes combustion method and fence absorption method.Wherein combustion method due to
Dangerous, poor controllability and the shortcomings of secondary pollution is caused to air is easily caused, so in recent years seldom by people
Use.And fence absorption method is widely used in processing oily wastewater pollution event in recent years as the method for most simple possible, turn round and look at
Name Si Yi, fence absorption method refers to set the oil fence to prevent oily diffusion in oily wastewater pollution region first, then using sorbing material
The oil in oil water mixture is absorbed, to reach the effect of water purifying.The key of this fence absorption method is adsorption material used
The physical and chemical performance and absorption property of material, the active charcoal of sorbing material, zeolite, the sponge nowadays commonly used etc..These materials
Loose structure ensure that it has adsorptivity, but absorption of this material to liquid is often no selective, so in processing
Often profit is inhaled together when oily wastewater pollution, and oil suction ratio is relatively low, and Oil Recovery difficulty is larger, and its own is unstable
Structure also broken cause secondary pollution.Therefore, a kind of profit with super wetting property and mechanical stability point is developed
It is urgent problem to be solved for processing oily wastewater pollution from material.
The process being found such as numerous scientific achievements, the discovery of super-hydrophobic phenomenon is also derived from people for Austria
The exploration of wonderful natural phenomena.A part of animals and plants in nature pass through the evolution of 1 years, in order to adapt to living environment,
Evolve and be provided with the surface of super wellability.As China Northern Song Dynasty composer of ci poetry Zhou Dunyi " goes out mud without dye, washed clear described in word work
Ripples is without goblin ", description be exactly lotus leaf surface in the Nature super-hydrophobic automatic cleaning surface performance, this phenomenon is referred to as
" lotus leaf effect (lotus-effect) ".Jiang Lei seminars are drawn by the sign observation analysis of the microstructure to lotus leaf surface
Conclusion：The coarse structure of the micro/nano level of lotus leaf surface and the material collective effect of low-surface-energy make it have super-hydrophobic automatic cleaning
Performance.In addition, substantial amounts of super-hydrophobic phenomenon, floral leaf piece (rice leaf, the rose of such as plant are also there is in nature
Piece etc.), the feather (goose, butterfly etc.) of animal, the leg of water skipper and the compound eye of mosquito etc..Water droplet is dropped in the floral leaf of above-mentioned plant
Above piece can rapid desufflation be spherical and quickly slide, the dust on surface etc. is taken away, with self-cleaning function；Butterfly's wing
Water droplet above can slide easily, in the rain wing can kept not drenched；And water skipper can be in the water surface
Move freely.Inspired by these natural phenomenas, people have developed various super infiltration functional materials, since super infiltration surface
Research occur since, a variety of materials with extreme wettable surfaces, which have succeeded, to be prepared by forefathers and is applied to water-oil separating
In.Extreme wettable surfaces applied to water-oil separating mainly include following two kinds：Super-hydrophobic/super-oleophilic material, it is super hydrophilic/
Superoleophobic material.
Preparing super-hydrophobic/super-oleophilic material needs in its surface construction coarse structure or uses low-surface energy substance to table
Face is modified, particularly as being：(1) coarse structure with certain roughness is constructed in material surface, then using low surface
Energy material is modified；(2) performance of super-hydrophobic/super-oleophilic is reached in low-surface energy substance surface construction coarse structure.
Because super-hydrophobic/super-oleophilic material is extremely to soak the functional material being developed earliest in Journal of Sex Research, so this kind of function
Material is also the functional material with super wellability surface being applied to earliest in water-oil separating.So far, researchers
To the research of super-hydrophobic/super-oleophilic material, convergence is ripe, and the functionalization material of many super-hydrophobic/super-oleophilics is successfully synthesized
Prepare.
But in the practical application for carrying out water-oil separating, super-hydrophobic/super-oleophilic material shows some and intrinsic lacked
Point：Using the mixture process of the super-hydrophobic/super-oleophilic functional material partition density organic solvent smaller than water or oil product and water
In easily cause the centre that water is blocked on oil product and super-hydrophobic/super-oleophilic water-oil separating material, hinder being normally carried out for separation；
The water-oil separating material of super-hydrophobic/super-oleophilic easily causes oil product in water-oil separating and separation material loose structure is blocked up
Plug, influences the separative efficiency and the rate of departure of water-oil separating, destroys its reusing.Opened by traditional oleophilic oil material
Hair, the water-oil separating material with superoleophobic/super hydrophilicity is increasingly becoming study hotspot.
The present invention utilizes sodium alginate and the gelation of calcium chloride reaction generation calcium alginate (Calcium Alginate)
Matter, while in stainless (steel) wire area load galapectite (Halloysite) and silicon ball (Silicon), constructing coarse surface knot
Structure, so that preparing super hydrophilic-bat-calcium alginate gel compound superoleophobic under water is modified composite membrane, for oil mixing with water
The processing of thing.
The content of the invention
The present invention relates to the preparation method and its usage that a kind of bat-calcium alginate gel compound is modified composite membrane, with
Sodium alginate, silicon ball, galapectite and calcium chloride be raw material, by simply impregnating, sol-gal process prepare bat-calcium alginate
Gel composite is modified composite membrane, and bat prepared by the method-calcium alginate gel compound, which is modified composite membrane, has excellent surpass
Hydrophilic-superoleophobic property, and different oil water mixtures being effectively separated under water.
The present invention is simply impregnated, sol-gal process is coated layer by layer in retinal surface using stainless (steel) wire as substrate by a step
Bat-calcium alginate gel, is successfully prepared bat-calcium alginate gel and is modified composite membrane, and use it for oil water mixture
Separation.
The present invention is achieved through the following technical solutions：
A kind of bat-calcium alginate gel compound is modified the preparation method of composite membrane, and step is as follows：
Step 1, configuration sodium alginate soln, add silicon ball and galapectite, and ultrasound is mixed, and obtains mixed liquor；
Step 2, stainless (steel) wire impregnated in the mixed liquor, after the completion of dipping, rinsed, dried with distilled water；
Step 3, step 2 is dried after sample impregnated in calcium chloride solution, after the completion of dipping, rinsed with distilled water,
Drying；
The operation of step 4, repeat step 2 and step 3, obtains bat-calcium alginate gel compound and is modified composite membrane, note
Composite membrane is modified for SH-CA gels.
In step 1, in the mixed liquor, the concentration of the sodium alginate is 0.1~1.0mg/mL, and the concentration of silicon ball is
1.0~5.0mg/mL, the concentration of galapectite is 1.0~5.0mg/mL.
In step 2, the stainless (steel) wire mesh number is 200~1000, and the dip time is 0.5~1.0min.
In step 3, the concentration of the calcium chloride solution is 1.0~5.0mg/mL, and the dip time is 10~30s.
In step 4, the number of operations of the repeat step 2 and step 3 is 5-15 times.
In step 2,3, the drying temperature is 40~50 DEG C, and the time is 1~3min.
Described bat-calcium alginate gel compound is modified composite membrane and carries out oil water mixture separation.
Beneficial effect：
(1) present invention by simply impregnating, sol-gal process, SH-CA gels are coated to stainless (steel) wire surface, by having
Machine-inorganic hybridization constructs coarse structure.The method operating process is simple, and raw material is easy to get pollution-free.
(2) when being separated using SH-CA gels modification composite membrane to oil water mixture, with good separating effect,
And a variety of oil water mixtures can be separated.
(3) SH-CA gels are modified compound membrane stability height, and can be recycled for multiple times, and are 1 to 100mL volume ratios：1
Oil water mixture separate 10 times after, still keep good oil-water separation.
Brief description of the drawings
Fig. 1 is the SEM figures that pure stainless steel nethike embrane (a) is modified composite membrane (b-d) with the SH-CA gels in embodiment 4.
Fig. 2 is the angle of the droplets contact under water schematic diagram of embodiment 4.
Embodiment
In order to illustrate technical scheme and technical purpose, below in conjunction with the accompanying drawings and specific embodiment is done to the present invention
It is further to introduce.
Embodiment 1：
Step 1：
The mixed solution of 20mL sodium alginates, silicon ball and galapectite is configured, sodium alginate concentration is 0.1mg/mL, and silicon ball is dense
Spend for 1.0mg/mL, galapectite concentration is 1.0mg/mL, and 200 mesh stainless (steel) wires are impregnated in mixed solution, react 0.5min,
Rinsed with distilled water；In the calcium chloride solution for immersing 1.0mg/mL, 10s is impregnated, is rinsed again with distilled water, is put into 40 DEG C of baking
1min is dried in case；Repeat the above steps 5 times, bat-calcium alginate gel compound is made and is modified composite membrane, SH- is designated as
CA5- 1 gel is modified composite membrane.
Step 2：
By obtained SH-CA5- 1 gel is modified composite membrane and is fixed to homemade oily-water seperating equipment, will with a small amount of distilled water
Retinal surface is soaked, and is then 1 by 100mL volume ratios：1 hexamethylene and the mixed solution of water are poured into the device put up.For
More accurately determine the water-oil separating efficiency of composite membrane, sample is divided into 3 parts, and each sample test 3 times.Entirely tested
Journey is carried out under gravity condition.Water-oil separating efficiency is calculated as follows：
Wherein R is separative efficiency, M0And MpThe weight of oil before and after respectively separating.
Test result indicates that SH-CA5- 1 gel, which is modified composite membrane, has excellent water-oil separating performance, and its separative efficiency reaches
To 98.5%.
Embodiment 2：
Step 1：
The mixed solution of 20mL sodium alginates, silicon ball and galapectite is configured, sodium alginate concentration is 0.5mg/mL, and silicon ball is dense
Spend for 3.0mg/mL, galapectite concentration is 3.0mg/mL, and 300 mesh stainless (steel) wires are impregnated in mixed solution, react 0.5min,
Rinsed with distilled water；In the calcium chloride solution for immersing 3.0mg/mL, 10s is impregnated, is rinsed again with distilled water, is put into 40 DEG C of baking
1min is dried in case；Repeat the above steps 5 times, bat-calcium alginate gel compound is made and is modified composite membrane, 3SH- is designated as
CA5- 5 gels are modified composite membrane.
Step 2：
By obtained 3SH-CA5- 5 gels are modified composite membrane and are fixed to homemade oily-water seperating equipment, according in embodiment 1
The operation of step 2 carries out water-oil separating experiment, and hexamethylene-aqueous mixtures, experimental result table are replaced with toluene-water oil water mixture
Bright water-oil separating efficiency is 99.0%.
Embodiment 3：
Step 1：
The mixed solution of 20mL sodium alginates, silicon ball and galapectite is configured, sodium alginate concentration is 0.7mg/mL, and silicon ball is dense
Spend for 3.0mg/mL, galapectite concentration is 3.0mg/mL, and 300 mesh stainless (steel) wires are impregnated in mixed solution, react 0.5min,
Rinsed with distilled water；In the calcium chloride solution for immersing 3.0mg/mL, 10s is impregnated, is rinsed again with distilled water, is put into 40 DEG C of baking
1min is dried in case；Repeat the above steps 10 times, bat-calcium alginate gel compound is made and is modified composite membrane, 3SH- is designated as
CA10- 7 gels are modified composite membrane.
Step 2：
By obtained 3SH-CA10- 7 gels are modified composite membrane and are fixed to homemade oily-water seperating equipment, according in embodiment 1
The operation of step 2 carries out water-oil separating experiment, test result indicates that water-oil separating efficiency is 99.2%.
Embodiment 4：
Step 1：
The mixed solution of 30mL sodium alginates, silicon ball and galapectite is configured, sodium alginate concentration is 0.7mg/mL, and silicon ball is dense
Spend for 5.0mg/mL, galapectite concentration is 5.0mg/mL, and 300 mesh stainless (steel) wires are impregnated in mixed solution, react 1.0min,
Rinsed with distilled water；In the calcium chloride solution for immersing 5.0mg/mL, 10s is impregnated, is rinsed again with distilled water, is put into 40 DEG C of baking
1min is dried in case；Repeat the above steps 15 times, bat-calcium alginate gel compound is made and is modified composite membrane, 5SH- is designated as
CA15- 7 gels are modified composite membrane.
Step 2：
By obtained 5SH-CA15- 7 gels are modified composite membrane film and are fixed to homemade oily-water seperating equipment, according to embodiment 1
The operation of middle step 2 carries out water-oil separating experiment, test result indicates that water-oil separating efficiency is 99.6%.
Fig. 1 is the SEM figures that pure stainless steel nethike embrane (a) is modified composite membrane (b-d) with the SH-CA gels in embodiment 4, from figure
In it can be seen that bat gel successfully load to stainless (steel) wire surface.
Fig. 2 is the angle of the droplets contact under water schematic diagram of embodiment 4, and the contact angle that SH-CA gels are modified composite membrane reaches
152o。
Embodiment 5：
Step 1：
The mixed solution of 40mL sodium alginates, silicon ball and galapectite is configured, sodium alginate concentration is 1.0mg/mL, and silicon ball is dense
Spend for 5.0mg/mL, galapectite concentration is 5.0mg/mL, and 1000 mesh stainless (steel) wires are impregnated in mixed solution, react
1.0min, is rinsed with distilled water；In the calcium chloride solution for immersing 5.0mg/mL, 30s is impregnated, is rinsed, is put into distilled water again
3min is dried in 50 DEG C of baking oven；Repeat the above steps 15 times, bat-calcium alginate gel compound be made and is modified composite membrane,
It is designated as 5SH-CA15- 7 gels are modified composite membrane.
Step 2：
By obtained 5SH-CA15- 7 gels are modified composite membrane and are fixed to homemade oily-water seperating equipment, according in embodiment 1
The operation of step 2 carries out water-oil separating experiment, test result indicates that water-oil separating efficiency is 99.1%.
Claims (7)
1. a kind of bat-calcium alginate gel compound is modified the preparation method of composite membrane, it is characterised in that step is as follows：
Step 1, configuration sodium alginate soln, add silicon ball and galapectite, and ultrasound is mixed, and obtains mixed liquor；
Step 2, stainless (steel) wire impregnated in the mixed liquor, after the completion of dipping, rinsed, dried with distilled water；
Step 3, step 2 is dried after sample impregnated in calcium chloride solution, after the completion of dipping, rinsed with distilled water, dry；
The operation of step 4, repeat step 2 and step 3, obtains bat-calcium alginate gel compound and is modified composite membrane.
2. a kind of bat according to claim 1-calcium alginate gel compound is modified the preparation method of composite membrane, it is special
Levy and be, in step 1, in the mixed liquor, the concentration of the sodium alginate is 0.1~1.0mg/mL, and the concentration of silicon ball is 1.0
~5.0mg/mL, the concentration of galapectite is 1.0~5.0mg/mL.
3. a kind of bat according to claim 1-calcium alginate gel compound is modified the preparation method of composite membrane, it is special
Levy and be, in step 2, the stainless (steel) wire mesh number is 200~1000, and the dip time is 0.5~1.0min.
4. a kind of bat according to claim 1-calcium alginate gel compound is modified the preparation method of composite membrane, it is special
Levy and be, in step 3, the concentration of the calcium chloride solution is 1.0~5.0mg/mL, and the dip time is 10~30s.
5. a kind of bat according to claim 1-calcium alginate gel compound is modified the preparation method of composite membrane, it is special
Levy and be, in step 4, the number of operations of the repeat step 2 and step 3 is 5-15 times.
6. a kind of bat according to claim 1-calcium alginate gel compound is modified the preparation method of composite membrane, it is special
Levy and be, in step 2,3, the drying temperature is 40~50 DEG C, and the time is 1~3min.
7. a kind of bat-calcium alginate gel compound described in claim 1~6 any one is modified the preparation side of composite membrane
Bat prepared by method-calcium alginate gel compound, which is modified composite membrane, is used for the purposes that oil water mixture is separated.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112107887A (en) * | 2020-08-26 | 2020-12-22 | 广东工业大学 | Underwater super-oleophobic oil-water separation material and preparation method and application thereof |
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| CN102049204A (en) * | 2011-01-17 | 2011-05-11 | 郑州大学 | Metal ion-carried nerchinskite nano tube/polyether sulfone hybridized antibacterial membrane and preparation method thereof |
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