CN111375357A - Preparation method of multifunctional nano aerogel with amphipathy - Google Patents
Preparation method of multifunctional nano aerogel with amphipathy Download PDFInfo
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- CN111375357A CN111375357A CN202010264807.1A CN202010264807A CN111375357A CN 111375357 A CN111375357 A CN 111375357A CN 202010264807 A CN202010264807 A CN 202010264807A CN 111375357 A CN111375357 A CN 111375357A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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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
- 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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/268—Polymers created by use of a template, e.g. molecularly imprinted polymers
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- 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
- B01J20/28047—Gels
Abstract
The invention discloses a preparation method of multifunctional nano aerogel with amphipathy, which is characterized in that gelatin is used as a framework to construct a 3D porous aerogel material, the material obtains special wetting characteristics through embedding of titanium dioxide and silicon dioxide nanoparticles, oil-water mixtures with different components and specific gravity can be selectively separated by utilizing the super-oleophobic or super-hydrophobic characteristics of the material, and meanwhile, the application of an ion imprinting technology and a grafting modification technology realizes functional expansion of the material, so that toxic metal ions and organic pollutants in oil-containing wastewater can be adsorbed in a targeted manner. The prepared aerogel is a functional nano material integrating efficient oil-water separation and targeted pollutant adsorption, has the advantages of reusability, natural degradation, strong oil stain resistance, good acid-base tolerance and the like, can separate complex oil-water mixtures and highly emulsified emulsions, has the oil-water separation efficiency of up to 99.7 percent, and can be applied to purification and treatment of various oily wastewater.
Description
Technical Field
The invention relates to a preparation method of nano aerogel, in particular to a preparation method of multifunctional nano aerogel with amphipathy. Belongs to the technical field of environment functional nano materials.
Background
With the rapid development of industry and the rapid growth of population, a large amount of oily wastewater with complex components is discharged into the ecological environment, causing destructive influence on the environment. Oily wastewater poses a great threat to aquatic organisms and water safety and brings challenges to human survival. Meanwhile, the existence of high-toxicity heavy metal ions and difficult-to-degrade organic pollutants increases the difficulty in treating the oily wastewater. The traditional method for purifying the oily wastewater comprises gravity separation, filtration, flocculation, flotation, adsorption, biodegradation and the like. However, although these methods are simple to operate, they have problems of low separation efficiency, large occupied space, poor oil/water selectivity, difficulty in reuse/recycle, low adsorption capacity, secondary pollution, etc. which limit their large-scale application. At present, the porous material is considered to be an effective, environment-friendly, simple and recyclable method for oil-water separation.
Aerogels are typically three-dimensional porous materials that are considered to be one of the most attractive oil-water separation materials due to their low density, large surface area, high porosity, greater adsorption capacity, self-supporting structure and good mechanical properties. Chinese patent CN109929134A discloses an intrinsic hydrophobic polyimide aerogel, a preparation method and application thereof, and water-in-oil emulsion separation is realized by utilizing high hydrophobicity. Chinese patent CN107364871A discloses a super-hydrophobic silica aerogel micro-powder, a preparation method and application thereof, and the super-hydrophobic silica aerogel micro-powder is prepared by using surface hydrophobic modification to realize oil-water separation. However, the surface of the aerogel material with single wetting property is easily polluted by high-viscosity oil and corroded by alkaline solution, and then the original super-hydrophobic property is lost in the oil-water separation process. And most of traditional aerogel materials are prepared from inorganic matters and petroleum-based organic matters, are difficult to biodegrade and recycle, and easily cause secondary pollution to the environment.
Gelatin is a widely used biological protein, widely found in animal skin, bone and bone marrow. Gelatin has been widely used in the food, chemical engineering and pharmaceutical industries due to its low cost, easy extraction, biocompatibility and biodegradability. The gelatin has abundant hydroxyl, carboxyl and amino in molecular chains, so that the gelatin is easy to functionalize materials and adsorb pollutants. The gelatin is used as a framework to construct the 3D porous structure material, so that the development of the aerogel material integrating oil/water separation and pollutant adsorption has important research significance and application value.
Disclosure of Invention
Aiming at the technical problems, the invention provides a preparation method of multifunctional gelatin nano aerogel with amphipathy. The aerogel material regulates and controls the surface wetting property of the material through nanoparticles, can selectively separate oil-water mixtures with different components and specific gravity by utilizing the super-oleophobic property in water and the super-hydrophobic property in oil, and can remove toxic metal ions and organic pollutants in oily wastewater in a targeted manner by utilizing an ion imprinting technology and a grafting modification technology, thereby realizing the oily wastewater purification technology integrating oil-water separation and pollutant adsorption.
The technical scheme of the invention is as follows:
a preparation method of multifunctional nano aerogel with amphipathy comprises the following steps:
a) dissolving gelatin in water under the condition of continuous stirring to obtain a uniform gelatin aqueous solution with the gelatin mass fraction of 4-8%, adding nano titanium dioxide and nano silicon dioxide into the prepared gelatin aqueous solution, and performing ultrasonic dispersion to obtain a milky suspension; wherein, the mass fraction of the nano titanium dioxide in the suspension is 0.1-0.3 wt%, and the mass fraction of the nano silicon dioxide in the suspension is 0.1-0.5 wt%;
b) pouring the suspension obtained in the step a) into a mold, gelatinizing at low temperature, and then immersing the suspension into an excessive ammonium salt aqueous solution for curing to obtain stable high-elasticity gelatin nano hydrogel;
c) immersing the gelatin nano hydrogel obtained in the step b) into excessive metal ion solution for ion imprinting functionalization modification, continuously stirring, and then carrying out weak acid washing on the gelatin nano hydrogel taken out of the metal ion solution to obtain the ion imprinting functionalization nano hydrogel;
d) adding the ion-imprinted functionalized gelatin nano hydrogel obtained in the step c) and a cross-linking agent into a polyethyleneimine aqueous solution for functional grafting modification to obtain a multifunctional nano hydrogel, wherein the mass percentage concentration of the polyethyleneimine aqueous solution is 3-5%; the mass ratio of the gelatin nano hydrogel to the cross-linking agent to the polyethyleneimine aqueous solution is 1:0.01: 1.1;
e) and d) carrying out freeze drying treatment on the multifunctional nano-hydrogel prepared in the step d) to obtain the ultralight, porous and amphiphilic multifunctional nano-aerogel.
The preparation method of the multifunctional nano aerogel with amphipathy comprises the following steps of a), stirring at the temperature of 50-60 ℃; the size of the nano titanium dioxide particles is 20-40nm, and the size of the nano silicon dioxide particles is 30-40 nm; the ultrasonic dispersion time is 6-8h, and the temperature is 60-70 ℃.
The preparation method of the multifunctional gelatin nano aerogel with amphipathy comprises the step b), wherein the concentration of the ammonium salt water solution is 20-40 wt%, the ammonium salt is any one or more of ammonium sulfate, ammonium chloride, ammonium nitrate and ammonium carbonate, and the curing time is 20-28 hours.
The preparation method of the multifunctional nano aerogel with amphipathy comprises the step of c), wherein metal ions in the metal ion solution in the step of c) are any one of copper ions, nickel ions, chromium ions, lead ions, cadmium ions, manganese ions and cobalt ions, and the concentration of the metal ions is 30-150 mg/L.
The preparation method of the multifunctional nano aerogel with amphipathy comprises the step d), wherein the cross-linking agent is any one of formaldehyde, glutaraldehyde, genipin and epichlorohydrin.
The preparation method of the multifunctional gelatin nano aerogel with amphipathy comprises the following steps of (a) carrying out freeze drying in step e) under vacuum for 24-48 h; the obtained multifunctional gelatin nano aerogel is a three-dimensional porous aerogel with a layered structure, the aperture is 2-50nm, and the density is 0.1-0.3g/cm3The porosity is 75-90%.
The amphiphilic multifunctional gelatin nano aerogel prepared by the invention has the following amphipathy: the multifunctional gelatin nano aerogel shows super-wetting characteristics in air, and the contact angles of a water phase and an oil phase are both less than 0 degree; the multifunctional nano aerogel shows super-oleophobic property after being wetted by water phase, and the contact angle of oil phase is larger than 135 degrees; the multifunctional nano aerogel shows super-hydrophobicity after being wetted by the oil phase, and the contact angle of the water phase is larger than 135 degrees.
Compared with the prior art, the invention has the following outstanding advanced technologies:
1. the aerogel material prepared by the invention has high-efficiency oil-water separation performance and can selectively separate an oil-water mixture.
2. The aerogel material prepared by the invention is a nano porous material, has small density, light weight, flame resistance and high stability, can be repeatedly utilized, can be degraded in a natural environment, and cannot cause secondary pollution.
3. The aerogel material prepared by the invention can treat oily wastewater with complex components, and is a functional nano material integrating efficient oil-water separation and targeted pollutant adsorption.
4. The aerogel material prepared by the invention can resist oil pollution due to the special double-wetting characteristic, can separate highly emulsified emulsion, has good tolerance to acid and alkali, and has the oil-water separation efficiency as high as 99.7%.
Drawings
FIG. 1 is a SEM schematic diagram of a multifunctional nano aerogel prepared by the invention
FIG. 2 is a schematic view of an oil-water separator used in the present invention
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used are not indicated by the manufacturer and are all commercially available.
The features and properties of the present invention are further described in detail in the following examples
Detailed description of the preferred embodiment 1
A preparation method of multifunctional gelatin nano aerogel with amphipathy comprises the following steps:
a) dissolving 10g of gelatin in 190g of water at 50 ℃ under continuous stirring to obtain a uniform 5 wt% gelatin aqueous solution; adding 0.1g of nano titanium dioxide and 0.1g of nano silicon dioxide into the prepared gelatin aqueous solution, and continuously performing ultrasonic dispersion for 6 hours at the temperature of 60 ℃ to obtain milky suspension;
b) pouring the suspension obtained in the step a) into a mould, gelatinizing at low temperature, and then soaking the suspension into an excessive 20 wt% ammonium sulfate solution for curing for 24 hours to obtain stable high-elasticity gelatin nano hydrogel;
c) immersing the gelatin nano hydrogel obtained in the step d) into an excessive nickel ion solution with the concentration of 50g/mL for ion imprinting functionalization modification, and after continuously stirring, carrying out weak acid washing on the gelatin nano hydrogel taken out of the metal ion solution to obtain the ion imprinting functionalized gelatin nano hydrogel;
d) adding 100g of the ion imprinted functionalized gelatin nano hydrogel obtained in the step c) and 1g of glutaraldehyde into 110g of polyethyleneimine water solution with the mass percentage concentration of 5% for functional grafting modification to obtain a multifunctional gelatin nano hydrogel;
e) and d) carrying out vacuum freeze-drying treatment on the multifunctional gelatin nano-hydrogel prepared in the step d) for 48 hours to obtain the ultralight, porous and amphiphilic multifunctional nano-aerogel.
The obtained multifunctional nano aerogel with amphipathy is used as a filler and placed in a separation device shown in figure 2, after the aerogel filler is wetted by an aqueous phase, the wetting characteristic of the surface of the aerogel is changed into super-oleophobic property, an oil-water mixture of an n-hexane-water system is added from the upper part of the device, the n-hexane is blocked above the super-oleophobic aerogel only under the action of gravity, the aqueous phase flows out from the lower part through the aerogel, and the oil-water separation efficiency reaches 99.7%.
Specific example 2
A preparation method of multifunctional nano aerogel with amphipathy comprises the following steps:
a) dissolving 16g of gelatin in 184g of water at 50 ℃ under continuous stirring to obtain a uniform 8 wt% gelatin aqueous solution; adding 0.15g of nano titanium dioxide and 0.1g of nano silicon dioxide into the prepared gelatin aqueous solution, and performing continuous ultrasonic dispersion for 8 hours at 70 ℃ to obtain milky suspension;
b) pouring the suspension obtained in the step a) into a mould, gelatinizing at low temperature, and then soaking the suspension into an excessive 30 wt% ammonium chloride solution for curing for 28 hours to obtain stable high-elasticity gelatin nano hydrogel;
c) immersing the gelatin nano hydrogel obtained in the step d) into an excessive nickel ion solution with the concentration of 80g/mL for ion imprinting functionalization modification, and after continuously stirring, carrying out weak acid washing on the gelatin nano hydrogel taken out of the metal ion solution to obtain the ion imprinting functionalized gelatin nano hydrogel;
d) adding 120g of ion imprinted functionalized gelatin nano hydrogel obtained in the step c) and 1.2g of genipin into 132g of polyethyleneimine aqueous solution with the mass percentage concentration of 4% for functional grafting modification to obtain multifunctional gelatin nano hydrogel;
e) and d) carrying out vacuum freeze-drying treatment on the multifunctional gelatin nano-hydrogel prepared in the step d) for 24 hours to obtain the ultralight, porous and amphiphilic multifunctional nano-aerogel.
The obtained multifunctional nano aerogel with amphipathy is used as a filler and is placed in a separation device shown in figure 2, after the aerogel filler is wetted by a water phase, the wetting characteristic of the surface of the aerogel is changed into super-oleophobic property, oil-in-water toluene emulsion containing 50g/mL of nickel ions is added from the upper part of the device, the toluene is blocked above the super-oleophobic aerogel under the action of gravity, water flows out from a lower outlet through the aerogel, the oil-water separation efficiency is 99.8%, meanwhile, the nickel ions in the water are adsorbed by chelate and functional groups in the aerogel, and the removal rate of the nickel ions is 98.6%.
Specific example 3
A preparation method of multifunctional gelatin nano aerogel with amphipathy comprises the following steps:
a) dissolving 12g of gelatin in 188g of water at 60 ℃ under continuous stirring to obtain a uniform 6 wt% gelatin aqueous solution; adding 0.1g of nano titanium dioxide and 0.15g of nano silicon dioxide into the prepared gelatin aqueous solution, and continuously stirring and ultrasonically dispersing for 7 hours at 70 ℃ to obtain milky suspension;
c) pouring the suspension obtained in the step b) into a mould, gelatinizing at low temperature, and then soaking the suspension into an excessive 40 wt% ammonium nitrate solution for curing for 28 hours to obtain the stable high-elasticity gelatin nano hydrogel;
d) immersing the gelatin nano hydrogel obtained in the step c) into an excessive copper ion solution with the concentration of 80g/mL for ion imprinting functionalization modification, and after continuously stirring, carrying out weak acid washing on the gelatin nano hydrogel taken out of the metal ion solution to obtain the ion imprinting functionalized gelatin nano hydrogel;
e) adding 110g of the ion imprinted functionalized gelatin nano hydrogel obtained in the step d) and 1.1g of formaldehyde into 121g of polyethyleneimine aqueous solution with the mass percentage concentration of 3% for functional grafting modification to obtain a multifunctional gelatin nano hydrogel;
f) and e) carrying out vacuum freeze-drying treatment on the multifunctional gelatin nano-hydrogel prepared in the step e) for 36 hours to obtain the ultralight, porous and amphiphilic multifunctional nano-aerogel.
The obtained multifunctional nano aerogel with amphipathy is used as a filler and is placed in a separation device shown in figure 2, after the aerogel filler is wetted by dichloromethane, the wetting property of the surface of the aerogel is changed into super-hydrophobicity, an oil-water mixture of a dichloromethane-water system containing 50g/mL of copper ions and 100g/mL of methyl orange (organic dye) is added from the upper part, water is blocked above the super-hydrophobic aerogel under the action of gravity, dichloromethane is discharged from a lower outlet through the aerogel, and the oil-water separation efficiency is 99.8%. Meanwhile, copper ions and methyl orange in the wastewater are adsorbed by the chelate and functional groups in the aerogel, the removal rate of the copper ions is 99%, and the removal rate of the methyl orange is 98.6%; the adsorbed methyl orange is subjected to photocatalytic degradation under the irradiation of ultraviolet light through titanium dioxide in the aerogel, and the degradation rate is 98.7%.
Claims (6)
1. A preparation method of multifunctional nano aerogel with amphipathy is characterized by comprising the following steps:
a) dissolving gelatin in water under the condition of continuous stirring to obtain a uniform gelatin aqueous solution with the gelatin mass fraction of 4-8%, adding nano titanium dioxide and nano silicon dioxide into the prepared gelatin aqueous solution, and performing ultrasonic dispersion to obtain a milky suspension; wherein, the mass fraction of the nano titanium dioxide in the suspension is 0.1-0.3 wt%, and the mass fraction of the nano silicon dioxide in the suspension is 0.1-0.5 wt%;
b) pouring the suspension obtained in the step a) into a mold, gelatinizing at low temperature, and then immersing the suspension into an excessive ammonium salt aqueous solution for curing to obtain stable high-elasticity gelatin nano hydrogel;
c) immersing the gelatin nano hydrogel obtained in the step b) into excessive metal ion solution for ion imprinting functionalization modification, continuously stirring, and then carrying out weak acid washing on the gelatin nano hydrogel taken out of the metal ion solution to obtain the ion imprinting functionalization nano hydrogel;
d) adding the ion-imprinted functionalized gelatin nano hydrogel obtained in the step c) and a cross-linking agent into a polyethyleneimine aqueous solution for functional grafting modification to obtain a multifunctional nano hydrogel, wherein the mass percentage concentration of the polyethyleneimine aqueous solution is 3-5%; the mass ratio of the gelatin nano hydrogel to the cross-linking agent to the polyethyleneimine aqueous solution is 1:0.01: 1.1;
e) freezing and drying the multifunctional nano-hydrogel prepared in the step d) to obtain the ultra-light and porous multifunctional nano-aerogel with amphipathy.
2. The method for preparing multifunctional nano aerogel having amphipathy of claim 1, wherein the stirring temperature in the step a) of the method is 50-60 ℃; the size of the nano titanium dioxide particles is 20-40nm, and the size of the nano silicon dioxide particles is 30-40 nm; the ultrasonic dispersion time is 6-8h, and the temperature is 60-70 ℃.
3. The preparation method of the multifunctional nano aerogel with amphipathy as claimed in claim 1, wherein the concentration of the aqueous solution of ammonium salt in the step b) of the method is 20-40 wt%, the ammonium salt is any one or more of ammonium sulfate, ammonium chloride, ammonium nitrate and ammonium carbonate, and the curing time is 20-28 h.
4. The method for preparing multifunctional nano aerogel with amphipathy according to claim 1, wherein the metal ions in the metal ion solution in step c) of the method are any one of copper ions, nickel ions, chromium ions, lead ions, cadmium ions, manganese ions and cobalt ions, and the concentration of the metal ions is 30-150 mg/L.
5. The method for preparing multifunctional nano aerogel with amphipathy of claim 1, wherein the cross-linking agent in the step d) of the method is any one of formaldehyde, glutaraldehyde, genipin and epichlorohydrin.
6. Method for the preparation of multifunctional nano-aerogels with amphiphilicity according to claim 1, wherein the cooling in step e) of the method is carried outThe freeze drying process is carried out under vacuum, and the drying time is 24-48 h; the obtained multifunctional gelatin nano aerogel is a three-dimensional porous aerogel with a layered structure, the aperture is 2-50nm, and the density is 0.1-0.3g/cm3The porosity is 75-90%.
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