CN114149021B - Method for preparing nano cerium from eastern beauty tea extract and application of nano cerium - Google Patents
Method for preparing nano cerium from eastern beauty tea extract and application of nano cerium Download PDFInfo
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- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 68
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 241001122767 Theaceae Species 0.000 title claims abstract 12
- 238000000034 method Methods 0.000 title abstract description 18
- 230000003796 beauty Effects 0.000 title abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 28
- 235000014347 soups Nutrition 0.000 claims abstract description 27
- 238000001354 calcination Methods 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 13
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000001179 sorption measurement Methods 0.000 claims description 76
- 239000002245 particle Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 9
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical group [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 150000002910 rare earth metals Chemical class 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 13
- 238000003786 synthesis reaction Methods 0.000 abstract description 11
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 abstract description 6
- 238000003980 solgel method Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 150000008442 polyphenolic compounds Chemical class 0.000 abstract description 5
- 235000013824 polyphenols Nutrition 0.000 abstract description 4
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 abstract description 3
- 150000001413 amino acids Chemical class 0.000 abstract description 3
- 229960001948 caffeine Drugs 0.000 abstract description 3
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 abstract description 3
- -1 cerium ions Chemical class 0.000 abstract description 3
- 239000000084 colloidal system Substances 0.000 abstract description 3
- 238000010668 complexation reaction Methods 0.000 abstract description 3
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 abstract description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 abstract description 2
- 244000269722 Thea sinensis Species 0.000 description 61
- 235000013616 tea Nutrition 0.000 description 60
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 description 57
- 230000000694 effects Effects 0.000 description 21
- 239000000243 solution Substances 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 13
- 229910000420 cerium oxide Inorganic materials 0.000 description 11
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 9
- 239000013078 crystal Substances 0.000 description 9
- 238000001069 Raman spectroscopy Methods 0.000 description 6
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- 238000002360 preparation method Methods 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 5
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- 239000002086 nanomaterial Substances 0.000 description 5
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- 238000005265 energy consumption Methods 0.000 description 2
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- 229910044991 metal oxide Inorganic materials 0.000 description 2
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- 239000012695 Ce precursor Substances 0.000 description 1
- 238000005169 Debye-Scherrer Methods 0.000 description 1
- IPMYMEWFZKHGAX-UHFFFAOYSA-N Isotheaflavin Natural products OC1CC2=C(O)C=C(O)C=C2OC1C(C1=C2)=CC(O)=C(O)C1=C(O)C(=O)C=C2C1C(O)CC2=C(O)C=C(O)C=C2O1 IPMYMEWFZKHGAX-UHFFFAOYSA-N 0.000 description 1
- UXRMWRBWCAGDQB-UHFFFAOYSA-N Theaflavin Natural products C1=CC(C2C(CC3=C(O)C=C(O)C=C3O2)O)=C(O)C(=O)C2=C1C(C1OC3=CC(O)=CC(O)=C3CC1O)=CC(O)=C2O UXRMWRBWCAGDQB-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
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- 239000010436 fluorite Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 235000009569 green tea Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
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- 235000014620 theaflavin Nutrition 0.000 description 1
- IPMYMEWFZKHGAX-ZKSIBHASSA-N theaflavin Chemical compound C1=C2C([C@H]3OC4=CC(O)=CC(O)=C4C[C@H]3O)=CC(O)=C(O)C2=C(O)C(=O)C=C1[C@@H]1[C@H](O)CC2=C(O)C=C(O)C=C2O1 IPMYMEWFZKHGAX-ZKSIBHASSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a method for preparing nano cerium from an eastern beauty tea extract and application thereof, which is used for green synthesis of nano cerium dioxide by a sol-gel method and specifically comprises the following steps: and heating the tea powder in a water bath, cooling, filtering, mixing the filtrate with cerium chloride, vibrating, baking at a high temperature, and calcining to obtain the nano cerium powder. The rich substances such as tea polyphenol, caffeine, amino acid and the like in the tea can be subjected to complexation with cerium ions, so that the colloid of the solution is realized, and cerium element is changed into a nanoscale state through long-time constant-temperature standing or constant-speed stirring. And green synthesis of nano CeO by tea soup 2 Simple operation, low cost, little pollution to the environment, nano CeO 2 Provides a new method and idea.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a method for preparing nano cerium from an eastern beauty tea extract and application thereof.
Background
The eastern American tea is Chinese traditional famous tea, is native to Taiwan province of China, and is rich in tea polyphenols, caffeine, amino acids and other substances in the tea can be subjected to complexation with cerium ions, so that the colloid of the solution is realized, and cerium element is changed into a nanoscale state through long-time constant-temperature standing or constant-speed stirring. The nano material has the characteristics of high strength, friction resistance and the like, has surface effect and macroscopic quantum tunneling effect, and is applied to the fields of aerospace and the like. Along with development of nano technology, the diameter of nano preparation technology is gradually diversified, and the nano preparation technology is generally classified into a liquid phase method, a gas phase method, a solid phase method and a biological method. Nanometer CeO 2 Often used as a carrier to enhance TiO 2 The photocatalytic performance of (2) can be prepared into a shell coated with TiO by a spray combustion method 2 Nano CeO of film 2 The composite oxide particles can prepare CeO with good monodispersity by adopting W/O type microemulsion to effectively couple by an emulsion method and a uniform precipitation method 2 Synthesis of nano CeO by changing current and electrode conditions 2 The electrochemical synthesis of (C) has also been reported by the prior art.
The above study shows that nano CeO 2 There are several synthesis methods, but the sol-gel method is a method with relatively simple operation and low cost, while green synthesis of nano CeO with tea soup 2 Less research is done. The invention is based on the concept of sustainable development of resources and environmental protection, and uses the eastern American tea soup and CeCl 3 Green synthesis of nano CeO from solution 2 The preparation method has little environmental pollution, low cost and easy operation, and is nano CeO 2 Provides a new method and idea
Disclosure of Invention
The invention aims to provide a method for preparing nano cerium from eastern beauty tea extract and application thereof, and nano CeO can be synthesized by green tea soup 2 Preparation ofThe cerium oxide is more stable and ordered in structure and exhibits excellent adsorption performance to the dye.
In order to achieve the above purpose, the present invention provides a method for preparing nano cerium from an eastern beauty tea extract, comprising the following steps:
(1) Crushing eastern American tea leaves, preparing tea soup, heating in a water bath, and stirring;
(2) Cooling the tea soup to room temperature, vacuum filtering, mixing filtrate with cerium chloride, and vibrating for 10-12 h;
(3) Drying the mixed solution prepared in the step (2), and taking the dried matter to calcine and grind to obtain rare earth CeO 2 Nanocrystalline powder.
Further, the heating temperature in the step (1) is 70-90 ℃, and the heating time is 60-80 min.
Further, the stirring time in the step (1) is once every 15min, and each stirring time is 1-2 s.
Further, in the tea soup obtained in the step (1), the tea powder is sieved by a sieve with 80-200 meshes, and the ratio of the tea powder to water is 3-5 g:100mL.
Further, the ratio of the filtrate to cerium chloride in the step (2) is 15-25 mL:0.05mol.
Further, in the step (3), the drying temperature is 100-140 ℃ and the drying time is 20-24 hours.
Further, in the step (3), the calcination temperature is 450-800 ℃ and the calcination time is 2 hours.
Further, the nano cerium is prepared by adopting the method for preparing the nano cerium by the eastern beauty tea extract.
Further, the application of nano cerium in dye adsorption.
In summary, the invention has the following advantages:
1. the invention adopts the traditional famous tea-eastern beauty tea to prepare the nano cerium through a sol-gel method, and substances such as tea polyphenol, caffeine, amino acid and the like which are rich in the tea can be complexed with cerium ions, so that the colloid of the solution is realized, cerium element is changed into a nano-scale state through long-time constant-temperature standing or constant-speed stirring, and the nano structure of the synthesized cerium oxide is more stable and has an ordered structure.
2. The invention uses tea as raw material, utilizes sol-gel method to prepare nano cerium, expands the utilization direction of tea to a certain extent, has little environmental pollution, low cost and easy operation, and is nano CeO 2 Provides a new method and idea.
3. The nano cerium prepared by the invention has excellent adsorption performance in Congo red adsorption tests, has good agglomeration phenomenon and stability, has good spherical and hexahedral fluorite structures, takes Ce (IV) as a main surface valence state, and has a particle size range of 8.8-11.4nm.
Drawings
FIG. 1 is a standard curve of Congo red;
FIG. 2 is a thermogravimetric analysis map of the nano-cerium prepared in example 1;
FIG. 3 is an XRD pattern of nano-cerium prepared in example 1;
FIG. 4 is a scanning electron microscope image of the nano cerium powder at different calcination temperatures;
wherein, FIG. 4 (a) is 100 ℃, FIG. 4 (b) is 200 ℃, FIG. 4 (c) is 300 ℃, FIG. 4 (d) is 450 ℃, FIG. 4 (e) is 650 ℃, and FIG. 4 (f) is 800 ℃;
FIG. 5 is an XPS spectrum of the nano cerium prepared in example 1;
FIG. 6 is a Raman spectrum analysis of the nano-cerium powder at different calcination temperatures;
FIG. 7 is a graph showing the comparison of the adsorption effect of nano-cerium with commercial nano-cerium at different calcination temperatures;
FIG. 8 is a graph of the adsorption rate of Congo red versus Congo red concentration for nano-cerium and commercial nano-cerium after calcination at 650 ℃;
wherein, fig. 8 (a) is the influence of congo red initial concentration on adsorption rate, and fig. 8 (b) is the influence of congo red initial concentration on adsorption amount;
FIG. 9 is a graph of adsorption rate versus adsorption time for Congo red for nano-cerium and commercial nano-cerium after calcination at 650 ℃;
FIG. 10 is a graph of adsorption rate versus adsorption temperature for Congo red for nano-cerium and commercial nano-cerium after calcination at 650 ℃.
Detailed Description
The principles and features of the present invention are described below in connection with the following examples, which are set forth to illustrate, but are not to be construed as limiting the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The details of the relevant reagents and materials used in the invention are shown in Table 1
TABLE 1 reagents and materials related thereto
Example 1
The embodiment provides a method for preparing nano cerium from eastern beauty tea extract, which comprises the following steps:
(1) Crushing eastern American tea leaves into tea powder by using a crusher, collecting the tea powder for standby, and sieving the tea powder by a 80-mesh sieve;
(2) Mixing tea powder with distilled water to obtain tea soup, heating in electric constant temperature water bath for 1 hr at 80deg.C, and stirring every 15 min;
(3) Cooling the tea soup to room temperature after stirring, filtering by a vacuum pump, and mixing filtrate with cerium chloride, wherein the mixing ratio of the cerium chloride to the tea soup is 0.05mol:20mL;
(4) And (3) oscillating the mixed liquor for 12 hours, placing the mixed liquor in a baking oven at 120 ℃ for drying for 24 hours, placing the dried material in a muffle furnace for high-temperature calcination, taking out the calcined dried material, and grinding to obtain the nano cerium powder.
Example 2
The embodiment provides a method for preparing nano cerium from eastern beauty tea extract, which comprises the following steps:
(1) Crushing eastern American tea leaves into tea powder by using a crusher, collecting the tea powder for standby, and sieving the tea powder with a 150-mesh sieve;
(2) Mixing tea powder with distilled water to obtain tea soup, heating in electric constant temperature water bath for 1 hr at 75deg.C, and stirring every 15 min;
(3) Cooling the tea soup to room temperature after stirring, filtering by a vacuum pump, and mixing filtrate with cerium chloride, wherein the mixing ratio of the cerium chloride to the tea soup is 0.05mol:25mL;
(4) And (3) oscillating the mixed solution for 12 hours, placing the mixed solution in a baking oven at 120 ℃ for drying for 24 hours, placing the dried product in a muffle furnace for high-temperature calcination, taking out the calcined dried product, and grinding to obtain the nano cerium powder.
Example 3
The embodiment provides a method for preparing nano cerium from eastern beauty tea extract, which comprises the following steps:
(1) Crushing eastern American tea leaves into tea powder by using a crusher, collecting the tea powder for standby, and sieving the tea powder by a 200-mesh sieve;
(2) Mixing tea powder with distilled water to obtain tea soup, heating in electric constant temperature water bath for 1 hr at 85deg.C, and stirring every 15 min;
(3) Cooling the tea soup to room temperature after stirring, filtering by a vacuum pump, and mixing filtrate with cerium chloride, wherein the mixing ratio of the cerium chloride to the tea soup is 0.05mol:15mL;
(4) And (3) oscillating the mixed solution for 12 hours, placing the mixed solution in a baking oven at 120 ℃ for drying for 24 hours, placing the dried product in a muffle furnace for high-temperature calcination, taking out the calcined dried product, and grinding to obtain the nano cerium powder.
Test example 1
Congo red degradation experiment
1. Preparation of Congo Red Standard Curve
Accurately weighing 0.1g of Congo red powder, adding distilled water to prepare Congo red mother liquor with concentration of 100mg/L, standing for 10min, diluting the Congo red solution with distilled water to obtain diluted Congo red solutions with concentrations of 2mg/L, 4mg/L, 6mg/L, 8mg/L and 12mg/L, adjusting the wavelength of a spectrophotometer to 497nm, detecting the concentration, recording the measured absorbance, and obtaining a standard curve of Congo red according to the diluted concentration and the corresponding absorbance as shown in figure 1.
2. Experimental procedure
A certain amount of the nano cerium powder prepared in example 1 was weighed by an electronic balance, placed in a 150mL conical flask, placed in a table type constant temperature oscillator, set at 25 ℃ and oscillated for 60min (except for an adsorption time test) under the condition of 200rpm for experiment, sampled after the reaction is finished, centrifuged for 5min at 5000rpm by a high-speed centrifuge, and the absorbance of the supernatant was measured by a spectrophotometer and then substituted into a standard curve for calculating the adsorption rate and adsorption amount of nano cerium to congo red.
R＝(C 0 -C t )/C 0 ×100％
Q t ＝(C 0 -C t )/M×V
Wherein: c (C) 0 For initial Congo red concentration, mg/L;
C t concentration of Congo red at any time, mg/L;
Q t the unit adsorption quantity of nano cerium at any time is mg/g;
v is the volume of the solution, mL;
m is the mass of nano cerium and g.
3. Results and analysis
3.1 characterization results of nano cerium
3.1.1 characterization results of nano cerium
The synthesis temperature of nano cerium oxide is searched, and the cerium sample synthesized by the sol-gel method is measured by using air as carrier gas through TGA/DTA, so that data are shown in figure 2.
As can be seen from FIG. 2, there is a significant loss of weight at 501℃which is CeCl 3 Reaction to produce CeO 2 For reasons of (2). The redox capacity of Ce is also affected by pH, and under weak acid conditions, ce 3+ Is easily oxidized to Ce 4+ At about 500 ℃, the generated energy consumption and reagent loss are used for the metal oxide CeO 2 Is a synthesis of (a).
3.1.2XRD analysis
XRD was used to analyze the decomposition of the gel cerium sample, and fig. 3 is an XRD pattern of the cerium sample. The nanometer cerium precursor synthesized by sol-gel method has relatively disordered crystalline phase and is mainly prepared from CeCl 3 ·7H 2 O、CeCl 3 ·4H 2 O and CeCl 3 ·3H 2 O composition, and the accompanying presence of ambiguous crystalline phases that may result from complexation of polyphenolic compounds and other organics in tea broth during sol-gel. With increasing calcination temperature, the uncertain crystal phase gradually disappears, mainly CeCl at about 300 DEG C 3 There is, at this stage, all the crystallization water has been decomposed. CeO (CeO) 2 The crystal diffraction peak of (2) starts to appear at 400 ℃ and shows a very distinct crystalline phase at 500-800 ℃. The 2 theta values are at 28.2, 33.1, 47.5 and 56.3, corresponding to the ceria face-centered fluorite cubic structure (PFD: 34-0439) of (111), (200), (220), (311). This result is consistent with the TGA measurement, indicating that the formation temperature of cerium oxide was about 500 ℃ in this study. By analyzing the full width at half maximum (FWHM) of the diffraction peak corresponding to the characteristic, the calculation of the nano cerium particle size is carried out by the full width at half maximum value of the diffraction peak corresponding to the Debye-Scherrer formula:
D scherrer ＝0.89λ/(βcosθ)
wherein: lambda is lambda ray wavelength, 0.154nm;
beta is the full width of the diffraction line;
θ is the half diffraction angle.
The results are summarized in Table 2.
TABLE 2 Synthesis of nano-cerium with different calcination temperatures
As can be seen from table 2: the grain size of the nano cerium oxide increases with the rise of temperature, the grain size range is 8.8-11.4nm, the lattice parameter slightly decreases with the increase of the grain size, the numerical value is lower than that of the standard card JCPDS34-0349, the change of the lattice parameter with the grain size can be explained by the relaxation of the grain surface for the nano crystal particles, the nano crystal grain has a core-shell structure, the core structure is very similar to that of bulk monocrystalline cerium oxide, and the lattice parameter locally increases on the surface due to the tendency of the surface relaxation. In addition, it has been found that relaxation of the grain surface contributes to line broadening, thereby reducing the measurement of dislocation density. The gel formed by the compounds such as tea polyphenol, theaflavin, thearubigin in the tea soup extract can make the particles more stable, and reduce the lattice parameter by reducing the relaxation of the particle surface.
3.1.3SEM analysis
To better observe the appearance of the nano cerium, the nano cerium powder obtained at different temperatures for 2 hours was analyzed by a scanning electron microscope to obtain fig. 4. The surface of the sample at 100 ℃ is smoother and flatter, prismatic structure appears at 200 ℃, particles show irregular shape and start to agglomerate at 300 ℃, and along with the rise of the temperature, the crystal phase becomes more obvious, and hexahedral CeO at 450 DEG C 2 Crystal formation, obtaining uniform spherical and hexahedral CeO at 800 DEG C 2 And (3) a sample. The agglomeration phenomenon, which is a common phenomenon in which particles tend to reduce the exposed area to lower the surface energy, is increasingly pronounced at 450-800 c, and when two particles are in contact, the two crystals tend to rotate relative to each other between the lattices to minimize the interfacial energy, so that the crystal planes of the same type tend to align themselves, or form coherent interfaces to reduce the interfacial energy.
3.1.4XPS analysis
To examine the chemical state and valence of cerium, XPS was used to determine the surface composition of the test sample and the spectrum of Ce 3d as shown in FIG. 5. Typical Ce 3d XPS nuclear energy spectra exhibit three spin-orbit bin characteristics (about 879-890eV,895-910eV, and about 916 eV). It consists of six peaks, corresponding to a bimodal pair of spin orbitals, which can be considered to have Ce 3d 5/2 (v) And Ce 3d 3/2 (u) the presence of (a). As shown in fig. 5, the marked v and u correspond to Ce 3d 5/2 And Ce 3d 3/2 Is a structure of (a). The highest binding energy peaks v '"and u'" are from Ce 3d 9 O2p 6 Ce 4f 0 In the final state, the lowest binding energy peaks v ', v ", u' and u" are formed by CeO 2 Provided by Ce 3d 9 O 2p 5 Ce 4f 1 And Ce 3d 9 O 2P 4 Ce 4f 2 Mixing in final state. The transfer of electrons from O2 p to the Ce 4f orbital and the decrease in Ce 3d binding energy is due to the interaction of the Ce 4f energy level with the Ce 3d core hole, which reduces the energy of the Ce 4f energy level. With Ce 3d 3/2 The relevant satellite peak u' "is indicative of the presence of tetravalent Ce (Ce 4+ Ions). All samples represented in fig. 5 present three spin-orbit bin characteristics (6 satellites peak 916.5 eV), indicating Ce (IV) is the predominant form of presence.
3.1.5 Raman Spectroscopy
Raman spectrum analysis of the nano cerium oxide obtained by calcining at different temperatures gave FIG. 6, at 463cm -1 Has a strong peak due to F of cubic fluorite structure of cerium oxide 2g The raman activity mode results from this mode due to Ce-O 8 The symmetrical stretching mode of the vibrating unit is that the molecule maintains its tetrahedral symmetry. This mode is therefore very sensitive to effects induced by heat, doping or grain size in the oxide sub-lattice. No other peaks were detected in the raman spectrum other than the spike.
The symmetrical character of the cerium oxide nanostructures produced by calcination at different temperatures appears to have the same character, and all samples are observed to be asymmetrical, if the oxygenic sublattice is disordered, the raman activity mode is affected by line broadening and an increase in asymmetry, due to a reduction in phonon lifetime in the nanocrystals. Based on XPS and Raman spectroscopy analysis, due to Ce 4+ The nano-structure of cerium oxide synthesized by tea extract is more stable and has an ordered structure.
Test example 2
Adsorption experiment of Congo Red
1. Comparative experiments
To understand the ability of the synthesized nano cerium to be applied to dye adsorption, ceO obtained by calcining at 450 ℃,650 ℃ and 800 ℃ is selected 2 Sample and use commercial CeO 2 In contrast, the experimental conditions were 25mL of Congo red at a concentration of 100mg/L, and 0.25g of synthetic and commercial CeO was added, respectively 2 Shaking at 25deg.C for 1min, centrifuging, collecting supernatant, and measuring in spectrophotometer to obtain adsorption effect as shown in FIG. 7, which shows that CeO at different calcining temperatures can be found 2 The adsorption effect on Congo red is higher than 95%, and is obviously higher than commercial CeO 2 . Nano CeO obtained by synthesizing sufficient tea soup 2 Has high active adsorption efficiency, and commercial CeO can be obviously observed from the appearance after adsorption 2 The adsorption efficiency is lower.
2. Influence of Congo Red initial concentration on adsorption Effect of Congo Red solution
Due to CeO at 450 DEG C 2 The nano crystal is formed initially, a small amount of impurity particles may be mixed in the crystal lattice, ceO at 800 DEG C 2 The nano-crystal may have lattice collapse at high temperature, so we choose CeO which is stable at 650 DEG C 2 The nanocrystals were used as samples for subsequent experiments. 0.25g CeO (calcined at 650 ℃ C. And commercially available) was taken separately 2 The samples were each added to 25mL of Congo red solution (concentrations of 100mg/L, 300mg/L, 600mg/L, 800mg/L, respectively), and the absorbance was measured after shaking at 200rpm for 60min with a constant temperature shaker at 25℃and centrifuging at 5000rpm for 5min with a high-speed refrigerated centrifuge, the adsorption effects of both being shown in FIG. 8. CeO calcined at 650 DEG C 2 The adsorption rate of Congo red has little change along with the increase of concentration of Congo red, and still maintains the adsorption effect exceeding 97.76% when the concentration reaches 800mg/L, which indicates CeO synthesized by tea soup 2 Still has a very strong chemical affinity for congo red. Whereas commercial CeO 2 The adsorption efficiency of (C) was decreased with increasing Congo red solution concentration, especially when the Congo red concentration was increased from 300mg/L to 800mg/L, and the adsorption rate was significantly decreased from 86.23% to 36.33%, presumably to be commercial CeO 2 The number of active sites on the surface and in the pores is smaller, and as the congo red concentration increases, the number of adsorption sites is accelerated to be occupied due to the increase of driving force among congo red molecules. Both have obvious increasing trend on the adsorption quantity of Congo red solution, and CeO calcined at 650 DEG C 2 The adsorption quantity of Congo red is from 9.65mg/g to 78.21mg/g, and the commercial CeO 2 The adsorption amount of Congo red is slowly increased from 9.04mg/g to 29.06mg/g, and Congo red molecules collide with each otherThe frequency rises with the increase of the concentration, the driving force is also enhanced, and the enhancement of the driving force weakens CeO 2 Mass transport resistance of the solid and liquid phases upon adsorption congo red reaction. The cerium sample synthesized by the tea soup has more active sites and dispersibility, has better adsorption effect on Congo red molecules, and has stronger affinity with Congo red due to the fact that cerium on the sample surface is mainly tetravalent.
3. Influence of adsorption time on Congo Red solution adsorption effect
The time gradients were set to 1, 3, 5, 10, 15, 30, 45, 60, 90, 120, 150min. Congo red initial concentration is set to 100mg/L, volume is 25ml, and nano CeO 2 And commercial CeO 2 The amount of the catalyst added was 0.25g, and the reaction temperature was 25 ℃. The difference in adsorption effect was observed from fig. 9. From the figure, it is evident that nano CeO obtained by calcining at 650℃is obtained 2 The adsorption rate of 94.97% can be reached in 1min, and the adsorption rate is stably maintained between 92% and 96% along with the progress of the reaction time, so as to reach the chemical reaction equilibrium stage, which can prove that the reaction equilibrium is reached in 1min, thus proving that the nano CeO 2 The adsorption effect on Congo red is extremely strong. Commercial CeO 2 The adsorption rate of Congo red increases with time, and the adsorption rate increases greatly at the beginning of the reaction and then becomes stable because of the large number of Congo red molecules and commercial CeO at the beginning of the reaction 2 The surface active sites bind and as the reaction proceeds the binding sites tend to saturate and the reaction equilibrates.
4. Influence of temperature on Congo Red solution adsorption Effect
Setting temperature gradient 5, 15, 25, 30, 45 ℃, adding 0.25g CeO obtained by calcining at 650 ℃ into 25mL 100mg/L Congo red solution 2 And commercial CeO 2 Absorbance was measured after shaking the shaker at 60 mm and both adsorption rates and adsorption amounts were plotted by comparative analysis to give fig. 10. As shown, the temperature increases. CeO obtained by calcining at 650 DEG C 2 The adsorption rate and the adsorption quantity of Congo red solution are stable at higher level, the fluctuation is in an error range, the highest adsorption rate and the lowest adsorption rate are respectively 95.89% and 96.58%, and the highest adsorption quantity and the lowest adsorption quantity are respectively9.59mg/g and 9.68mg/g. Commercial CeO 2 As the temperature increases, both the adsorption rate and the adsorption amount tend to increase, probably because the temperature increases, increasing the rate of congo red molecules binding to the adsorption sites, speeding up the adsorption process.
To sum up, nano CeO 2 Has good spherical and hexahedral fluorite structure, the surface valence state is mainly Ce (IV), and the grain diameter range is 8.8-11.4nm. Nanometer CeO synthesized by tea soup 2 The adsorption effect on Congo red is far better than that of commercial nano CeO 2 The nano degradation rate is kept at a higher level with the increase of Congo red concentration, temperature and time, and the adsorption quantity is increased.
At the same time, it can be seen that: (1) Nanometer CeO synthesized by tea soup 2 Has good agglomeration phenomenon and stability, and TGA thermogravimetric analysis shows that there is a large amount of weight loss at 501 ℃ due to CeCl 3 Reaction to produce CeO 2 Under weak acid condition, ce 3+ Is easily oxidized to Ce 4+ About 500 ℃, the generated energy consumption and reagent loss are used for the metal oxide CeO 2 The synthesis was completed at 591 ℃. XRD analysis results show that nano CeO 2 The synthesis is carried out at 400-500 ℃, which is consistent with the analysis result of TGA, and the particle size of the nano-particles is 8.8-11.4nm through formula calculation. SEM analysis showed that agglomeration was increasingly evident at 450-800℃and uniform spherical and hexahedral crystals were obtained at 800℃because planes were present between crystals that rotated relative to each other to tend to be coherent with each other to reduce surface energy. XPS analysis shows that with Ce 3d 3/2 The associated satellite peak u' "is indicative of the presence of tetravalent Ce in the Ce compound, and all samples have three spin-orbit bin characteristics (6 satellite peaks 916.5 eV), indicating Ce (IV) is the predominant form of presence. Raman spectroscopy at 463cm -1 Has a strong peak, which indicates that cerium oxide has a good F2 g Raman activity mode of a cubic fluorite structure, due to Ce-O 8 The symmetrical stretching mode of the vibrating unit keeps tetrahedral symmetry.
(2) Congo red initial concentration versus nano CeO 2 The adsorption effect has less influence
CeO calcined at 650 DEG C 2 For congoThe adsorption rate of red has small change along with the rise of Congo red concentration, and the adsorption effect of the red is still maintained to be more than 97.76% when the concentration reaches 800mg/L, so that CeO synthesized by tea soup is obtained 2 Still has a very strong chemical affinity for congo red. The collision frequency of Congo red molecules increases with the increase of the concentration, the driving force is also enhanced, and the CeO is weakened by the enhancement of the driving force 2 Mass transport resistance of the solid and liquid phases upon adsorption congo red reaction. The cerium sample synthesized by the tea soup has more active sites on the surface and dispersibility, and cerium on the surface of the sample is mainly tetravalent and has stronger affinity with Congo red, thereby being beneficial to the adsorption reaction.
(3) Adsorption time and temperature versus nano CeO 2 Has promoting effect on adsorption effect
Nanometer CeO 2 The adsorption rate of 94.97% can be reached within 1min, the adsorption rate is stabilized between 92% and 96% along with the time, and the nano CeO is increased along with the temperature rise 2 Both the adsorption rate and the adsorption amount for congo red were stable at higher levels and slightly increased, since the increase in temperature promoted the binding rate of congo red molecules to the adsorption sites.
While specific embodiments of the invention have been described in detail, it should not be construed as limiting the scope of the patent. Various modifications and variations which may be made by those skilled in the art without the creative effort are within the scope of the patent described in the claims.
Claims (6)
1. The nano cerium for dye adsorption is characterized in that the nano cerium has a spherical and/or hexahedral fluorite structure, the particle size of the nano cerium is 8.8-11.4nm, the lattice parameter is 0.5405-0.5408 nm, and the surface valence state is IV; the nano cerium is prepared through the following steps:
(1) Crushing eastern American tea leaves, preparing tea soup, heating in a water bath, and stirring;
(2) Cooling the tea soup to room temperature, vacuum filtering, mixing filtrate with cerium chloride, and vibrating for 10-12 h;
(3) Drying the mixed solution prepared in the step (2), taking a dried product, calcining for 2 hours at 450-800 ℃ and grinding to prepare rare earth CeO 2 Nanocrystalline powder.
2. The nano-cerium for dye adsorption according to claim 1, wherein the heating temperature in the step (1) is 70 to 90 ℃ and the heating time is 60 to 80min.
3. The nano-cerium for dye adsorption according to claim 1, wherein the stirring time in the step (1) is one stirring every 15min for 1 to 2s.
4. The nano cerium for dye adsorption according to claim 1, wherein in the tea soup of the step (1), the tea powder is sieved by a sieve of 80-200 meshes, and the ratio of the tea powder to water is 3-5 g:100mL.
5. The nano-cerium for dye adsorption according to claim 1, wherein the ratio of filtrate to cerium chloride in the step (2) is 15 to 25mL:0.05mol.
6. The nano cerium for dye adsorption according to claim 1, wherein the drying temperature in the step (3) is 100 to 140 ℃ and the drying time is 20 to 24 hours.
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