CN115487837B - Nanocomposite prepared by loading titanium dioxide on deep sea rare earth-rich clay - Google Patents

Nanocomposite prepared by loading titanium dioxide on deep sea rare earth-rich clay Download PDF

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CN115487837B
CN115487837B CN202211261187.1A CN202211261187A CN115487837B CN 115487837 B CN115487837 B CN 115487837B CN 202211261187 A CN202211261187 A CN 202211261187A CN 115487837 B CN115487837 B CN 115487837B
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rare earth
clay
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CN115487837A (en
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张培萍
张龙宇
石学法
黄牧
于淼
刘彤彤
于金生
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Jilin University
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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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/14—Phosphorus; Compounds thereof
    • B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
    • B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • 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
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • 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
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/10—Photocatalysts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

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  • Materials Engineering (AREA)
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Abstract

The invention relates to a nanocomposite prepared by loading titanium dioxide on deep sea rare earth-rich clay. The deep sea rare earth-rich clay is utilized to have a mesoporous structure (the specific surface area is 80m 2 ·g ‑1 About, the average pore diameter is 7.4nm, and the pore volume is about 0.145cm 3 ·g ‑1 ) The method has the characteristics of being rich in rare earth elements, and the like, and is used for modifying TiO deposited between and on the surface of the lamellar clay by dissolving out the rare earth elements in the clay in the synthesis process 2 A nanocomposite material having high photocatalytic properties is obtained. The test shows that the removal rate of the prepared nanocomposite to the simulated pollutant RhB solution with the concentration of 10mg/L reaches more than 99%, and the effect is higher than that of commercial TiO prepared by the same mass method 2 (P25)。

Description

Nanocomposite prepared by loading titanium dioxide on deep sea rare earth-rich clay
Technical Field
The invention relates to a nanocomposite material which is prepared by loading deep sea rare earth-rich clay with titanium dioxide, has good photocatalytic performance and can be used for purifying sewage.
Background
According to the existing research, the deep sea sediment which has large area of super-normal enrichment of medium-heavy rare earth elements in deep sea basin and takes clay minerals as main components is a novel marine mineral resource with huge resource potential and application potential. The lithology laws, bi Dongjie, huang Mu, in vast, luo Yiming, zhou Tiancheng, zhang Zhaoqi, liu Jihua, geological report, 2021,40 (Z1): 195-208, in the deep sea rare earth distribution law and mineralisation "one herein indicates that in pacific alone sediments, the amount of rare earth resources in deep sea rare earth-rich clay is 1000 times more than the total amount of known rare earth resources on land, and in pacific western is more found to be up to 6000 x 10 -6 Clay sample of (a). Because of the unique deep sea environment, the deep sea rare earth-rich clay has the characteristics of fine particles and poor crystallization, and is a potential high-quality mesoporous loading material.
Titanium dioxide (TiO) 2 ) Is the earliest sent outThe present invention relates to a semiconductor with photodegradation effect, which makes the research of the photocatalytic effect of the semiconductor enter a new era. TiO (titanium dioxide) 2 Although having the advantages of corrosion resistance, innocuity, durability and low cost, can decompose CO 2 The catalyst has strong catalytic potential in the applications of organic pollutants, harmful gases, hydrogen production from pyrolysis water and the like, but the wider forbidden band (3.0-3.2 eV) enables the catalyst to absorb only the ultraviolet light part accounting for 4 percent of sunlight, thus limiting the preparation of pure TiO 2 And (3) utilizing sunlight.
The TiO can be improved by doping metal ions 2 Photocatalytic efficiency, wherein rare earth ions can cause TiO after doping due to unique 4f electronic structure 2 Lattice defects and lattice distortions form trapping centers capable of inhibiting the recombination of photo-generated electrons and holes, form doping levels, and reduce TiO 2 Is a band gap of (c). Such as Lin Xiahui, wang Zhangming, rogown, ding Wenming, university of Guizhou, university of teachers, 2015,33 (05): 96-99, in "Sm 3+ Doped nano TiO 2 The preparation of (C) and its visible light photocatalytic performance "are indicated herein as Sm 3+ To TiO at a doping level of 1% 2 The modification effect of (2) was optimal, and after irradiation with visible light for 3 hours, the degradation rate of 100mg of the prepared catalyst to 100mL of a rhodamine B solution with a concentration of 20ppm was 80%. In addition, the clay may be TiO 2 Providing a large number of surface active sites, which allows clay/modified TiO 2 Nanocomposite to TiO 2 Has higher catalytic activity. At present, clay is loaded with rare earth metal ion modified TiO 2 Less research as photocatalysts, e.g., soldiers, yang Jintian, zhang Linping, university of Huzhou academy of education, 2006 (01): 64-67, in "neodymium doped TiO 2 In the introduction, "investigation of the immobilization and photocatalytic activity thereof", indicates that when TiO 2 When the proportion of doped neodymium in the catalyst is about 0.1%, the synthesized load type doped neodymium TiO 2 The photocatalyst has the best degradation effect on phenol, and under the irradiation of ultraviolet light for 1h, the degradation rate of 6mg of the photocatalyst on 100ml of phenol water solution with the concentration of 6mg/L is 86%. SHEN Boxiong, YAO Yan, MA Hongqing, LIU Ting CHINESE JOURNAL OF CATALYSIS, 2011,32:1803-1811, in "Ceria Modified MnO x /TiO 2 -Pillared Clays Catalysts for the Selective Catalytic Reduction of NO with NH 3 at Low Temperature A titanium-base column clay is prepared by ion exchange method, and doped ions Ce and Mn are introduced in the subsequent process to obtain a catalyst with abundant mesoporous structure and larger specific surface area, wherein 8% Mn-2% Ce/TiO 2 The PILC has a NO removal of 95% at 200 ℃. However, in the prior clay, modified TiO is loaded 2 In the report, rare earth metal ions used for doping are all TiO-loaded on clay 2 The clay as a carrier is also often purified by several layers of procedures, which allows for the synthesis of clay/TiO 2 The manufacturing cost of the photocatalyst increases. The deep sea rare earth-rich clay has poor crystallization, the rare earth is uniformly distributed in the clay carrier, the clay structure can be slightly destroyed under milder conditions, and the rare earth oxide in the clay is in the form of ions in the solution, thereby realizing the synthesis of TiO 2 Into the crystal lattice forcing TiO 2 The lattice is distorted to form additional doping energy level, thereby realizing one-step synthesis of clay-loaded modified TiO 2 A photocatalyst. However, there is no existing method for loading rare earth-rich clay in deep sea with TiO 2 The chemical compositions of the deep sea rare earth-rich clay used in the present patent are shown in table 1.
TABLE 1 chemical composition (wt%) of deep sea rare earth-rich clay
Disclosure of Invention
1. The invention uses deep sea rare earth-rich clay as mesoporous material to load nano TiO 2 The photocatalytic material with strong degradation capability is prepared, and the loading capacity is 40mg clay/TiO of 25 percent 2 Nanocomposite samples (containing 10 mgTiO) 2 ) At neutral pH, 10ml of the simulated contaminant dye rhodamine B (RHB) with the concentration of 10mg/L can be completely removed within 90 min.
2. To achieve the effect of 1, a certain mass of deep sea rare earth-rich clay needs to be dispersed in deionized water in advanceStirring and carrying out ultrasonic treatment to obtain the deep sea rare earth-enriched clay suspension with the mass fraction of 2%. Pouring titanium sulfate into deep sea rare earth-rich clay suspension, stirring until the suspension is completely dissolved, then placing the suspension into a constant-temperature water bath dry pot, gradually heating to 80 ℃, stirring for 3 hours, and transferring the suspension onto a magnetic stirring table after the constant-temperature water bath for 3 hours. Weighing NaOH solution with the mass of 10 times of that of titanium sulfate and the concentration of 1mol/L, slowly dripping the NaOH solution into the clay suspension, adjusting the pH of the system, and stirring for 30min. Transferring the stirred suspension into a polytetrafluoroethylene-lined reaction kettle, reacting for 6-12h at 120-180 ℃, pouring out supernatant after the reaction, centrifuging with deionized water, washing a sample for 3 times, then placing in a drying oven, drying at 80 ℃, and grinding to obtain a final composite product. TiO can be obtained by adjusting the adding amount of titanium sulfate (75-300% of clay mass) 2 The mass of the photocatalytic material is 20% -50% of the mass of the composite body.
Advantageous effects
1. The invention provides a new application way of deep sea rare earth-rich clay, reasonably uses the rare earth-rich crystallization difference of the deep sea clay, has the characteristic of mesoporous structure, and realizes TiO in the compounding process 2 Doping treatment improves the added value of the deep sea rare earth-rich clay, and has great significance for fully developing and utilizing ocean resources.
2. Deep sea rare earth-rich clay and TiO 2 The nano composite material obtained by combination has good photocatalysis performance and contains TiO with equal mass 2 In the case of (a), the degradation efficiency of RhB solution for treating simulated pollutant is better than that of pure TiO synthesized by the same method 2 . (degradation rate within 180min is 100%)
Detailed Description
The invention aims at realizing the following technical scheme:
1 preparing deep sea rare earth-rich clay/TiO 2 A nanocomposite.
1) Dispersing deep sea rare earth-rich clay in distilled water through a magnetic stirrer to form clay suspension with the mass fraction of 2%, and then placing the suspension into an ultrasonic cleaner for ultrasonic treatment.
2) Weighing titanium sulfate with the mass of 75-300% of that of the deep sea rare earth-rich clay, pouring the titanium sulfate into the treated clay suspension, and stirring for a period of time at room temperature to completely dissolve the titanium sulfate.
3) Transferring the suspension to a constant-temperature water bath kettle, stirring for 3 hours at 80 ℃, after the constant-temperature water bath is finished, dropwise adding the prepared NaOH solution (1 mol/L, the mass is 10 times of that of the titanium sulfate) into the suspension, and transferring the suspension to a magnetic stirring table for stirring for a period of time.
4) Filling the sample into a reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle into an oven, and heating for 6-12h at 120-180 ℃.
5) The supernatant was separated by centrifugation, and the obtained precipitate was repeatedly washed three times with distilled water by centrifugation.
6) The washed sample was placed in an oven and incubated at 80 c until the sample was dried.
2. And (3) testing the photocatalytic performance of the composite material: preparing 10mg/L RhB aqueous solution, placing 10ml into 20ml glass bottle with cover, adding prepared sample, and ensuring that all prepared samples contain TiO with equal mass (10 mg) 2 . Adding a magnet into the bottle, closing the bottle cap, and stirring for 2 hours in a dark state until the sample reaches adsorption equilibrium on the RhB. And simulating visible light by adopting an LED lamp with the power of 50W, and irradiating RhB at a position 15cm away from the sample to perform a photodegradation experiment. The absorbance curve of the simulated pollutant RhB in the range of 700nm-400nm is measured by an ultraviolet spectrophotometer, and the initial absorbance value C of 10mg/L RhB at 554nm and the absorbance value C0 of the solution after the RhB is adsorbed by the sample are respectively recorded. Subsequently, 3ml of the solution was taken every 10min, the absorbance of the simulated contamination solution, once catalytically degraded, was measured and noted as Ct, and the solution was immediately poured back after measurement. The method for calculating the removal rate (eta) of the RhB by the samples at different time in the degradation process is as follows:
adsorption percentage η0 (%) =100 (C-C0)/C
Percent degradation η (%) =100 (C-Ct)/C
Example 1
(1) Through a magnetic stirrer, 0.6g of deep sea rare earth-rich clay is uniformly dispersed in 30ml of distilled water, and then the suspension is put into an ultrasonic cleaner and is subjected to ultrasonic treatment for 10min, so that the deep sea rare earth-rich clay sheet is completely opened.
(2) 0.6g of titanium sulfate is poured into 30ml of deep sea rare earth-rich clay suspension and stirred for 30min at room temperature to completely dissolve the titanium sulfate.
(3) Transferring the suspension to a constant-temperature water bath kettle, stirring for 3 hours at 80 ℃, after the constant-temperature water bath is finished, dropwise adding 6ml of prepared NaOH solution (1 mol/L) into the suspension, and transferring the suspension to a magnetic stirring table for stirring for 30 minutes.
(4) The sample was filled into a reaction kettle with a polytetrafluoroethylene liner, and the reaction kettle was placed in an oven and heated at 160 ℃ for 12 hours.
(5) The reacted sample was poured into a centrifuge tube, centrifuged at 5000RPM for 3 minutes, and repeatedly centrifuged and washed 3 times with distilled water until the excess ions in the solution were removed.
(6) The washed sample was placed in an oven and incubated at 80℃for 7h until the sample was dried.
(7) The initial concentration of 10mg/L RhB solution and the absorbance value at 554nm of the adsorption saturation for 2h were measured and designated as C and C0, respectively. The absorbance at 554nm was then measured every 10min and recorded as Ct and quickly returned after measurement until removal was complete. The adsorption rate of the sample to RhB is calculated to be 52.4%, and the removal rate within 90min is calculated to be 100%.
Example 2
(1) Through a magnetic stirrer, 0.6g of deep sea rare earth-rich clay is uniformly dispersed in 30ml of distilled water, and then the suspension is put into an ultrasonic cleaner and is subjected to ultrasonic treatment for 10min, so that the deep sea rare earth-rich clay sheet is completely opened.
(2) 0.45g of titanium sulfate was poured into 30ml of deep sea rare earth-rich clay suspension and stirred at room temperature for 30min to completely dissolve the titanium sulfate.
(3) Transferring the suspension to a constant-temperature water bath kettle, stirring for 3 hours at 80 ℃, after the constant-temperature water bath is finished, dropwise adding 4.5ml of prepared NaOH solution (1 mol/L) into the suspension, and transferring the suspension to a magnetic stirring table for stirring for 30 minutes.
(4) The sample was filled into a reaction kettle with a polytetrafluoroethylene liner, and the reaction kettle was placed in an oven and heated at 160 ℃ for 12 hours.
(5) The reacted sample was poured into a centrifuge tube, centrifuged at 5000RPM for 3 minutes, and repeatedly centrifuged and washed 3 times with distilled water until the excess ions in the solution were removed.
(6) The washed sample was placed in an oven and incubated at 80℃for 7h until the sample was dried.
(7) The initial concentration of 10mg/L RhB solution and the absorbance value at 554nm of the adsorption saturation for 2h were measured and designated as C and C0, respectively. The absorbance at 554nm was then measured every 10min and recorded as Ct and quickly returned after measurement until removal was complete. The adsorption rate of the sample to RhB is calculated to be about 66%, and the removal rate within 100min is 99.4%.
Example 3
(1) Through a magnetic stirrer, 0.6g of deep sea rare earth-rich clay is uniformly dispersed in 30ml of distilled water, and then the suspension is put into an ultrasonic cleaner for 10 minutes, so that the deep sea rare earth-rich clay sheet is completely opened.
(2) 1.8g of titanium sulfate was poured into 30ml of deep sea rare earth-rich clay suspension and stirred at room temperature for 30min to completely dissolve the titanium sulfate.
(3) Transferring the suspension to a constant-temperature water bath kettle, stirring for 3 hours at 80 ℃, after the constant-temperature water bath is finished, dropwise adding 18ml of prepared NaOH solution (1 mol/L) into the suspension, and transferring the suspension to a magnetic stirring table for stirring for 30 minutes.
(4) The sample was filled into a reaction kettle with a polytetrafluoroethylene liner, and the reaction kettle was placed in an oven and heated at 160 ℃ for 12 hours.
(5) The reacted sample was poured into a centrifuge tube, centrifuged at 5000RPM for 3 minutes, and repeatedly centrifuged and washed 3 times with distilled water until the excess ions in the solution were removed.
(6) The washed sample was placed in an oven and incubated at 80℃for 7h until the sample was dried.
(7) The initial concentration of 10mg/L RhB solution and the absorbance value at 554nm of the adsorption saturation for 2h were measured and designated as C and C0, respectively. The absorbance at 554nm was then measured every 10min and recorded as Ct and quickly returned after measurement until removal was complete. The adsorption rate of the sample to RhB is calculated to be about 34%, and the removal rate within 120min is 100%.

Claims (1)

1. The nanocomposite prepared by loading titanium dioxide on deep sea rare earth-rich clay is characterized in that: the specific surface area of the carrier can reach 80m 2 ·g -1 Average pore diameter of 7.4nm and pore volume of 0.145cm 3 ·g -1 And is TiO in the synthesis process 2 Providing rare earth elements required for modification; the removal rate of rhodamine B RhB with the concentration of 10mg/L by the prepared nano composite material is more than 99 percent; firstly, expanding and dispersing deep sea rare earth-rich clay: dispersing deep-sea rare earth-rich clay with a certain mass in deionized water, stirring for a certain time, and then placing the mixture into an ultrasonic cleaner for ultrasonic treatment for 10min so as to obtain 2wt% of fully-expanded deep-sea rare earth-rich clay suspension; the following formulation is required: the mass ratio of the titanium sulfate to the NaOH solution of 1mol/L is 1:10, the mass of the titanium sulfate is 75-300% of the mass of the clay, and the generated TiO is prepared 2 Accounting for 20 to 50 percent of the complex; pouring titanium sulfate into deep sea rare earth-rich clay suspension, stirring until the titanium sulfate is completely dissolved, then placing the suspension into a constant-temperature water bath dry pot, gradually heating to 80 ℃, and stirring for 3 hours; after the constant-temperature water bath is carried out for 3 hours, transferring the suspension to a magnetic stirring table, slowly dripping the prepared NaOH solution into the suspension to adjust the pH, and stirring for 30 minutes; transferring the stirred suspension into a polytetrafluoroethylene-lined reaction kettle, reacting for 12 hours at 160 ℃, pouring out supernatant after the reaction is finished, centrifuging with deionized water, washing a sample for 3 times, then placing the sample into a drying box, drying at 80 ℃, and grinding to obtain a final composite product.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100861085B1 (en) * 2008-04-16 2008-09-30 허연무 Coating material possible to emit negative ion and its manufacturing method
JP2009096964A (en) * 2007-10-17 2009-05-07 I Think:Kk Material and method for removing heavy metal using quartz diorite porphyry
CN105797762A (en) * 2016-04-06 2016-07-27 苏磊 Photocatalytic ceramsite as well as preparation method and application thereof
CN106492886A (en) * 2016-10-13 2017-03-15 东华大学 A kind of methods for making and using same of mixing rare metal catalyst
CN111013565A (en) * 2019-12-25 2020-04-17 常州大学 Ytterbium and erbium doped titanium dioxide/attapulgite nano composite material and preparation method and application thereof
CN113797890A (en) * 2021-10-11 2021-12-17 吉林大学 Method for preparing catalytic and adsorption material from deep sea clay

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009096964A (en) * 2007-10-17 2009-05-07 I Think:Kk Material and method for removing heavy metal using quartz diorite porphyry
KR100861085B1 (en) * 2008-04-16 2008-09-30 허연무 Coating material possible to emit negative ion and its manufacturing method
CN105797762A (en) * 2016-04-06 2016-07-27 苏磊 Photocatalytic ceramsite as well as preparation method and application thereof
CN106492886A (en) * 2016-10-13 2017-03-15 东华大学 A kind of methods for making and using same of mixing rare metal catalyst
CN111013565A (en) * 2019-12-25 2020-04-17 常州大学 Ytterbium and erbium doped titanium dioxide/attapulgite nano composite material and preparation method and application thereof
CN113797890A (en) * 2021-10-11 2021-12-17 吉林大学 Method for preparing catalytic and adsorption material from deep sea clay

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