WO2022217906A1 - Nanotube de carbone à parois multiples modifié, membrane à basse pression associée, procédé de préparation associé et utilisation associée - Google Patents

Nanotube de carbone à parois multiples modifié, membrane à basse pression associée, procédé de préparation associé et utilisation associée Download PDF

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WO2022217906A1
WO2022217906A1 PCT/CN2021/130182 CN2021130182W WO2022217906A1 WO 2022217906 A1 WO2022217906 A1 WO 2022217906A1 CN 2021130182 W CN2021130182 W CN 2021130182W WO 2022217906 A1 WO2022217906 A1 WO 2022217906A1
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walled carbon
carbon nanotube
modified multi
low
membrane
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PCT/CN2021/130182
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English (en)
Chinese (zh)
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郭瑾
王钰
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北京工业大学
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/168—After-treatment
    • 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
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00—Structure or properties of carbon nanotubes
    • C01B2202/06—Multi-walled nanotubes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00—Structure or properties of carbon nanotubes
    • C01B2202/20—Nanotubes characterized by their properties
    • C01B2202/34—Length
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00—Structure or properties of carbon nanotubes
    • C01B2202/20—Nanotubes characterized by their properties
    • C01B2202/36—Diameter
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents

Definitions

  • the invention relates to the technical field of multi-walled carbon nanotubes, in particular to a modified multi-walled carbon nanotube and a low-pressure membrane thereof, as well as a preparation method and application thereof.
  • Dyes are commonly found in wastewater from industries such as textiles, leather, paper, printing and cosmetics.
  • Dye wastewater has the characteristics of large chroma, complex composition, high biological toxicity and refractory degradation, which brings great difficulties to the treatment of dye wastewater.
  • the increasing discharge of dye wastewater into the aquatic environment will seriously harm biodiversity and the natural activities of aquatic systems.
  • Many physical, chemical and biological methods such as adsorption, membrane separation, ozone treatment, coagulation/flocculation, photocatalytic degradation, ion exchange, biosorption and biodegradation, have been used to remove wastewater from wastewater of dyes.
  • Activated carbon is the most widely used conventional adsorbent in dye wastewater adsorption treatment.
  • the pore structure of activated carbon is uneven, the pore size is widely distributed, the proportion of micropores and macropores is high, and the proportion of mesopores is small.
  • Most of the dye molecules are larger in size, such as methylene blue, which is larger than 1.3 nm, and can only enter mesopores or micropores with larger pore sizes, which leads to low utilization efficiency of activated carbon.
  • activated carbon contains a large proportion of inner pores, and the process of dye molecules diffusing from the liquid phase into the inner pores of activated carbon and being adsorbed is relatively slow. Using activated carbon to adsorb and purify dye wastewater requires a long equilibrium time, which is not conducive to the regeneration of saturated activated carbon. The removal effect of polar organics is relatively poor.
  • Carbon nanotubes have attracted much attention due to their ultra-high specific surface area and excellent mechanical, electrical and thermal properties.
  • CNT has a clear structure, uniform surface, open adsorption surface and mesoporous structure, and CNT also has a good treatment effect on polar organics.
  • the special structure of CNT enables its surface to be functionalized to remove pollutants of different properties.
  • the multi-walled carbon nanotube (MWCNT) has a simple production process, a relatively cheap price and a wider range of applications.
  • MWCNTs are prone to agglomeration when put into water, which reduces the available adsorption sites on the surface of MWCNTs and seriously affects the adsorption efficiency of MWCNTs.
  • Non-covalent functionalization of MWCNTs can effectively improve the dispersibility of MWCNTs without destroying the structure of carbon nanotubes.
  • Dispersants for non-covalent functionalization of MWCNTs include surfactants, peptides and proteins, and polysaccharides.
  • Humic acid (HA) exists in almost all water sources, and its content accounts for 40-90% of the total dissolved organic carbon in water. Similar to surfactants, HA is also amphiphilic, containing both hydrophilic groups (carboxyl groups, phenolic groups) and hydrophobic groups (aromatic rings, aromatic hydrocarbons). Studies have shown that HA improves the dispersibility of CNTs. In addition, HA-encapsulated CNTs have lower toxicity, which will reduce the ecological risk of CNT release into the environment.
  • the purpose of the present invention is to provide a method for preparing a modified multi-walled carbon nanotube and a low pressure membrane thereof in order to overcome the deficiencies of the prior art.
  • the preparation method of the invention does not cause any damage to the structure and performance of the multi-walled carbon nanotubes, and simultaneously avoids the ecological risk of the multi-walled carbon nanotubes entering the water environment.
  • the modified multi-walled carbon nanotube low-pressure membrane of the present invention maintains the operation range of the low-pressure membrane in the methylene blue dye removal process, has low cost, high efficiency, simple removal method and easy realization.
  • the invention provides a preparation method of modified multi-walled carbon nanotubes, comprising the following steps:
  • the present invention also provides a preparation method of the modified multi-walled carbon nanotube low-pressure film, comprising the following steps:
  • the modified multi-wall carbon nanotube dispersion liquid is subjected to solid-liquid separation using a microfiltration porous membrane to obtain a modified multi-wall carbon nanotube low-pressure membrane.
  • the outer diameter of the multi-walled carbon nanotubes in step 1) is 30-50 nm, the inner diameter is 8-15 nm, and the length is less than or equal to 10 ⁇ m; the concentration of the humic acid solution is 0.1-50 mg/mL.
  • the power of the ultrasonic treatment in step 1) is 100-200 W, and the time is 10-20 min; the concentration of the modified multi-walled carbon nanotube dispersion liquid is 0.5-2 mg/mL.
  • the present invention also provides the modified multi-walled carbon nanotubes obtained by the preparation method described in the above scheme.
  • the pore size of the microfiltration porous membrane is 0.4-0.5 ⁇ m, and the pressure of the solid-liquid separation is 0.08-0.12 MPa.
  • the present invention also provides the modified multi-walled carbon nanotube low pressure film obtained by the preparation method described in the above scheme.
  • the loading amount of the modified multi-walled carbon nanotubes on the low-pressure film of the modified multi-walled carbon nanotubes is ⁇ 22.39 g/m 2 .
  • the present invention also provides an application of the modified multi-wall carbon nanotubes or the low-pressure membrane of the modified multi-wall carbon nanotubes described in the above technical solution in removing methylene blue from water.
  • the present invention also provides a method for removing methylene blue from water using the modified multi-walled carbon nanotube low-pressure membrane described in the above technical solution, and using the modified multi-walled carbon nanotube low-pressure membrane to filter an aqueous solution containing methylene blue dye under constant flow;
  • the time of flow filtration is 180-220 min, the flow rate is 60-80 L ⁇ m -2 ⁇ h -1 , and in the constant flow filtration, the rotational speed of the peristaltic pump is 0.4-0.6 r/min.
  • the preparation process of the modified multi-walled carbon nanotubes and the low-pressure membrane thereof of the present invention is simple, does not cause any damage to the structure and performance of the multi-walled carbon nanotubes, and simultaneously avoids the ecological risk of the multi-walled carbon nanotubes entering the water environment.
  • the modified multi-walled carbon nanotube low-pressure membrane of the present invention is kept in the operating range of the low-pressure membrane in the methylene blue dye removal process, with low cost, high methylene blue removal efficiency, and the removal effect is hardly affected by the concentration of Na + and Ca 2+ .
  • the removal method is simple and easy to implement.
  • Fig. 1 is the modified multi-walled carbon nanotube low pressure film of embodiment 1;
  • Figure 2 is a comparison diagram of pure water flux under different pressures of the modified multi-walled carbon nanotube low-pressure membrane, the 0.45 ⁇ m polyethersulfone-based membrane and the original multi-walled carbon nanotube membrane of Example 1;
  • Figure 3 is a graph showing the effect of different concentrations of methylene blue solutions on the removal of methylene blue from the modified multi-walled carbon nanotube low-pressure membrane, 0.45 ⁇ m polyethersulfone-based membrane and original multi-walled carbon nanotube membrane of Example 1;
  • Figure 4 is a graph showing the change of the transmembrane pressure difference when the modified multi-walled carbon nanotube low-pressure membrane, the 0.45 ⁇ m polyethersulfone-based membrane and the original multi-walled carbon nanotube membrane of Example 1 filter 50 mg/L methylene blue solution;
  • Example 5 is a graph showing the effect of different pH values on the removal of methylene blue from the modified multi-walled carbon nanotube low-pressure film and the original multi-walled carbon nanotube film of Example 1;
  • FIG. 6 is a graph showing the effect of different Na concentrations on the removal of methylene blue from the modified multi - walled carbon nanotube low-pressure film and the original multi-walled carbon nanotube film of Example 1;
  • the invention provides a preparation method of modified multi-walled carbon nanotubes, comprising the following steps:
  • the present invention also provides a preparation method of the modified multi-walled carbon nanotube low-pressure film, comprising the following steps:
  • the modified multi-walled carbon nanotube dispersion liquid is subjected to solid-liquid separation using a microfiltration porous membrane to obtain a modified multi-walled carbon nanotube low-pressure membrane.
  • the outer diameter of the multi-walled carbon nanotubes in step 1) is preferably 30-50 nm, more preferably 35 to 45 nm, more preferably 40 nm; the inner diameter of the multi-walled carbon nanotubes is preferably 8 to 15 nm, more preferably 10 to 12 nm; the length of the multi-walled carbon nanotubes is preferably ⁇ 10 ⁇ m, more preferably 1 to 9 ⁇ m ;
  • the concentration of the humic acid solution is preferably 0.1-50 mg/mL, more preferably 3-40 mg/mL, and more preferably 10-20 mg/mL.
  • the present invention also provides the modified multi-walled carbon nanotubes obtained by the preparation method described in the above scheme.
  • the present invention preferably adopts the pressure filtration method to make the modified multi-wall carbon nanotube dispersion liquid pass through the microfiltration porous membrane, and in the process of solid-liquid separation, the modified multi-wall carbon nanotubes are separated
  • the walled carbon nanotubes are deposited on the surface of the microfiltration porous membrane;
  • the pore size of the microfiltration porous membrane of the present invention is preferably 0.4-0.5 ⁇ m, more preferably 0.42-0.48 ⁇ m, more preferably 0.44-0.46 ⁇ m;
  • the membrane is preferably a polyethersulfone membrane;
  • the pressure of the solid-liquid separation is preferably 0.08-0.12 MPa, more preferably 0.1 MPa.
  • the modified multi-walled carbon nanotube low-pressure membrane is preferably washed and dried; the washing is preferably ultrapure water. Rinse several times until the TOC value of the effluent is less than or equal to 0.2mg/L.
  • the present invention also provides the modified multi-walled carbon nanotube low pressure film obtained by the preparation method described in the above scheme.
  • the loading amount of modified multi-walled carbon nanotubes on the low-pressure membrane of the present invention is preferably ⁇ 22.39 g/m 2 .
  • the present invention also provides the application of the modified multi-walled carbon nanotubes described in the above scheme or the low-pressure membrane of the modified multi-walled carbon nanotubes described in the above scheme in removing methylene blue from water.
  • the present invention also provides a method for removing methylene blue from water by using the modified multi-walled carbon nanotube low-pressure membrane described in the above scheme, and using the modified multi-walled carbon nanotube low-pressure membrane to filter an aqueous solution containing methylene blue dye under constant flow;
  • the filtering time is preferably 180-220min, more preferably 190-210min, more preferably 200min;
  • the flow rate of the constant-flow filtration is preferably 60-80L ⁇ m -2 ⁇ h -1 , more preferably 65-75L ⁇ m -2 ⁇ h -1 , more preferably 75L ⁇ m -2 ⁇ h -1 ;
  • the rotational speed of the peristaltic pump is preferably 0.4 to 0.6 r/min, more preferably 0.5 r/min.
  • the influence of Na + and Ca 2+ concentrations is very small and can be ignored;
  • the concentration of Na + in the methylene blue aqueous solution is preferably 0 ⁇ 10 mmol/L, the concentration of Ca 2+ is preferably 0 to 5 mmol/L.
  • the concentration of methylene blue is preferably 10-50 mg/L.
  • the acidity and alkalinity of the aqueous solution have obvious effects on the removal of methylene blue, and the alkaline solution is more conducive to the removal of methylene blue.
  • the multi-walled carbon nanotube dispersion was passed through a polyethersulfone membrane with a pore size of 0.45 ⁇ m by a pressure filtration method (the pressure was 0.1 MPa), and then the modified multi-walled carbon nanotube low-pressure membrane was washed with ultrapure water through the membrane until the water was discharged.
  • the TOC value is lower than 0.2mg/L, and the low-pressure membrane is dried for use. According to the effective area of the polyethersulfone-based membrane and the amount of multi-walled carbon nanotubes, the modified multi-walled carbon nanotubes low-pressure membrane can be calculated, and the loading amount of the modified multi-walled carbon nanotubes is 22.39 g/m 2 .
  • the modified multi-walled carbon nanotube low-pressure film of Example 1 is shown in FIG. 1 .
  • 75 mg of multi-walled carbon nanotubes with an outer diameter of 50 nm, an inner diameter of 15 nm, and a length of 10 ⁇ m were added to a humic acid solution with a concentration of 25 mg/mL and a volume of 50 mL, and the solution was ultrasonically treated with an ultrasonic crusher to obtain a concentration of It is 1.5mg/mL modified multi-walled carbon nanotube dispersion, the ultrasonic treatment time is 20min, and the power is 180W.
  • the multi-walled carbon nanotube dispersion was passed through a polyethersulfone membrane with a pore size of 0.5 ⁇ m by the pressure filtration method (the pressure was 0.12 MPa), and then the modified multi-walled carbon nanotubes low-pressure membrane was washed with ultrapure water through the membrane until the water was discharged.
  • the TOC value is lower than 0.2mg/L, and the low-pressure membrane is dried for use. According to the effective area of the polyethersulfone-based membrane and the amount of multi-walled carbon nanotubes, the modified multi-walled carbon nanotubes low-pressure membrane can be calculated, and the loading amount of the modified multi-walled carbon nanotubes is 28 g/m 2 .
  • the multi-walled carbon nanotube dispersion was passed through a polyethersulfone membrane with a pore size of 0.4 ⁇ m by a pressure filtration method (the pressure was 0.08 MPa), and then the modified multi-walled carbon nanotube low-pressure membrane was washed with ultrapure water through the membrane until the water was discharged.
  • the TOC value is lower than 0.2mg/L, and the low-pressure membrane is dried for use. According to the effective area of the polyethersulfone-based membrane and the amount of multi-walled carbon nanotubes, the modified multi-walled carbon nanotubes low-pressure membrane can be calculated, and the loading amount of the modified multi-walled carbon nanotubes is 24 g/m 2 .
  • the modified multi-walled carbon nanotube low-pressure membrane prepared in Example 1 was used to filter the aqueous solutions with methylene blue dye concentrations of 10 mg/L, 20 mg/L, 30 mg/L and 50 mg/L using a constant current filter device, respectively.
  • the flow rate was 70L ⁇ m -2 ⁇ h -1
  • the filtration time was 200min
  • the speed of the peristaltic pump was 0.5r/min
  • the pH value of the methylene blue dye-containing aqueous solution was 7.
  • the aqueous solutions with methylene blue dye concentrations of 10 mg/L, 20 mg/L, 30 mg/L and 50 mg/L were filtered using a polyethersulfone-based membrane with a pore size of 0.45 ⁇ m (the polyethersulfone-based membrane was exactly the same as in Example 1), and the constant current
  • the filtering conditions are the same as in Application Example 1.
  • the unmodified original multi-walled carbon nanotube membranes (multi-walled carbon nanotubes were the same as those in Example 1) were used to filter aqueous solutions with methylene blue dye concentrations of 10 mg/L, 20 mg/L, 30 mg/L and 50 mg/L, respectively.
  • the conditions for stream filtering are the same as in Application Example 1.
  • Figure 4 shows the changes in the transmembrane pressure difference of the modified multi-wall carbon nanotube low-pressure membrane, the polyethersulfone-based membrane, and the unmodified pristine multi-wall carbon nanotube membrane.
  • the transmembrane pressure difference of the modified MWCNTs low-pressure membrane for filtration of methylene blue dye is higher, but much lower than that of nanofiltration and reverse osmosis membranes Pressure difference
  • the transmembrane pressure difference of the modified multi-walled carbon nanotube low pressure membrane of the present invention still belongs to the operation category of the low pressure membrane.
  • the modified multi-walled carbon nanotube low-pressure membrane prepared in Example 1 was used to filter the aqueous solutions containing methylene blue dye with pH values of 3.38, 5.93 and 10.2, respectively. -2 ⁇ h -1 , the filtration time was 200 min, the rotational speed of the peristaltic pump was 0.5 r/min, and the concentration of methylene blue was 50 mg/L.
  • multi-walled carbon nanotubes are the same as in Example 1 to filter aqueous solutions containing methylene blue dye with pH values of 3.38, 5.93 and 10.2, respectively, conditions and application examples of constant flow filtration 3 is the same.
  • the modified multi-walled carbon nanotube low-pressure membrane prepared in Example 1 is used to filter the methylene blue aqueous solution containing Na + (Na + from NaCl) with a concentration of 0, 5mmol/L and 10mmol/L using a constant current filter device.
  • the concentration of methylene blue was 50mg/L
  • the pH value was 10.2.
  • the flow rate was 70L ⁇ m -2 ⁇ h -1
  • the filtration time was 200min
  • the speed of the peristaltic pump was 0.5r/min.
  • the unmodified original multi-walled carbon nanotube membrane (multi-walled carbon nanotubes are the same as in Example 1) was used to filter methylene blue aqueous solutions containing Na + concentrations of 0, 5 mmol/L and 10 mmol/L, respectively, under constant flow filtration conditions Same as application example 4.
  • the effect of Na + concentration on the removal effect of methylene blue is shown in FIG. 6 . It can be seen from FIG. 6 that the effect of Na + concentration on the removal effect of methylene blue by the modified multi-walled carbon nanotube low-pressure membrane of the present invention is very small, indicating that the modification of the present invention
  • the removal of methylene blue by the low-pressure membrane of multi-walled carbon nanotubes is not limited by the concentration of Na + in the solution.
  • the modified multi-walled carbon nanotube low-pressure membrane prepared in Example 1 was used to filter the methylene blue aqueous solution containing Ca 2+ (Ca 2+ from CaCl 2 ) with a concentration of 0, 1 mmol/L and 5 mmol/L using a constant-current filter device,
  • the concentration of methylene blue is 50 mg/L
  • the pH value is 10.2.
  • the flow rate was 70L ⁇ m -2 ⁇ h -1
  • the filtration time was 200min
  • the speed of the peristaltic pump was 0.5r/min.
  • the unmodified original multi-walled carbon nanotube membranes (multi-walled carbon nanotubes were the same as those in Example 1) were used to filter methylene blue aqueous solutions containing Ca concentrations of 0, 1 mmol/L and 5 mmol/L, respectively.
  • the conditions are the same as in Application Example 5.

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  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
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  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
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Abstract

L'invention concerne un procédé de préparation d'un nanotube de carbone à parois multiples modifié, le procédé comprenant : la soumission d'un nanotube de carbone à parois multiples et d'une solution d'acide humique à un traitement par ultrasons pour obtenir une dispersion de nanotube de carbone à parois multiples modifié ; et l'élimination du solvant de la dispersion de nanotube de carbone à parois multiples modifié pour obtenir le nanotube de carbone à parois multiples modifié. En outre, la dispersion de nanotube de carbone à parois multiples modifié est soumise à une séparation solide-liquide à l'aide d'une membrane poreuse de microfiltration pour obtenir une membrane basse pression de nanotube de carbone à parois multiples modifié. Le procédé de préparation ne provoque pas d'endommagement de la structure et des propriétés du nanotube de carbone à parois multiples ; de plus, le risque écologique lié à l'entrée d'un nanotube de carbone à parois multiples dans un environnement aqueux est évité. Le nanotube de carbone à parois multiples modifié et la membrane basse pression de celui-ci sont utilisés pour éliminer un colorant au bleu de méthylène d'une solution aqueuse et le procédé d'élimination est simple, facile à mettre en œuvre, à faible coût et hautement efficace.
PCT/CN2021/130182 2021-04-14 2021-11-12 Nanotube de carbone à parois multiples modifié, membrane à basse pression associée, procédé de préparation associé et utilisation associée WO2022217906A1 (fr)

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