CN112808227B - Hybrid aerogel adsorbent, preparation method thereof and application thereof in wastewater treatment - Google Patents
Hybrid aerogel adsorbent, preparation method thereof and application thereof in wastewater treatment Download PDFInfo
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Abstract
The application discloses a hybrid aerogel adsorbent which is formed by taking honeycomb silicon dioxide/titanium dioxide nano fibers as a framework material and intertwining nano silicon dioxide particles and nano titanium dioxide particles. The application also discloses a preparation method of the hybrid aerogel adsorbent and application of the hybrid aerogel adsorbent in wastewater treatment. The hybrid aerogel adsorbent provided by the application has the advantages of large specific surface area, strong adsorption capacity, high wastewater treatment efficiency, no secondary pollution to water, simple preparation method and low cost.
Description
Technical Field
The application relates to the field of wastewater treatment, in particular to a hybrid aerogel adsorbent, a preparation method thereof and application thereof in wastewater treatment.
Background
Water is a precious natural resource, is an indispensable basic substance in the production and life of people, and plays an important role in the survival and development of society. At present, the problem of water resource pollution is solved, and the hot spot of the research is studied. The method for treating the wastewater mainly comprises a physical method, a chemical method, a biological method and the like, wherein the adsorption method in the physical method is widely applied because of simple process, easy operation and low cost. Chinese patent CN201810695178.0 provides an adsorbent for adsorption treatment of electroplating wastewater, which comprises the following components in parts by mass: 20-30 parts of diatomite powder, 15-20 parts of medical stone powder, 25-30 parts of lipase liquid, 5-8 parts of sodium humate, 15-18 parts of nano ferroferric oxide, 15-18 parts of carboxymethyl starch sodium, 5-8 parts of polyaluminum chloride, 5-9 parts of anhydrous magnesium chloride, 6-9 parts of magnesium oxide, 5-10 parts of isobutyl 2, 4-dichlorophenoxyacetate and 5-12 parts of bacillus cereus bacterial agent. The adsorbent for the adsorption treatment of the electroplating wastewater has strong adsorption capacity to heavy metals in the electroplating wastewater, and the adsorption capacity to heavy metals in the electroplating wastewater reaches 90%; and the microbial inoculum is added, so that bacteria in electroplating wastewater are effectively treated, and the treated sewage meets the discharge requirement. Chinese patent CN201910300252.9 discloses a fiber-based aerogel adsorbent and its application in adsorbing dyeing wastewater, which is prepared from cellulose, acrylic acid and acrylamide by polymerization, wherein the mass ratio of cellulose, acrylic acid and acrylamide is 1:8-12:1-3. According to the application, functional groups are introduced into cellulose molecules through molecular design, and the cellulose-based adsorption material with high-efficiency adsorption performance is obtained through process control, so that the double purposes of recycling cellulose-containing textile waste resources and treating waste with waste by combining high-efficiency and rapid removal of dye in dyeing wastewater are realized. From the prior art, the key point of the wastewater treatment by the adsorption method is to provide an adsorbent with strong adsorption capacity.
Disclosure of Invention
One of the technical problems to be solved by the application is as follows: providing a hybrid aerogel adsorbent; the adsorbent takes a three-dimensional network structure formed by silica/titanium dioxide nanofibers as a framework, takes silica sol as an adhesive, and entangles nano silica particles and nano titanium dioxide particles in the three-dimensional network structure to form the honeycomb adsorbent with layered porous structure, and has the advantages of large specific surface area, good dispersibility, good mechanical property and excellent adsorption property.
The second technical problem to be solved by the application is as follows: the application provides a preparation method of a hybrid aerogel adsorbent, which combines a coaxial spinning method and a sol-gel method, prepares a stable porous titanium dioxide/silicon dioxide three-dimensional fiber network through directional freeze drying, adopts silicon dioxide sol as nano glue, and entangles nano silicon dioxide particles and nano titanium dioxide particles in the fiber network to form the stable aerogel.
The third technical problem to be solved by the application is: the application provides an application of the hybrid aerogel adsorbent in wastewater treatment, and the hybrid aerogel adsorbent provided by the application has high treatment efficiency and no secondary pollution to water body when being used for wastewater treatment.
In order to solve the first technical problem, the technical scheme of the application is as follows:
a hybrid aerogel adsorbent is formed by taking honeycomb silicon dioxide/titanium dioxide nano fibers as a framework material and intertwining nano silicon dioxide particles and nano titanium dioxide particles; in the silica/titanium dioxide nanofiber aerogel, the mole ratio of silicon atoms to titanium atoms is (1-2): 1, a step of; the particle sizes of the nano titanium dioxide particles and the nano silicon dioxide particles are respectively 20-30nm and 20-30nm.
In order to solve the second technical problem, the technical scheme of the application is as follows:
a method for preparing a hybrid aerogel adsorbent, comprising the steps of:
(1) Mixing ethyl orthosilicate, deionized water, absolute ethyl alcohol and acetic acid, stirring and hydrolyzing to prepare a silicon dioxide precursor sol solution; mixing tetrabutyl titanate, deionized water, absolute ethyl alcohol and acetic acid, stirring and hydrolyzing to prepare a titanium dioxide precursor sol solution; mixing a silica precursor sol solution with an ethanol solution of polyvinyl butyral to obtain a spinning solution A, and mixing a titania precursor sol solution with an ethanol solution of polyvinyl butyral to obtain a spinning solution B; finally, taking spinning solution A as a sheath solution, taking spinning solution B as a core solution, preparing core-shell fibers by adopting a coaxial spinning method, and placing the fibers with a core-shell structure into a muffle furnace for calcination to prepare porous titanium dioxide/silicon dioxide core-shell fibers;
(2) Dispersing the prepared porous titanium dioxide/silicon dioxide core-shell fiber and titanium dioxide precursor sol solution in polyethylene oxide solution, then adding nano silicon dioxide and nano titanium dioxide respectively, continuously stirring and dispersing, transferring the prepared dispersion into a dendritic die, directionally freeze-drying in a liquid nitrogen bath for 10-20h, and finally placing the dried solid in a muffle furnace, heating to 700 ℃ at a speed of 5 ℃/min, and calcining for 2-3h to obtain the hybrid aerogel adsorbent.
As a preferable mode of the above technical scheme, in step (1), when the silica precursor sol solution is prepared, the molar ratio of tetraethyl orthosilicate, deionized water, absolute ethyl alcohol, and acetic acid is 1: (3-4): (0.5-1): (0.01-0.02).
As a preferable mode of the above technical scheme, in the step (1), when the titania precursor sol solution is prepared, the molar ratio of tetrabutyl titanate, deionized water, absolute ethyl alcohol and acetic acid is 1: (2-5): (0.5-0.8): (0.015-0.02).
As a preferable mode of the above technical scheme, in the step (1), the mass concentration of the ethanol solution of the polyvinyl butyral is 20-25%, and when the spinning solution a and the spinning solution B are prepared, the mass ratio of the silica precursor sol solution to the ethanol solution of the polyvinyl butyral and the mass ratio of the titania precursor sol solution to the ethanol solution of the polyvinyl butyral are (2-4): 1.
as a preferable mode of the above technical scheme, in the step (1), the condition of the calcination is: firstly, heating to 200 ℃ at a speed of 5 ℃/min, preserving heat for 1h, then heating to 800 ℃ at a speed of 10 ℃/min, and preserving heat for 1-2h.
As a preferable mode of the technical scheme, in the step (1), the diameter of the porous titanium dioxide/silicon dioxide core-shell fiber is 100-200nm, and the length is 30-50 mu m.
As a preferable mode of the above technical solution, in the step (2), the mass ratio of the porous titanium dioxide/silicon dioxide core-shell fiber, the titanium dioxide precursor sol solution, the polyethylene oxide solution, the nano silicon dioxide and the nano titanium dioxide is 1: (0.2-0.3): 200: (0.05-0.1): (0.05-0.1).
In order to solve the third technical problem, the technical scheme of the application is as follows:
the application of the hybrid aerogel adsorbent in wastewater treatment comprises the following specific processes: adding the prepared hybrid aerogel adsorbent into the wastewater, stirring, and filtering to obtain the treated wastewater.
As the preferable choice of the technical proposal, the adding amount of the hybrid aerogel adsorbent is 1-2g/L, the stirring speed during the treatment is 100-200 rpm, and the stirring time is 1-2h.
Due to the adoption of the technical scheme, the application has the beneficial effects that:
the hybrid aerogel adsorbent provided by the application is prepared by taking honeycomb silicon dioxide/titanium dioxide nanofiber as a framework material and intertwining nano silicon dioxide particles and nano titanium dioxide particles, wherein the prepared hybrid aerogel adsorbent has the concentration of 0.1-0.2mg/cm 3 Has strong adsorption capacity, and can be well removed when being used for wastewater treatmentContaminants in the wastewater.
The application adopts the combination of a coaxial spinning process and sol gel, firstly prepares porous hollow titanium dioxide/silicon dioxide core-shell fiber, then disperses the porous hollow titanium dioxide/silicon dioxide core-shell fiber in polymer solution, adds silicon dioxide sol as nano glue to prepare homogenized solution, places the solution in a dendritic mold, carries out directional freeze drying, forms a large number of ice crystals in the drying process, stacks the porous hollow titanium dioxide/silicon dioxide core-shell fiber among the formed ice crystals, and also clamps polyethylene oxide, titanium dioxide particles and silicon dioxide particles among the ice crystals, and adheres to the surface of the porous hollow titanium dioxide/silicon dioxide core-shell fiber through hydrogen bonds, thus being locked in a three-dimensional network, and the ice crystals sublimate and are replaced by air along with the progress of freeze drying, and removes the polyethylene oxide in the subsequent calcination process to prepare the stable hybrid aerogel adsorbent which has good mechanical property and excellent adsorption property.
Detailed Description
The application is further illustrated below with reference to examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application.
The following raw materials have the following performance parameters:
polyvinyl butyral: the molecular weight is 40000-70000.
Polyethylene oxide: the molecular weight is 5000000.
Example 1
(1) 1mol of ethyl orthosilicate, 3mol of deionized water, 0.5mol of absolute ethyl alcohol and 0.01mol of acetic acid are mixed, stirred and hydrolyzed for 1 hour to prepare a silica precursor sol solution; 1mol of tetrabutyl titanate, 3mol of deionized water, 0.5mol of absolute ethyl alcohol and 0.015mol of absolute ethyl alcohol are mixed, stirred and hydrolyzed for 1 hour to prepare a titanium dioxide precursor sol solution; 8g of a silica precursor sol solution and 4g of an ethanol solution of 20% by mass concentration of polyvinyl butyral are mixed to prepare a spinning solution A, and 8g of a titania precursor sol solution and 4g of an ethanol solution of 20% by mass concentration of polyvinyl butyral are mixed to prepare a spinning solution B; finally, taking spinning solution A as a sheath solution, taking spinning solution B as a core solution, preparing core-shell fibers by adopting a coaxial spinning method, placing the fibers with a core-shell structure in a muffle furnace, firstly heating to 200 ℃ at a speed of 5 ℃/min, preserving heat for 1h, then heating to 800 ℃ at a speed of 10 ℃/min, preserving heat for 1h, and preparing the porous titanium dioxide/silicon dioxide core-shell fibers with a diameter of 100nm and a length of 30 mu m;
(2) Dispersing 10g of the prepared porous titanium dioxide/silicon dioxide core-shell fiber and 2g of titanium dioxide precursor sol solution in 200g of polyethylene oxide solution with the mass concentration of 0.01%, then respectively adding 0.05g of nano silicon dioxide and 0.05g of nano titanium dioxide, continuously stirring and dispersing, transferring the prepared dispersion liquid into a dendritic die, directionally freeze-drying in a liquid nitrogen bath for 10h, and finally placing the dried solid in a muffle furnace, heating to 700 ℃ at the speed of 5 ℃/min, and calcining for 2h to prepare the hybrid aerogel adsorbent.
Example 2
(1) 1mol of ethyl orthosilicate, 4mol of deionized water, 1mol of absolute ethyl alcohol and 0.01-0.02mol of acetic acid are mixed, stirred and hydrolyzed for 2 hours to prepare a silica precursor sol solution; 1mol of tetrabutyl titanate, 4mol of deionized water, 1mol of absolute ethyl alcohol and 0.02mol of absolute ethyl alcohol are mixed, stirred and hydrolyzed for 2 hours to prepare a titanium dioxide precursor sol solution; mixing 16g of a silica precursor sol solution and 4g of an ethanol solution of 25% polyvinyl butyral in mass concentration to prepare a spinning solution A, and mixing 16g of a titania precursor sol solution and 4g of an ethanol solution of 25% polyvinyl butyral in mass concentration to prepare a spinning solution B; finally, taking spinning solution A as a sheath solution, taking spinning solution B as a core layer solution, preparing core-shell fibers by adopting a coaxial spinning method, placing the fibers with a core-shell structure in a muffle furnace, firstly heating to 200 ℃ at a speed of 5 ℃/min, preserving heat for 1h, then heating to 800 ℃ at a speed of 10 ℃/min, preserving heat for 2h, and preparing the porous titanium dioxide/silicon dioxide core-shell fibers with a diameter of 100nm and a length of 50 mu m;
(2) 10g of the prepared porous titanium dioxide/silicon dioxide core-shell fiber and 2.5g of titanium dioxide precursor sol solution are dispersed in 200g of polyethylene oxide solution with the mass concentration of 0.01%, then 0.05g of nano silicon dioxide and 0.05g of nano titanium dioxide are respectively added, stirring and dispersion are continued, the prepared dispersion is transferred into a dendritic die, directional freeze drying is carried out in a liquid nitrogen bath for 15h, and finally the dried solid is placed in a muffle furnace and heated to 700 ℃ at the speed of 5 ℃/min for calcination for 2h, so that the hybrid aerogel adsorbent is prepared.
Example 3
(1) 1mol of ethyl orthosilicate, 3mol of deionized water, 1mol of absolute ethyl alcohol and 0.02mol of acetic acid are mixed, stirred and hydrolyzed for 1.5 hours to prepare a silica precursor sol solution; 1mol of tetrabutyl titanate, 3mol of deionized water, 1mol of absolute ethyl alcohol and 0.015mol of absolute ethyl alcohol are mixed, stirred and hydrolyzed for 1.5 hours to prepare a titanium dioxide precursor sol solution; 10g of a silica precursor sol solution and 4g of an ethanol solution of polyvinyl butyral with a mass concentration of 21% are mixed to prepare a spinning solution A, and 10g of a titania precursor sol solution and 4g of an ethanol solution of polyvinyl butyral with a mass concentration of 21% are mixed to prepare a spinning solution B; finally, taking spinning solution A as a sheath solution, taking spinning solution B as a core layer solution, preparing core-shell fibers by adopting a coaxial spinning method, placing the fibers with a core-shell structure in a muffle furnace, firstly heating to 200 ℃ at a speed of 5 ℃/min, preserving heat for 1h, then heating to 800 ℃ at a speed of 10 ℃/min, preserving heat for 2h, and preparing the porous titanium dioxide/silicon dioxide core-shell fibers with a diameter of 150nm and a length of 40 mu m;
(2) Dispersing 10g of the prepared porous titanium dioxide/silicon dioxide core-shell fiber and 3g of titanium dioxide precursor sol solution in 200g of polyethylene oxide solution with the mass concentration of 0.01%, then respectively adding 0.1g of nano silicon dioxide and 0.1g of nano titanium dioxide, continuously stirring and dispersing, transferring the prepared dispersion liquid into a dendritic die, directionally freeze-drying in a liquid nitrogen bath for 20h, and finally placing the dried solid in a muffle furnace, heating to 700 ℃ at the speed of 5 ℃/min, and calcining for 3h to prepare the hybrid aerogel adsorbent.
Example 4
(1) 1mol of ethyl orthosilicate, 4mol of deionized water, 1mol of absolute ethyl alcohol and 0.015mol of acetic acid are mixed, stirred and hydrolyzed for 2 hours to prepare a silica precursor sol solution; 1mol of tetrabutyl titanate, 3mol of deionized water, 0.5mol of absolute ethyl alcohol and 0.015mol of water are mixed, stirred and hydrolyzed for 1 to 2 hours to prepare a titanium dioxide precursor sol solution; mixing 12g of a silica precursor sol solution and 4g of an ethanol solution of 22% polyvinyl butyral in mass concentration to prepare a spinning solution A, and mixing 12g of a titania precursor sol solution and 4g of an ethanol solution of 22% polyvinyl butyral in mass concentration to prepare a spinning solution B; finally, taking spinning solution A as a sheath layer solution, taking spinning solution B as a core layer solution, preparing core-shell fibers by adopting a coaxial spinning method, placing the fibers with a core-shell structure in a muffle furnace, firstly heating to 200 ℃ at a speed of 5 ℃/min, preserving heat for 1h, then heating to 800 ℃ at a speed of 10 ℃/min, preserving heat for 1.5h, and preparing the porous titanium dioxide/silicon dioxide core-shell fibers with a diameter of 150nm and a length of 40 mu m;
(2) Dispersing 10g of the prepared porous titanium dioxide/silicon dioxide core-shell fiber and 2g of titanium dioxide precursor sol solution in 200g of polyethylene oxide solution with the mass concentration of 0.01%, then respectively adding 0.08g of nano silicon dioxide and 0.08g of nano titanium dioxide, continuously stirring and dispersing, transferring the prepared dispersion liquid into a dendritic die, directionally freeze-drying in a liquid nitrogen bath for 18h, and finally placing the dried solid in a muffle furnace, heating to 700 ℃ at the speed of 5 ℃/min, and calcining for 3h to prepare the hybrid aerogel adsorbent.
Application examples
The method comprises the steps of taking methylene blue solution with the concentration of 1000mg/L as wastewater to be treated, respectively adding the adsorbents prepared in the examples 1-4 into the wastewater to be treated in the proportion of 1g/L, stirring for 2 hours at the rotating speed of 100-200 rpm, treating and then filtering to obtain treated wastewater, testing the concentration of methylene blue in the treated wastewater, and calculating the removal rate of dye molecules. The control group uses honeycomb activated carbon sold by Huixin water-saving materials factory in the consolidated city, and the test results are shown in table 2.
TABLE 2
As can be seen from the test results, compared with the commercially available honeycomb activated carbon, the hybrid aerogel adsorbent prepared by the application has better adsorption effect and can well remove dye molecules in wastewater.
Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
Claims (9)
1. A hybrid aerogel adsorbent, characterized by: the hybrid aerogel adsorbent takes honeycomb silicon dioxide/titanium dioxide nano fibers as a framework material, and is formed by intertwining nano silicon dioxide particles and nano titanium dioxide particles; in the silica/titanium dioxide nanofiber aerogel, the mole ratio of silicon to titanium atoms is (1-2): 1, a step of; the particle sizes of the nano titanium dioxide particles and the nano silicon dioxide particles are respectively 20-30nm and 20-30nm;
the preparation of the hybrid aerogel adsorbent comprises the following steps:
(1) Mixing ethyl orthosilicate, deionized water, absolute ethyl alcohol and acetic acid, stirring and hydrolyzing to prepare a silicon dioxide precursor sol solution; mixing tetrabutyl titanate, deionized water, absolute ethyl alcohol and acetic acid, stirring and hydrolyzing to prepare a titanium dioxide precursor sol solution; mixing a silica precursor sol solution with an ethanol solution of polyvinyl butyral to obtain a spinning solution A, and mixing a titania precursor sol solution with an ethanol solution of polyvinyl butyral to obtain a spinning solution B; finally, taking spinning solution A as a sheath solution, taking spinning solution B as a core solution, preparing core-shell fibers by adopting a coaxial spinning method, and placing the fibers with a core-shell structure into a muffle furnace for calcination to prepare porous titanium dioxide/silicon dioxide core-shell fibers;
(2) Dispersing the prepared porous titanium dioxide/silicon dioxide core-shell fiber and titanium dioxide precursor sol solution in polyethylene oxide solution, then adding nano silicon dioxide and nano titanium dioxide respectively, continuously stirring and dispersing, transferring the prepared dispersion into a dendritic die, directionally freeze-drying in a liquid nitrogen bath for 10-20h, and finally placing the dried solid in a muffle furnace, heating to 700 ℃ at a speed of 5 ℃/min, and calcining for 2-3h to obtain the hybrid aerogel adsorbent.
2. The hybrid aerogel adsorbent of claim 1, wherein: in the step (1), when the silica precursor sol solution is prepared, the molar ratio of the tetraethoxysilane to the deionized water to the absolute ethyl alcohol to the acetic acid is 1: (3-4): (0.5-1): (0.01-0.02).
3. The hybrid aerogel adsorbent of claim 1, wherein: in the step (1), when the titanium dioxide precursor sol solution is prepared, the molar ratio of tetrabutyl titanate, deionized water, absolute ethyl alcohol and acetic acid is 1: (2-5): (0.5-0.8): (0.015-0.02).
4. The hybrid aerogel adsorbent of claim 1, wherein: in the step (1), the mass concentration of the ethanol solution of the polyvinyl butyral is 20-25%, and when the spinning solution A and the spinning solution B are prepared, the mass ratio of the silica precursor sol solution to the ethanol solution of the polyvinyl butyral and the mass ratio of the titania precursor sol solution to the ethanol solution of the polyvinyl butyral are (2-4): 1.
5. the hybrid aerogel adsorbent of claim 1, wherein: in the step (1), the calcining conditions are as follows: firstly, heating to 200 ℃ at a speed of 5 ℃/min, preserving heat for 1h, then heating to 800 ℃ at a speed of 10 ℃/min, and preserving heat for 1-2h.
6. The hybrid aerogel adsorbent of claim 1, wherein: in the step (1), the diameter of the porous titanium dioxide/silicon dioxide core-shell fiber is 100-200nm, and the length is 30-50 mu m.
7. The hybrid aerogel adsorbent of claim 1, wherein: in the step (2), the mass ratio of the porous titanium dioxide/silicon dioxide core-shell fiber, the titanium dioxide precursor sol solution, the polyethylene oxide solution, the nano silicon dioxide and the nano titanium dioxide is 1: (0.2-0.3): 200: (0.05-0.1): (0.05-0.1).
8. Use of a hybrid aerogel adsorbent according to any of claims 1 to 7 in wastewater treatment, characterized in that: the specific process is as follows: adding the prepared hybrid aerogel adsorbent into the wastewater, stirring, and filtering to obtain the treated wastewater.
9. The use of a hybrid aerogel adsorbent as claimed in claim 8 in wastewater treatment, wherein: the adding amount of the hybrid aerogel adsorbent is 1-2g/L, the stirring speed during treatment is 100-200 rpm, and the stirring time is 1-2h.
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| CN110467421A (en) * | 2019-07-03 | 2019-11-19 | 加新科技(深圳)有限公司 | A kind of functional fiber element aerogel composite and preparation method thereof |
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