CN110743398B - Preparation method of rare earth ion doped calcium alginate/carbon nanotube hydrogel antibacterial filter membrane - Google Patents
Preparation method of rare earth ion doped calcium alginate/carbon nanotube hydrogel antibacterial filter membrane Download PDFInfo
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- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2325/00—Details relating to properties of membranes
- B01D2325/48—Antimicrobial properties
Abstract
The invention discloses a preparation method of a rare earth ion doped calcium alginate/carbon nano tube hydrogel antibacterial filter membrane. Firstly, dissolving the carboxylated carbon nanotubes and sodium alginate in water to obtain a membrane casting solution, scraping the membrane casting solution into a membrane, and soaking the membrane in a soluble calcium salt water solution for full crosslinking to obtain the calcium alginate hydrogel membrane containing the carboxylated carbon nanotubes. The calcium ions can simultaneously crosslink carboxyl on the carboxylated carbon nano tube and carboxyl on the alginate to generate the organic-inorganic hybrid material, thereby improving the strength of the calcium alginate hydrogel and reducing the swelling performance of the calcium alginate hydrogel. The carboxylated carbon nano tubes endow the calcium alginate hydrogel with certain antibacterial performance. In order to further improve the antibacterial performance and the mechanical strength of the hydrogel, the calcium alginate hydrogel filtering membrane containing the carboxylated carbon nanotubes is soaked in a rare earth ion solution for secondary crosslinking to obtain the rare earth ion doped calcium alginate/carbon nanotube hydrogel antibacterial filtering membrane.
Description
Technical Field
The invention relates to a preparation method of a rare earth ion doped calcium alginate/carbon nano tube hydrogel antibacterial filtering membrane, belonging to the field of functional materials and membrane separation.
The invention relates to the technical fields of rare earth, antibiosis, a filter membrane, hydrogel and the like. In particular to a preparation method of a rare earth ion doped calcium alginate/carbon nano tube hydrogel antibacterial filter membrane.
Background
Common membrane filter materials such as Polyethylene (PE), polypropylene (PP), polyvinyl chloride (PVC), polyvinylidene fluoride (PVDF), clustering (PSF), etc. are very likely to cause adsorption of organic substances (proteins, etc.) on the surface and in membrane pores of the membrane, causing membrane pollution, resulting in severe attenuation of filtration flux, due to low surface energy and strong hydrophobicity. One approach to mitigate membrane fouling is to hydrophilize modify hydrophobic membranes to address this feature. Common hydrophilic modification methods include blending modification, surface coating modification, surface grafting modification and the like. However, these methods have problems that the modification process is complicated, the hydrophilic effect is unstable, or the bulk film is damaged during the production. More importantly, these methods cannot fundamentally solve the problem of hydrophilicity of the membrane and thus cannot fundamentally solve the contamination of the membrane. If the membrane body is made of hydrophilic substances, the pollution phenomenon caused by hydrophobicity does not exist. The polymer hydrogel is a hydrophilic substance which has a chemically or physically crosslinked structure, can absorb a large amount of water and can maintain a certain shape in water.
As industry has developed, water pollution has become a serious environmental problem. The development of new and potential functional materials is a meaningful attempt in water pollution treatment and is gradually developing as a research hotspot for water treatment. The hydrogel has the excellent characteristics of high-efficiency adsorption performance, low cost, no toxicity and the like, so that the hydrogel arouses the interest of a large number of researchers and is widely applied to the field of water treatment. In conventional wastewater treatment processes, TiO2Nanoparticles are generally utilized in the form of suspension systems because of the large surface area of their particles. However, suspended TiO in the wastewater2The separation of nanoparticles necessarily increases operating costs and causes secondary pollution, thus greatly limiting its practical applications [ appl.catal.b, 2009, 88: 323-330 ]. Has explored and realized TiO2Immobilization on different supports, such as glass, stainless steel plates, fibers, carbon nanotubes, polymers, etc. S.k.papageorgiou et al studied the photocatalytic/ultrafiltration removal process of toxic-containing wastewater. TiO 22The photocatalyst is effectively immobilized in the calcium alginate hollow fiber. Wang et al utilized hydrothermal method to produce Carbon Nanotubes (CNTs) and P-TiO at different ratios2Synthesize CNTs/P-TiO2Nano catalyst, this catalyst is TiO2Has higher catalytic activity and wider spectral response range.
Carbon nanotubes are widely used in various fields due to their unique structures. In 2007, Kang et al in professor Elimelch of Yale university inspired from the toxicity of the nanotube, the interaction between SWNTS and bacteria was detected, and the result found that SWNTS exhibits excellent antibacterial performance. Subsequently, the laboratory has conducted a series of intensive studies on the antibacterial properties of the carbon nanotubes. Different from common chemical reagents, the carbon nanotube has different sizes, structures and appearances, and different preparation modes, impurities and chemical modifications can also cause the difference of the biological effect of the carbon nanotube cells. The physicochemical properties of the carbon nanotubes are closely related to the antibacterial activity exhibited by the carbon nanotubes.
The antibacterial effect of rare earth has attracted people's attention, and an external bactericide with the trade name of Ceriform is sold in the European market in 1906, the main chemical component of the bactericide is ceric potassium sulfate, and other cerium salts also have antibacterial ability. Jancso et al discovered that the neodymium and samarium compounds of the ferrotitanium reagent have anti-inflammatory properties, and then made them into ointment type medicines Phlog. Experiments show that Phlog has the maximum anti-inflammatory effect when the ratio of the rare earth to the ferrotitanium is 1: 2, and the ointment with the content of 3% has the best use effect. In recent years, a large number of researches show that the gargle containing 3% of neodymium sulfosalicylate and 0.1% of chlorhexidine is effective in inhibiting dental plaque, particularly has good effect on relieving gingival inflammation, and shows that rare earth ions have obvious anti-inflammatory effect. Rare earth compounds also often exhibit other superior bacteriostatic properties. For example, the ternary complex of camphorsulfonic acid, phenanthroline and rare earth has a stronger inhibitory effect on staphylococcus aureus, bacillus, pseudomonas aeruginosa, etc. than the corresponding ligand and binary complex.
The invention discloses a preparation method of a rare earth ion doped calcium alginate/carbon nano tube hydrogel antibacterial filter membrane. Firstly, dissolving the carboxylated carbon nanotubes and sodium alginate in water to obtain a membrane casting solution, scraping the membrane casting solution into a membrane, and soaking the membrane in a soluble calcium salt water solution for full crosslinking to obtain the calcium alginate hydrogel membrane containing the carboxylated carbon nanotubes. The calcium ions can simultaneously crosslink carboxyl on the carboxylated carbon nano tube and carboxyl on the alginate to generate the organic-inorganic hybrid material, thereby improving the strength of the calcium alginate hydrogel and reducing the swelling performance of the calcium alginate hydrogel. The carboxylated carbon nanotubes endow the calcium alginate hydrogel with antibacterial performance. In order to further improve the antibacterial performance and the mechanical strength of the hydrogel, the calcium alginate hydrogel filtering membrane containing the carboxylated carbon nanotubes is soaked in an aqueous solution of rare earth ions with the mass percentage concentration of 0.1-5% for secondary crosslinking, so that the rare earth ion doped calcium alginate/carbon nanotube hydrogel antibacterial filtering membrane is obtained.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to solve the technical problems that the traditional filtering membrane has poor hydrophilicity, is not polluted, has low strength and is easy to degrade by bacteria.
The invention provides a preparation method of a rare earth ion-doped calcium alginate/carbon nano tube hydrogel antibacterial filter membrane, which solves the problems that the traditional filter membrane is poor in hydrophilicity and not pollution-resistant, and the calcium alginate hydrogel filter membrane is low in strength and easy to degrade by bacteria.
The invention provides a preparation method of a rare earth ion doped calcium alginate/carbon nano tube hydrogel antibacterial filter membrane, which is characterized by comprising the following steps:
a) preparing a mixture water solution of the carboxylated carbon nano tube with the mass percentage concentration of 0.01-5%, then adding sodium alginate solid powder with the mass percentage concentration of 0.2-8% into the mixture water solution, stirring while adding, performing ultrasonic dispersion to obtain a mixture water solution of the carboxylated carbon nano tube and the sodium alginate, and standing and defoaming to obtain a casting solution;
b) preparing soluble calcium salt water solution with mass percent concentration of 0.2-20% as coagulating bath;
c) pouring the casting solution obtained in the step a) on a dry and clean glass plate, scraping the glass plate by using a glass rod with two ends wound with copper wires with the diameter of 20-1500 mu m, immediately putting the glass plate and the scraped film into the coagulating bath obtained in the step b) for soaking for 5-240min, reacting soluble calcium salt with sodium alginate to generate calcium alginate hydrogel, and simultaneously crosslinking carboxyl on carboxylated carbon nanotubes in the calcium alginate hydrogel to generate an organic-inorganic hybrid structure, and adding the physical enhancement effect of the carboxylated carbon nanotubes, so that the mechanical strength of the calcium alginate hydrogel is improved, and the swelling performance of the calcium alginate hydrogel is reduced; the carboxylated carbon nano tubes endow the calcium alginate hydrogel with antibacterial performance;
d) in order to further improve the antibacterial performance and mechanical strength of the hydrogel, the calcium alginate hydrogel membrane containing the carboxylated carbon nanotubes obtained in the step c) is soaked in an aqueous solution of rare earth ions with the mass percentage concentration of 0.1-5% for secondary crosslinking, so that the rare earth ion doped calcium alginate/carbon nanotube hydrogel antibacterial filtering membrane is obtained.
The carboxylated carbon nanotube is any one or a mixture of two or more of carboxylated single-wall carbon nanotube, carboxylated double-wall carbon nanotube and carboxylated multi-wall carbon nanotube; the soluble calcium salt is any one or mixture of two or more of calcium chloride, calcium nitrate, calcium dihydrogen phosphate and calcium gluconate; the rare earth ions are any one or a mixture of two or more of lanthanum ions, terbium ions, cerium ions, neodymium ions and samarium ions.
The carboxylated carbon nanotubes and the rare earth ions endow the calcium alginate hydrogel filtering membrane with good antibacterial performance, and the calcium alginate hydrogel filtering membrane is prevented from being degraded by bacteria in the using process; the structure of the calcium alginate hydrogel filtering membrane is changed by the crosslinking of the rare earth ions, and the pure water flux of the calcium alginate/carbon nano tube hydrogel antibacterial filtering membrane doped with the rare earth ions is 1.5-3 times of that of the calcium alginate filtering membrane.
The preparation method is simple, the preparation process is green and environment-friendly, and the obtained rare earth ion doped calcium alginate/carbon nanotube hydrogel antibacterial filtering membrane has good pollution resistance and has good application prospects in dye desalination, brown sugar decolorization and protein purification.
Detailed Description
Specific examples of the present invention will be described below, but the present invention is not limited to the examples.
Example 1.
a) Preparing a mixture water solution of carboxylated single-walled carbon nanotubes with the mass percentage concentration of 0.01%, then adding sodium alginate solid powder with the mass percentage concentration of 0.2% into the mixture water solution, stirring while adding, performing ultrasonic dispersion to obtain a mixture water solution of the carboxylated single-walled carbon nanotubes and the sodium alginate, and standing and defoaming to obtain a membrane casting solution;
b) preparing a calcium chloride water solution with the mass percentage concentration of 0.2 percent as a coagulating bath;
c) pouring the casting solution obtained in the step a) on a dry and clean glass plate, scraping the glass plate by using a glass rod with copper wires with the diameter of 20 microns wound at two ends, immediately putting the glass plate and the scraped film into the coagulating bath obtained in the step b) for soaking for 5min, reacting calcium chloride with sodium alginate to generate calcium alginate hydrogel, and simultaneously crosslinking carboxyl on carboxylated single-walled carbon nanotubes in the calcium alginate hydrogel to generate an organic-inorganic hybrid structure, and adding the physical enhancement effect of the carboxylated single-walled carbon nanotubes, so that the mechanical strength of the calcium alginate hydrogel is improved, and the swelling performance of the calcium alginate hydrogel is reduced; the carboxylated single-walled carbon nanotubes endow the calcium alginate hydrogel with antibacterial performance;
d) in order to further improve the antibacterial performance and mechanical strength of the hydrogel, the calcium alginate hydrogel membrane containing the carboxylated single-walled carbon nanotubes obtained in the step c) is soaked in an aqueous solution of lanthanum ions with the mass percentage concentration of 0.1% for secondary crosslinking to obtain a lanthanum ion-doped calcium alginate/carbon nanotube hydrogel antibacterial filtering membrane, and the pure water flux of the filtering membrane is 1.5 times that of the calcium alginate filtering membrane.
Example 2.
a) Preparing a mixture water solution of the carboxylated double-walled carbon nanotube with the mass percentage concentration of 5%, then adding sodium alginate solid powder with the mass percentage concentration of 8% into the mixture water solution, stirring while adding, performing ultrasonic dispersion to obtain a mixture water solution of the carboxylated double-walled carbon nanotube and the sodium alginate, and standing and defoaming to obtain a membrane casting solution;
b) preparing a calcium nitrate water solution with the mass percentage concentration of 20 percent as a coagulating bath;
c) pouring the casting solution obtained in the step a) on a dry and clean glass plate, scraping the glass plate by using a glass rod with two ends wound with copper wires with the diameter of 1500 mu m, immediately putting the glass plate and the scraped film into the coagulating bath obtained in the step b) for soaking for 240min, reacting calcium nitrate with sodium alginate to generate calcium alginate hydrogel, and simultaneously crosslinking the calcium alginate hydrogel with carboxyl on carboxylated double-wall carbon nanotubes in the calcium alginate hydrogel to generate an organic-inorganic hybrid structure, and adding the physical enhancement effect of the carboxylated double-wall carbon nanotubes, so that the mechanical strength of the calcium alginate hydrogel is improved, and the swelling performance of the calcium alginate hydrogel is reduced; the carboxylated double-wall carbon nano tube endows the calcium alginate hydrogel with antibacterial performance;
d) in order to further improve the antibacterial performance and mechanical strength of the hydrogel, the calcium alginate hydrogel membrane containing the carboxylated double-wall carbon nano tubes obtained in the step c) is soaked in a water solution of cerium ions with the mass percentage concentration of 5% for secondary crosslinking, so that the cerium ion-doped calcium alginate/carbon nano tube hydrogel antibacterial filtering membrane is obtained, and the pure water flux of the filtering membrane is 1.8 times that of the calcium alginate filtering membrane.
Example 3.
a) Preparing a mixture aqueous solution of carboxylated multi-wall carbon nanotubes with the mass percentage concentration of 1%, then adding sodium alginate solid powder with the mass percentage concentration of 2% into the mixture aqueous solution, stirring while adding, performing ultrasonic dispersion to obtain a mixture aqueous solution of the carboxylated multi-wall carbon nanotubes and the sodium alginate, and standing and defoaming to obtain a membrane casting solution;
b) preparing a calcium dihydrogen phosphate water solution with the mass percentage concentration of 10 percent as a coagulating bath;
c) pouring the casting solution obtained in the step a) on a dry and clean glass plate, scraping the glass plate by using a glass rod with copper wires with the diameter of 500 mu m wound at two ends, immediately putting the glass plate and the scraped film into the coagulating bath obtained in the step b) for soaking for 60min, reacting calcium dihydrogen phosphate with sodium alginate to generate calcium alginate hydrogel, and simultaneously crosslinking carboxyl on carboxylated multi-walled carbon nanotubes in the calcium alginate hydrogel to generate an organic-inorganic hybrid structure, and adding the physical enhancement effect of the carboxylated multi-walled carbon nanotubes, so that the mechanical strength of the calcium alginate hydrogel is improved, and the swelling performance of the calcium alginate hydrogel is reduced; the carboxylated multi-walled carbon nano-tube endows the calcium alginate hydrogel with antibacterial performance;
d) in order to further improve the antibacterial performance and the mechanical strength of the hydrogel, the calcium alginate hydrogel membrane containing the carboxylated multi-walled carbon nanotubes obtained in the step c) is soaked in a terbium ion aqueous solution with the mass percentage concentration of 0.5% for secondary crosslinking to obtain a terbium ion-doped calcium alginate/carbon nanotube hydrogel antibacterial filtering membrane, and the pure water flux of the filtering membrane is 3 times that of the calcium alginate filtering membrane.
Example 4.
a) Preparing a mixture water solution of the carboxylated double-walled carbon nanotube with the mass percentage concentration of 1%, then adding sodium alginate solid powder with the mass percentage concentration of 1% into the mixture water solution, stirring while adding, performing ultrasonic dispersion to obtain a mixture water solution of the carboxylated double-walled carbon nanotube and the sodium alginate, and standing and defoaming to obtain a membrane casting solution;
b) preparing a calcium gluconate water solution with the mass percentage concentration of 5 percent as a coagulating bath;
c) pouring the casting solution obtained in the step a) on a dry and clean glass plate, scraping the glass plate by using a glass rod with two ends wound with copper wires with the diameter of 500 mu m, immediately putting the glass plate and the scraped film into the coagulating bath obtained in the step b) for soaking for 120min, reacting calcium gluconate with sodium alginate to generate calcium alginate hydrogel, and simultaneously crosslinking carboxyl on carboxylated double-wall carbon nanotubes in the calcium alginate hydrogel to generate an organic-inorganic hybrid structure, and adding the physical enhancement effect of the carboxylated double-wall carbon nanotubes, so that the mechanical strength of the calcium alginate hydrogel is improved, and the swelling performance of the calcium alginate hydrogel is reduced; the carboxylated double-wall carbon nano tube endows the calcium alginate hydrogel with antibacterial performance;
d) in order to further improve the antibacterial performance and mechanical strength of the hydrogel, the calcium alginate hydrogel membrane containing the carboxylated double-wall carbon nano tubes obtained in the step c) is soaked in an aqueous solution of neodymium ions with the mass percentage concentration of 2% for secondary crosslinking, so that the neodymium ion-doped calcium alginate/carbon nano tube hydrogel antibacterial filtering membrane is obtained, and the pure water flux of the filtering membrane is 2.8 times that of the calcium alginate filtering membrane.
Claims (5)
1. A preparation method of a rare earth ion doped calcium alginate/carbon nano tube hydrogel antibacterial filter membrane is characterized by comprising the following steps:
a) preparing a mixture water solution of the carboxylated carbon nano tube with the mass percentage concentration of 0.01-5%, then adding sodium alginate solid powder with the mass percentage concentration of 0.2-8% into the mixture water solution, stirring while adding, performing ultrasonic dispersion to obtain a mixture water solution of the carboxylated carbon nano tube and the sodium alginate, and standing and defoaming to obtain a casting solution;
b) preparing soluble calcium salt water solution with mass percent concentration of 0.2-20% as coagulating bath;
c) pouring the casting solution obtained in the step a) on a dry and clean glass plate, scraping the glass plate by using a glass rod with two ends wound with copper wires with the diameter of 20-1500 mu m, immediately putting the glass plate and the scraped film into the coagulating bath obtained in the step b) for soaking for 5-240min, reacting soluble calcium salt with sodium alginate to generate calcium alginate hydrogel, and simultaneously crosslinking carboxyl on carboxylated carbon nanotubes in the calcium alginate hydrogel to generate an organic-inorganic hybrid structure, and adding the physical enhancement effect of the carboxylated carbon nanotubes, so that the mechanical strength of the calcium alginate hydrogel is improved, and the swelling performance of the calcium alginate hydrogel is reduced; the carboxylated carbon nano tubes endow the calcium alginate hydrogel with antibacterial performance;
d) in order to further improve the antibacterial performance and mechanical strength of the hydrogel, the calcium alginate hydrogel membrane containing the carboxylated carbon nanotubes obtained in the step c) is soaked in an aqueous solution of rare earth ions with the mass percentage concentration of 0.1-5% for secondary crosslinking, so that the rare earth ion doped calcium alginate/carbon nanotube hydrogel antibacterial filtering membrane is obtained.
2. The method for preparing a rare earth ion doped calcium alginate/carbon nanotube hydrogel antibacterial filter membrane as claimed in claim 1, wherein the carboxylated carbon nanotubes are any one or a mixture of two or more of carboxylated single-walled carbon nanotubes, carboxylated double-walled carbon nanotubes and carboxylated multi-walled carbon nanotubes.
3. The method for preparing a rare earth ion doped calcium alginate/carbon nanotube hydrogel antibacterial filter membrane according to claim 1, wherein the soluble calcium salt is any one or a mixture of two or more of calcium chloride, calcium nitrate, calcium dihydrogen phosphate and calcium gluconate.
4. The method for preparing the rare earth ion-doped calcium alginate/carbon nanotube hydrogel antibacterial filtering membrane according to claim 1, wherein the rare earth ion is any one or a mixture of two or more of lanthanum ion, terbium ion, cerium ion, neodymium ion and samarium ion.
5. Use of the membrane obtained by the preparation method according to claim 1 in dye desalination, brown sugar decolorization and protein purification.
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