CN107376665A - A kind of preparation method of chitosan-based organic inorganic hybridization porous membrane - Google Patents
A kind of preparation method of chitosan-based organic inorganic hybridization porous membrane Download PDFInfo
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- CN107376665A CN107376665A CN201710823618.1A CN201710823618A CN107376665A CN 107376665 A CN107376665 A CN 107376665A CN 201710823618 A CN201710823618 A CN 201710823618A CN 107376665 A CN107376665 A CN 107376665A
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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
-
- 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
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- 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
Abstract
A kind of preparation method of chitosan-based organic inorganic hybridization porous membrane, is related to heavy metal ion-containing waste water processing technology field.The present invention is using CS and amino silicane coupling agent as primary raw material, add appropriate pore creating material NaCl, premixed through solution, solgel reaction in situ, casting film-forming, natural air drying, base extraction, washing, a series of processes such as drying, chitosan-based organic inorganic hybridization porous membrane is made.The present invention by CS and amino silicane coupling agent it is hybrid cross-linked after, the dissolubility of CS in acid waste water can not only be suppressed, while introduce amino, increase the adsorption site position to metal ion, it is possible to achieve such as absorption of chromium, lead, cadmium ion in waste water.Moreover, the hybridization porous film after absorption can reuse after regeneration treatment, adsorption effect is not decreased obviously.
Description
Technical field
The present invention relates to heavy metal ion-containing waste water processing technology field, is specifically related to a kind of chitosan-based organic-nothing
The preparation method of the hybridization porous film of machine.
Background technology
With the fast development of China's economic, all there is more serious water to varying degrees for China most cities
Body pollution problem.Industrial wastewater that is many unprocessed or dealing with improperly is directly discharged into rivers and lakes, causes natural water tight
Heavily contaminated, contents of heavy metal elements therein have ascendant trend year by year, the ecological safety in serious threat China.In water body, weight
Even if metal ion concentration very little, can also be deposited in algae and bed mud, utilized and accumulated by aquatiles such as fish and shellfishes,
Food chain concentration is produced, directly threatens higher organism to include the mankind.Therefore, the removal of Heavy Metals in Waters ion turns into research
Focus.
Research shows that CS (chitosan) and CS derivative heavy metal ions have good suction-operated.However, pure CS
It is easily soluble in in the acid waste water containing heavy metal ion, while adsorbing metal ions, is dissolved in the water again, can neither
Heavy metal ion is removed, introduces new pollution again, therefore pure CS can not meet absorption containing heavy metal ion requirement.
But by CS by with after silane coupler hydridization, forming cross-linked network molecule, original adsorptivity can be kept
Can, and it is not soluble in water.Donghua University Ph.D. Dissertation --- the preparation of chitosan-based hybrid organic-inorganic film and its application
It can be disclosed in research：1. nano silicon, chitosan and vinylsiloxane using blending method can be made chitosan/
Improved silica nano hybrid film.The hybridized film can be with the dyestuff in adsorbent solution, but can not adsorb heavy metal ion.②
Using chitosan and carboxymethyl cellulose blending as organic matrix, with silicone couplet γ-glycidyl ether oxygen propyl trimethoxy
Silane prepares organic and inorganic chitosan/carboxymethyl cellulose/silicon composite hybridization film as crosslinking agent by solution blended process.
The composite hybridization film can adsorb dichromate ion.3. using aldehyde functions and amido functional group schiff base reaction, in shell
Chitosan/dialdehyde starch/silicon hybridization film is made in hinge in glycan acid solution.The hybridized film can adsorb dyestuff.
Using the relevant report of chitosan derivatives adsorbing separation heavy metal ions in wastewater, so far there are no.
The content of the invention
It is an object of the invention to provide a kind of preparation of the simply chitosan-based hybrid inorganic-organic porous membrane of method
Method, obtained hybridization porous film have high absorption property, are the adsorbing and removing and recovery profit of heavy metal ions in wastewater
With a kind of new approach of offer.
To achieve these goals, the technical solution adopted in the present invention is：
A kind of preparation method of chitosan-based hybrid inorganic-organic porous membrane, specific preparation process are as follows：
1., prepare coating liquid
20g chitosan (CS) is weighed, is dissolved in the acetic acid solution that 1000mL percents by volume are 2%；4g is weighed again
NaCl powders add into solution, stirring and dissolving, stand defoaming, obtain A liquid；
25mL amino silicane coupling agent is measured, adds into 100mL absolute ethyl alcohol, stirs, obtains B liquid；
B liquid is slowly dropped in A liquid, at room temperature stirring reaction 4h, stands defoaming and obtain coating liquid；
2., prepare hybridized film
The solution after standing is drawn, is poured into the glass separate slot of clean dry, casting film-forming, natural air drying produces hydridization
Film；
3., prepare hybrid inorganic-organic perforated membrane
Hybridized film is added into 5% NaOH solution and soaks 4h, takes out film, then 4h is soaked in water, is then taken out
Dried in 60 DEG C of baking ovens, produce hybrid inorganic-organic porous membrane.
The present invention adds appropriate pore creating material NaCl using CS and amino silicane coupling agent as primary raw material, premixed through solution,
A series of processes such as sol gel reaction in situ, casting film-forming, natural air drying, base extraction, washing, drying, chitosan is made
The hybridization porous film of base organic-inorganic.
(such as γ-diethylenetriamine hydroxypropyl methyl dimethoxysilane is (referred to as with amino silicane coupling agent by CS by the present invention
KH-603), N- aminoethyls-gamma-aminopropyl-triethoxy-silane (abbreviation KH-791), N- (β-aminoethyl)-γ-aminopropyl front three
TMOS (abbreviation KH-792)) it is hybrid cross-linked after, the dissolubility of CS in acid waste water can not only be suppressed, while introduce amino,
Increase the adsorption site position to metal ion, it is possible to achieve such as absorption of chromium, lead, cadmium ion in waste water.It is moreover, miscellaneous after absorption
Changing perforated membrane can be reused after regeneration treatment, and adsorption effect is not decreased obviously.
Relative to prior art, beneficial effects of the present invention performance is as follows：
1) NaCl, is added in sol-gel process, obtained film can obtain porous membrane, will increase thin through washing
The specific surface area of film, significantly increase the adsorption effect of film heavy metal ion.
2), obtained film can promote hybridized film to solidify, it is no longer dissolved in the water, not even through base extraction
It is dissolved in acidic aqueous solution, this is highly beneficial to processing acidic industrial effluent.
3), technique is simple, energy-conserving and environment-protective, raw material are cheap and easy to get.Technological process is short, and step is few, without using harmful organic
Solvent, all processes are carried out at room temperature.Film after use is renewable, is used for multiple times.
Brief description of the drawings
Preparation method with accompanying drawing to the chitosan-based hybrid inorganic-organic porous membrane of the present invention with reference to embodiments
Make and being discussed further.
The step of Fig. 1 is embodiment 1 1. used in chitosan (CS) raw material field emission scanning electron microscope
(FE-SEM) photo；
The step of Fig. 2 is embodiment 1 2. in the field emission scanning electron microscope (FE-SEM) of prepared hybridized film shine
Piece；
The step of Fig. 3 is embodiment 1 3. in prepared hybrid inorganic-organic perforated membrane Flied emission scanning electron microscopy
Mirror (FE-SEM) photo.
Embodiment
Embodiment 1
A kind of preparation method of chitosan-based hybrid inorganic-organic porous membrane, specific preparation process are as follows：
1., prepare coating liquid
20g chitosan (CS) is weighed, is dissolved in the acetic acid solution that 1000mL percents by volume are 2%.4g is weighed again
NaCl powders add into solution, stirring and dissolving, stand defoaming, obtain A liquid.
25mL γ-diethylenetriamine hydroxypropyl methyl dimethoxysilane (abbreviation KH-603) is measured, is added to 100mL's
In absolute ethyl alcohol, stir, obtain B liquid.
B liquid is slowly dropped in A liquid, at room temperature stirring reaction 4h, stands defoaming and obtain coating liquid.
2., prepare hybridized film
The solution after standing is drawn, is poured into the glass separate slot of clean dry, casting film-forming, natural air drying produces hydridization
Film.
3., prepare hybrid inorganic-organic perforated membrane
Hybridized film is added into 5% NaOH solution and soaks 4h, takes out film, then 4h is soaked in water, is then taken out
Dried in 60 DEG C of baking ovens, produce hybrid inorganic-organic porous membrane.
As shown in Figure 1, pure CS surface is smooth, and hybridized film (not washing away NaCl) rough surface is (such as Fig. 2 institutes
Show) because CS is reacted with silane coupler, cross-linked network structure is formed, and produce certain phase separation.And add
Enter the hybridized film and after washing after NaCl immersions, the hole showed increased (as shown in Figure 3) of film, form hybridization porous
Film.The hybridization porous film prepared has larger specific surface area, adds the point position of hybridized film adsorbing metal ions.
The hybridization porous film being prepared in the present embodiment is placed on to 100mg/L Cr (NO3)3Water is removed in solution
The Adsorption experiment of middle trivalent chromic ion.Experimentation is as follows：The above-mentioned hybridization porous films being prepared of 1g are weighed to be placed in
In 100mL conical flask, 100mg/L Cr (NO are then pipetted3)3Solution 50mL is soaked to it, then they are collectively disposed at
12h is adsorbed in 25 DEG C of insulating box, is then filtered out from conical flask sample with funnel, is used to test after collecting filtrate.Pass through
Before Atomic Absorption Spectrometer detection absorption after the concentration of original solution and absorption in remaining filtrate trivalent chromic ion concentration, by
This can calculate Cr3+Adsorbance on hybridization porous film.Test result indicates that：Hybridization porous film pair manufactured in the present embodiment
Cr3+Adsorbance is 1.2mg/g, therefore prepares hybridization porous film and can adsorb chromium ion in waste water solution.
Embodiment 2
A kind of preparation method of chitosan-based hybrid inorganic-organic porous membrane, specific preparation process are as follows：
1., prepare coating liquid
20g chitosan (CS) is weighed, is dissolved in the acetic acid solution that 1000mL percents by volume are 2%.4g is weighed again
NaCl powders add into solution, stirring and dissolving, stand defoaming, obtain A liquid.
25mL N- aminoethyls-gamma-aminopropyl-triethoxy-silane (abbreviation KH-791) is measured, is added to 100mL nothing
In water-ethanol, stir, obtain B liquid.
B liquid is slowly dropped in A liquid, at room temperature stirring reaction 4h, stands defoaming and obtain coating liquid.
2., prepare hybridized film
The solution after standing is drawn, is poured into the glass separate slot of clean dry, casting film-forming, natural air drying produces hydridization
Film.
3., prepare hybrid inorganic-organic perforated membrane
Hybridized film is added into 5% NaOH solution and soaks 4h, takes out film, then 4h is soaked in water, is then taken out
Dried in 60 DEG C of baking ovens, produce hybrid inorganic-organic porous membrane.
The hybridization porous film being prepared in the present embodiment is placed on to 100mg/L Cr (NO3)3Water is removed in solution
The Adsorption experiment of middle trivalent chromic ion.Experimentation is the same as embodiment 1.Test result indicates that：Hydridization manufactured in the present embodiment
Perforated membrane is to Cr3+Adsorbance is 1.0mg/g, therefore prepares hybridization porous film and can adsorb chromium ion in waste water solution.
Embodiment 3
A kind of preparation method of chitosan-based hybrid inorganic-organic porous membrane, specific preparation process are as follows：
1., prepare coating liquid
20g chitosan (CS) is weighed, is dissolved in the acetic acid solution that 1000mL percents by volume are 2%.4g is weighed again
NaCl powders add into solution, stirring and dissolving, stand defoaming, obtain A liquid.
25mL N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane (abbreviation KH-792) is measured, is added to 100mL
Absolute ethyl alcohol in, stir, obtain B liquid.
B liquid is slowly dropped in A liquid, at room temperature stirring reaction 4h, stands defoaming and obtain coating liquid.
2., prepare hybridized film
The solution after standing is drawn, is poured into the glass separate slot of clean dry, casting film-forming, natural air drying produces hydridization
Film.
3., prepare hybrid inorganic-organic perforated membrane
Hybridized film is added into 5% NaOH solution and soaks 4h, takes out film, then 4h is soaked in water, is then taken out
Dried in 60 DEG C of baking ovens, produce hybrid inorganic-organic porous membrane.
The hybridization porous film being prepared in the present embodiment is placed on to 100mg/L Pb (NO3)2Water is removed in solution
The Adsorption experiment of middle lead (II) ion.Experimentation is as follows：The above-mentioned hybridization porous films being prepared of 1g are weighed to be placed in
In 100mL conical flask, 100mg/L Pb (NO are then pipetted3)2Solution 50mL is soaked to it, then they are collectively disposed at
12h is adsorbed in 25 DEG C of insulating box, is then filtered out from conical flask sample with funnel, is used to test after collecting filtrate.Pass through
Before Atomic Absorption Spectrometer detection absorption after the concentration of original solution and absorption in remaining filtrate lead (II) ion concentration, by
This can calculate Pb2+Adsorbance on hybridization porous film.Test result indicates that：Hybridization porous film pair manufactured in the present embodiment
Pb2+Adsorbance is 1.5mg/g, therefore prepares hybridization porous film and can adsorb lead ion in waste water solution.
Above content is only to design example and explanation of the invention, affiliated those skilled in the art
Various modifications or supplement are made to described specific embodiment or is substituted using similar mode, without departing from invention
Design or surmount scope defined in the claims, protection scope of the present invention all should be belonged to.
Claims (2)
1. a kind of preparation method of chitosan-based hybrid inorganic-organic porous membrane, it is characterised in that specific preparation process is such as
Under：
1., prepare coating liquid
20g chitosan (CS) is weighed, is dissolved in the acetic acid solution that 1000mL percents by volume are 2%；Weigh 4g's again
NaCl powders are added into solution, stirring and dissolving, are stood defoaming, are obtained A liquid；
25mL amino silicane coupling agent is measured, adds into 100mL absolute ethyl alcohol, stirs, obtains B liquid；
B liquid is slowly dropped in A liquid, at room temperature stirring reaction 4h, stands defoaming and obtain coating liquid；
2., prepare hybridized film
The solution after standing is drawn, is poured into the glass separate slot of clean dry, casting film-forming, natural air drying produces hybridized film；
3., prepare hybrid inorganic-organic perforated membrane
Hybridized film is added into 5% NaOH solution and soaks 4h, takes out film, then 4h is soaked in water, is then taken out in 60
Dried in DEG C baking oven, produce hybrid inorganic-organic porous membrane.
2. preparation method as claimed in claim 1, it is characterised in that 1. middle amino silicane coupling agent is γ-divinyl to step
Triamine hydroxypropyl methyl dimethoxysilane, N- aminoethyls-gamma-aminopropyl-triethoxy-silane, N- (β-aminoethyl)-γ-ammonia third
One or more mixtures in base trimethoxy silane.
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Cited By (8)
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| CN108250421A (en) * | 2018-01-19 | 2018-07-06 | 郭涛 | A kind of Degradable environment-friendlyplastic plastic film and preparation method thereof |
| CN110600672A (en) * | 2019-08-07 | 2019-12-20 | 华南师范大学 | Flexible self-supporting three-dimensional porous electrode and preparation method thereof |
| CN111495333A (en) * | 2019-07-18 | 2020-08-07 | 河北燕岛环保科技股份有限公司 | Preparation method of composite membrane capable of adsorbing heavy metals and organic pollutants |
| CN111821954A (en) * | 2020-07-25 | 2020-10-27 | 合肥学院 | Preparation method and application of hybrid membrane adsorbent for removing nickel ions in water |
| CN111974355A (en) * | 2020-07-13 | 2020-11-24 | 广西科技大学 | Chitosan/fibroin-based dual-structure porous adsorption filter material with silicon dioxide as pore-foaming agent and preparation method thereof |
| CN114307669A (en) * | 2021-12-01 | 2022-04-12 | 佛山市南海区苏科大环境研究院 | Water-soluble aldehyde starch-polyethyleneimine coating modified polymer film and preparation method thereof |
| CN114307667A (en) * | 2021-12-01 | 2022-04-12 | 佛山市南海区苏科大环境研究院 | Water-soluble aldehyde-based cyclodextrin-polyethyleneimine coating modified polymer film and preparation method thereof |
| CN114752002A (en) * | 2022-04-06 | 2022-07-15 | 东莞理工学院 | Organic modified chitosan adsorbent for removing PFASs, preparation method and application |
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| CN111495333A (en) * | 2019-07-18 | 2020-08-07 | 河北燕岛环保科技股份有限公司 | Preparation method of composite membrane capable of adsorbing heavy metals and organic pollutants |
| CN110600672A (en) * | 2019-08-07 | 2019-12-20 | 华南师范大学 | Flexible self-supporting three-dimensional porous electrode and preparation method thereof |
| CN111974355A (en) * | 2020-07-13 | 2020-11-24 | 广西科技大学 | Chitosan/fibroin-based dual-structure porous adsorption filter material with silicon dioxide as pore-foaming agent and preparation method thereof |
| CN111821954A (en) * | 2020-07-25 | 2020-10-27 | 合肥学院 | Preparation method and application of hybrid membrane adsorbent for removing nickel ions in water |
| CN114307669A (en) * | 2021-12-01 | 2022-04-12 | 佛山市南海区苏科大环境研究院 | Water-soluble aldehyde starch-polyethyleneimine coating modified polymer film and preparation method thereof |
| CN114307667A (en) * | 2021-12-01 | 2022-04-12 | 佛山市南海区苏科大环境研究院 | Water-soluble aldehyde-based cyclodextrin-polyethyleneimine coating modified polymer film and preparation method thereof |
| CN114307667B (en) * | 2021-12-01 | 2024-03-15 | 苏州科技大学 | Water-soluble aldehyde cyclodextrin-polyethyleneimine coating modified polymer film and preparation method thereof |
| CN114307669B (en) * | 2021-12-01 | 2024-03-15 | 苏州科技大学 | Water-soluble aldehyde starch-polyethyleneimine coating modified polymer film and preparation method thereof |
| CN114752002A (en) * | 2022-04-06 | 2022-07-15 | 东莞理工学院 | Organic modified chitosan adsorbent for removing PFASs, preparation method and application |
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