CN112028103B - Carbon functionalized Pr 6 O 11 Preparation method of (1) - Google Patents

Carbon functionalized Pr 6 O 11 Preparation method of (1) Download PDF

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CN112028103B
CN112028103B CN202010839082.4A CN202010839082A CN112028103B CN 112028103 B CN112028103 B CN 112028103B CN 202010839082 A CN202010839082 A CN 202010839082A CN 112028103 B CN112028103 B CN 112028103B
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acid dye
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CN112028103A (en
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郝仕油
商娟
伍轩逸
肖忠连
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Xingzhi College of Zhejiang Normal University
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    • 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
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    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
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Abstract

The invention relates to a preparation method of carbon functionalized praseodymium oxide, which comprises the following steps: firstly, a certain amount of Pr (NO) is dissolved in an acid dye solution 3 ) 3 ·6H 2 Adding ammonia water, adjusting the pH value of the solution to a certain range, aging the mixed solution for a certain time, filtering and drying; and then, under the protection of nitrogen, controlling the heating rate of the dried sample, heating to a certain temperature, calcining the mixture for a certain time, and cooling to room temperature to obtain the carbon-functionalized praseodymium oxide material.

Description

Carbon functionalized Pr 6 O 11 Preparation method of (1)
Technical Field
The invention belongs to the technical field of composite oxide preparation, and particularly relates to carbon functionalized Pr 6 O 11 The preparation method of (1).
Background
"Green water Qingshan, namely Jinshan and Yinshan", this explains that a good ecological environment plays a decisive role in human survival. However, with the industrialization of the past decades, the environment is greatly damaged, and organic pollutants, heavy metal ions, carbon dioxide, and the like greatly break the environmental balance. In order to remove the above-mentioned environmental destructive substances, many methods such as adsorption method, membrane separation method, photocatalytic method, etc. have been proposed. Among these methods, the photocatalytic method is favored by researchers because of its low cost, easy operation, and capability of removing environmental pollutants more thoroughly. (Shima H, Hossain M M, Lee I, et al. Mater. chem. Phy., 2017,185: 73-82; Tahir MB, Kiran H, Iqbal T, environ. Sci. Pollutit. R.,2019,26: 10515-.
Numerous studies have shown that the main factors affecting the photocatalytic efficiency are as follows: (1) the absorption efficiency of the catalyst to light, particularly visible light; (2) the adsorption efficiency of the catalyst on pollutants; (3) the yield and separation efficiency of photo-generated electrons and holes. Therefore, in response to the above factors, researchers have proposed various measures to improve photocatalytic efficiency. The material has high adsorption and absorption efficiency on pollutants and visible light and is good for photo-generated electronsConductors, carbon materials, e.g. graphene, C 3 N 4 Activated carbon, etc., are attracting much attention. (ZHang S, Li B F, Wang X X, et al. chem. Eng.J.,2020,390: 124642; Florent M, Giannakoudakis D A, Bandosz T J, appl.Catal.B,2020,172: 119038; Devi TB, Mohanta D, Ahmaruzzaman M, J.Ind. Eng.chem.,2019,76: 160-)
In all rare earth elements, praseodymium oxide has a number of different phases and has different oxygen concentrations (Abu-Zied B M, appl. Surf. Sci.,2019,471: 246-255). At normal temperature and pressure, Pr 6 O 11 The most stable is a typical n-type semiconductor, and the forbidden band width is 1.7-3.3 eV. Therefore, it has a better photocatalytic efficiency (Karunakaran C, hanalaksimi R D, radiat. Phys. chem.,2009,78: 8-12; Zinatloo-Ajabshir S, Salaviti-Niasari M, New J. chem.,2015,39, 3948-. To further improve Pr 6 O 11 Photocatalytic efficiency of (3), synthetic carbon functionalized Pr 6 O 11 Is an effective way. Shnde et al are as C 3 N 4 As a carbon source, synthesize Pr 6 O 11 /g-C 3 N 4 The photocatalytic efficiency of the composite material is greatly higher than that of pure Pr 6 O 11 Or g-C 3 N 4 In (1). (blend A G, Ghugal S G, Vidyasagar D, mater. Res. Bull.,2018,107:154-
In the existing chinese patent literature, the relevant patents disclosing the preparation method of carbon-functionalized rare earth oxides are as follows:
CN106206068A 'preparation method of carbon nanotube composite nano cerium dioxide electrode material', discloses a method for preparing electrode material by Ce (NO) 3 ) 3 ·6H 2 O, polyvinylpyrrolidone and modified carbon nanotubes as raw materials, and a hydrothermal method is utilized to prepare the carbon nanotube composite nano cerium dioxide electrode material.
CN107335422A 'preparation method of carbon functionalized cerium oxide', discloses a method for preparing cerium oxide by Ce (NO) 3 ) 3 ·6H 2 Synthesizing CeO by taking O as a raw material and ammonia water as a precipitator 2 ·xH 2 O, adsorbing the dye (dye) in the dye solution to form CeO 2 ·xH 2 O @ dye by high temperature calcination of CeO 2 ·xH 2 O @ dye, a process for preparing carbon functionalized ceria.
CN101264883 "preparation method of core-shell structure composite material of rare earth metal oxide and carbon nanotube", discloses a method for preparing homogeneous core-shell structure composite material of rare earth metal oxide and carbon nanotube, which comprises uniformly dispersing carbon nanotube in ethylene glycol solution of rare earth nitrate and polyvinylpyrrolidone, heating and refluxing to coat the surface of carbon nanotube with rare earth metal oxide, thereby forming core-shell structure.
As can be seen from the above documents, the carbon materials used in the preparation of carbon-functionalized rare earth oxides are generally commercial products (e.g., C) 3 N 4 Carbon nano tubes) which have weak binding force with rare earth oxides, easily cause the blocking of photoelectron conduction between the interfaces of the rare earth oxides and carbon materials, and reduce the separation efficiency of photoelectrons and cavities; in addition, although dye is used as a carbon source to synthesize the carbon-functionalized rare earth oxide, the method firstly synthesizes a precursor of the rare earth oxide, then adsorbs the dye, and synthesizes a target product through calcination, so that the rare earth oxide and the carbon in the final product cannot be uniformly dispersed, and the carbon bond forming efficiency and the photocatalytic degradation efficiency of the product are influenced. Aiming at the problems, the invention adopts Pr (NO) 3 ) 3 ·6H 2 O is rare earth raw material, and is uniformly dissolved in acid dye solution, ammonia water is used as precipitator, and the pH value of the solution is controlled to ensure that Pr (OH) 3 Uniformly separate out from the solution with the acid dye, so that Pr (OH) in the precursor 3 Is uniformly dispersed with acid dye, and after calcination, Pr 6 O 11 And carbon is also uniformly dispersed. Therefore, the carbon obtained by decomposition of the acid dye is easily reacted with Pr during calcination 6 O 11 The oxygen and praseodymium in the catalyst form a carbon bond, which is beneficial to the transmission of photo-generated electrons to the surface of the catalyst and related substances (such as O) 2 、H 2 O 2 ) Formation of active species (e.g. of
Figure BDA0002640751740000021
·HO 2 HO, etc.),thereby catalyzing and degrading the dye completely. In addition, the uniform dispersion of carbon and rare earth oxide is beneficial to the absorption of the product to visible light, and the yield of photo-generated electrons and holes is improved, so that the photocatalytic efficiency of the product is improved.
Up to now, NO patent and related literature reports the utilization of Pr (NO) 3 ) 3 ·6H 2 O and acid dye are taken as raw materials, and Pr (OH) is uniformly separated out simultaneously 3 With acid dye, the carbon functionalized Pr with higher photocatalytic efficiency is prepared by adjusting the calcination temperature 6 O 11 。
Disclosure of Invention
The invention aims to provide a preparation method of carbon functionalized praseodymium oxide which has high photocatalytic degradation efficiency on organic matters (acid red 14 is used as a probe molecule).
In order to solve the technical problem, the technical scheme adopted by the invention is as follows:
a preparation method of carbon functionalized praseodymium oxide comprises the following steps:
1) taking a certain amount of Pr (NO) 3 ) 3 ·6H 2 Dissolving O in a certain amount of acid dye solution, and stirring to dissolve the O into a uniformly mixed solution;
2) at Pr (NO) 3 ) 3 Adding NH with the mass percent of 25 percent into the mixed solution of the acid dye dropwise with stirring 3 ·H 2 O, adjusting the pH value of the solution, and then aging for 2-4 h;
3) filtering, washing with water, washing with alcohol, and oven drying the aged mixture to obtain carbon-functionalized Pr 6 O 11 A precursor;
4) placing the precursor in a tube furnace, heating to a certain temperature at a heating rate of 4-6 ℃/min under the protection of nitrogen, keeping the temperature for 3-4h, and naturally cooling to room temperature to obtain the carbon functionalized Pr 6 O 11 A material.
In the above preparation process, Pr (NO) 3 ) 3 ·6H 2 And O is completely dissolved in the acid dye solution to form a uniformly mixed solution.
Controlling Pr (NO) during the above preparation process 3 ) 3 ·6H 2 O andthe acid dye quantity and the purpose of adjusting the pH value of the solution are to ensure that Pr (OH) 3 And the acid dye is completely separated out of the solution at the same time.
In the preparation process, carbon functionalized Pr with higher photocatalytic efficiency is obtained 6 O 11 The material takes acid dye red 14 and acid orange 7 as carbon sources.
In the preparation process, the aim of controlling the calcination temperature is to synthesize the carbon functionalized Pr with better photocatalytic efficiency 6 O 11 A material.
Compared with the prior art, the invention has the following outstanding characteristics and effects: in the present invention, Pr (NO) 3 ) 3 ·6H 2 O is completely dissolved in the acid dye solution by regulating the pH value of the solution, Pr (OH) 3 Precipitating out from the solution simultaneously with the acid dye; due to Pr (NO) 3 ) 3 ·6H 2 O and the acid dye form a uniform mixed solution, and are uniformly mixed with each other when they are precipitated from the solution, and carbon and Pr are obtained as a product after calcination 6 O 11 Also homogeneously mixed; due to the acidic dye and Pr (NO) 3 ) 3 ·6H 2 O is uniformly separated out from the solution, so that carbon converted from the acid dye is easy to form carbon bonds with Pr and O during calcination, and photoproduction electron transfer is facilitated; because the product contains carbon and Pr 6 O 11 Is uniformly mixed, so the product has higher absorption to visible light; compared with the prior art, the method has the advantages of ingenious, simple and feasible design and high-efficiency removal effect on pollutants such as dye and the like. From XRD (figure 1), the synthesized product has Pr at crystal planes of (111), (200) and (220) 6 O 11 The characteristic peak of the synthesized product is proved to be Pr when the corresponding crystal peak position is consistent with a standard card (JCPDS File number-00-042- 6 O 11 . After carbon functionalization, the absorption intensity of the sample to ultraviolet-visible light is higher than that of the pure sample (see the attached figure 2 for details). From the C1s XPS chart (fig. 3a), it can be seen that in the Carbon-functionalized sample, there are distinct peaks at 284.5, 285.9, 288.1, 289.3eV, which can be assigned to C-O, C-C, C ═ C, etc. bonds (Teng CC, Ma CCM, Lu CH, et al, Carbon,2011,49:5107-5116) to prove that the carbon bond exists in the material, which is beneficial to the separation of the photo-generated electrons and the holes, so that the fluorescence emission spectrum intensity of the carbon functionalized material is weaker (FIG. 3 b). After carbon functionalization, Pr 6 O 11 The adsorption efficiency to the dye is improved, and the absorption intensity to visible light is increased; after the carbon bond is formed, the separation of photoproduction electrons and holes is facilitated; therefore, the synthesized sample has better photocatalytic degradation efficiency to the related dye (acid red 14) (see the detailed figure 4).
In conclusion, the carbon-functionalized praseodymium oxide prepared by the invention has the advantages of high dye adsorption capacity, high light absorption (especially visible light absorption) intensity, capability of efficiently separating photoproduction electrons from holes by a formed carbon bond and capability of efficiently degrading acid red 14 by using visible light, so that the carbon-functionalized praseodymium oxide has potential application value in the aspect of photocatalytic degradation of organic pollutants.
Drawings
FIG. 1 Pr 6 O 11 And C-Pr 6 O 11 XRD pattern of (a);
FIG. 2 Pr 6 O 11 And C-Pr 6 O 11 Ultraviolet-visible absorption diagram of (a);
FIG. 3C-Pr 6 O 11 C1s XPS (a) and Pr of (1) 6 O 11 And C-Pr 6 O 11 Graph (b) of fluorescence spectrum of (c);
FIG. 4 shows Pr under irradiation of visible light 6 O 11 And C-Pr 6 O 11 Graph of catalytic degradation efficiency for acid red 14 (acid red 14 solution concentration 0.2mM, volume 20mL, catalyst mass 20mg, pH 6).
Detailed Description
The production process of the present invention is further illustrated by the following examples, but the present invention is not limited to the following examples.
Example 1
Taking 0.8g of Pr (NO) 3 ) 3 ·6H 2 Dissolving O in 80mL of acid dye solution with the concentration of 0.05mmol/L, and stirring to dissolve the O to form uniformly mixed solution; at Pr (NO) 3 ) 3 Adding NH with the mass percentage of 25 percent into the acid dye mixed solution while stirring 3 ·H 2 O, adjusting the pH value of the solution to 8.0, and then aging for 2 hours; filtering, washing with water, washing with alcohol, and oven drying the aged mixture to obtain carbon-functionalized Pr 6 O 11 A precursor; placing the precursor in a tube furnace, heating to 550 ℃ at the heating rate of 4 ℃/min under the protection of nitrogen, keeping the temperature for 3 hours, and naturally cooling to room temperature to obtain the carbon functionalized Pr 6 O 11 A material.
Example 2
Taking 0.8g of Pr (NO) 3 ) 3 ·6H 2 Dissolving O in 100mL of acid dye solution with the concentration of 0.75mmol/L, and stirring to dissolve the O to form uniformly mixed solution; at Pr (NO) 3 ) 3 Adding NH with the mass percentage of 25 percent into the acid dye mixed solution while stirring 3 ·H 2 O, adjusting the pH value of the solution to 8.5, and then aging for 3 hours; filtering, washing with water, washing with alcohol, and oven drying the aged mixture to obtain carbon-functionalized Pr 6 O 11 A precursor; placing the precursor in a tube furnace, heating to 600 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen, keeping the temperature for 3.5h, and naturally cooling to room temperature to obtain the carbon functionalized Pr 6 O 11 A material.
Example 3
Taking 0.8g of Pr (NO) 3 ) 3 ·6H 2 Dissolving O in 120mL of acid dye solution with the concentration of 0.10mmol/L, and stirring to dissolve the O to form uniformly mixed solution; at Pr (NO) 3 ) 3 Adding NH with the mass percentage of 25 percent into the acid dye mixed solution while stirring 3 ·H 2 O, adjusting the pH value of the solution to 9.5, and then aging for 4 h; filtering, washing with water, washing with alcohol, and oven drying the aged mixture to obtain carbon-functionalized Pr 6 O 11 A precursor; placing the precursor in a tube furnace, heating to 650 ℃ at the heating rate of 6 ℃/min under the protection of nitrogen, keeping the temperature for 4 hours, and naturally cooling to room temperature to obtain the carbon functionalized Pr 6 O 11 A material.
Example 4
Taking 1.0g of Pr (NO) 3 ) 3 ·6H 2 Dissolving O in 80mL of acid dye solution with the concentration of 0.05mmol/L, stirring to dissolve the O to form uniform mixtureCombining the solution; at Pr (NO) 3 ) 3 Adding NH with the mass percentage of 25 percent into the acid dye mixed solution while stirring 3 ·H 2 O, adjusting the pH value of the solution to 8.0, and then aging for 2 h; filtering, washing with water, washing with alcohol, and oven drying the aged mixture to obtain carbon-functionalized Pr 6 O 11 A precursor; placing the precursor in a tube furnace, heating to 550 ℃ at the heating rate of 4 ℃/min under the protection of nitrogen, keeping the temperature for 3 hours, and naturally cooling to room temperature to obtain the carbon functionalized Pr 6 O 11 A material.
Example 5
1.0g of Pr (NO) 3 ) 3 ·6H 2 Dissolving O in 100mL of acid dye solution with the concentration of 0.75mmol/L, and stirring to dissolve the O to form uniformly mixed solution; at Pr (NO) 3 ) 3 Adding NH with the mass percentage of 25 percent into the acid dye mixed solution while stirring 3 ·H 2 O, adjusting the pH value of the solution to 8.5, and then aging for 3 hours; filtering, washing with water, washing with alcohol, and oven drying the aging mixture to obtain carbon-functionalized Pr 6 O 11 A precursor; placing the precursor in a tube furnace, heating to 600 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen, keeping the temperature for 3.5h, and naturally cooling to room temperature to obtain the carbon functionalized Pr 6 O 11 A material.
Example 6
Taking 1.0g of Pr (NO) 3 ) 3 ·6H 2 Dissolving O in 120mL of acid dye solution with the concentration of 0.10mmol/L, and stirring to dissolve the O to form uniformly mixed solution; at Pr (NO) 3 ) 3 Adding NH with the mass percentage of 25 percent into the acid dye mixed solution while stirring 3 ·H 2 O, adjusting the pH value of the solution to 9.5, and then aging for 4 h; filtering, washing with water, washing with alcohol, and oven drying the aged mixture to obtain carbon-functionalized Pr 6 O 11 A precursor; placing the precursor in a tube furnace, heating to 650 ℃ at the heating rate of 6 ℃/min under the protection of nitrogen, keeping the temperature for 4 hours, and naturally cooling to room temperature to obtain the carbon functionalized Pr 6 O 11 A material.
Example 7
Taking 1.2g of Pr (NO) 3 ) 3 ·6H 2 Dissolving O in 80mL of acid dye solution with the concentration of 0.05mmol/L, and stirring to dissolve the O to form uniformly mixed solution; at Pr (NO) 3 ) 3 Adding NH with the mass percentage of 25 percent into the acid dye mixed solution while stirring 3 ·H 2 O, adjusting the pH value of the solution to 8.0, and then aging for 2 h; filtering, washing with water, washing with alcohol, and oven drying the aged mixture to obtain carbon-functionalized Pr 6 O 11 A precursor; placing the precursor in a tube furnace, heating to 550 ℃ at the heating rate of 4 ℃/min under the protection of nitrogen, keeping the temperature for 3 hours, and naturally cooling to room temperature to obtain the carbon functionalized Pr 6 O 11 A material.
Example 8
Taking 1.2g of Pr (NO) 3 ) 3 ·6H 2 Dissolving O in 100mL of acid dye solution with the concentration of 0.75mmol/L, and stirring to dissolve the O to form uniformly mixed solution; at Pr (NO) 3 ) 3 Adding NH with the mass percentage of 25 percent into the acid dye mixed solution while stirring 3 ·H 2 O, adjusting the pH value of the solution to 8.5, and then aging for 3 h; filtering, washing with water, washing with alcohol, and oven drying the aged mixture to obtain carbon-functionalized Pr 6 O 11 A precursor; placing the precursor in a tube furnace, heating to 600 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen, keeping the temperature for 3.5h, and naturally cooling to room temperature to obtain the carbon functionalized Pr 6 O 11 A material.
Example 9
Taking 1.2g of Pr (NO) 3 ) 3 ·6H 2 Dissolving O in 120mL of acid dye solution with the concentration of 0.10mmol/L, and stirring to dissolve the O to form uniformly mixed solution; at Pr (NO) 3 ) 3 Adding NH with the mass percent of 25 percent into the mixed solution of the acid dye dropwise with stirring 3 ·H 2 O, adjusting the pH value of the solution to 9.5, and then aging for 4 h; filtering, washing with water, washing with alcohol, and oven drying the aged mixture to obtain carbon-functionalized Pr 6 O 11 A precursor; placing the precursor in a tube furnace, heating to 650 ℃ at the heating rate of 6 ℃/min under the protection of nitrogen, keeping the temperature for 4 hours, and naturally cooling to room temperatureObtaining carbon functionalized Pr 6 O 11 A material.

Claims (7)

1. Carbon functionalized Pr 6 O 11 The preparation method is characterized by comprising the following steps:
1) taking a certain amount of Pr (NO) 3 ) 3 ·6H 2 Dissolving O in a certain amount of acid dye solution, and stirring to dissolve the O to form a mixed solution;
2) at Pr (NO) 3 ) 3 Adding NH with the mass percentage of 25 percent into the acid dye mixed solution while stirring 3 ·H 2 O, adjusting the pH value of the solution, and then aging for 2-4 h;
3) filtering, washing with water, washing with alcohol, and oven drying the aged mixture to obtain carbon-functionalized Pr 6 O 11 A precursor;
4) placing the precursor in a tube furnace, heating to a certain temperature at a heating rate of 4-6 ℃/min under the protection of nitrogen, keeping the temperature for 3-4h, and naturally cooling to room temperature to obtain the carbon functionalized Pr 6 O 11 A material.
2. The method of claim 1, wherein: in the above preparation process, Pr (NO) 3 ) 3 ·6H 2 The amount of O is 0.8-1.2 g.
3. The method of claim 1, wherein: in the preparation process, the acid dye is one or two of acid red 14 and acid orange 7, the concentration of the acid dye is 0.05-0.10mmol/L, and the volume of the acid dye is 80-120 mL.
4. The method of claim 1, wherein: in the above preparation process, Pr (NO) 3 ) 3 ·6H 2 And O is fully dissolved in the acid dye solution to form a uniformly dispersed mixed solution.
5. The production method according to claim 1, characterized in that: in the above-mentioned preparation process, useNH 3 ·H 2 O adjusting the pH value of the mixed solution to 8.0-9.5 to ensure that Pr (OH) 3 And the acid dye is uniformly separated out of the solution at the same time.
6. The method of claim 1, wherein: in the preparation process, Pr (OH) in the precursor 3 Is uniformly dispersed with acid dye, and after calcination, Pr 6 O 11 And carbon is also uniformly dispersed.
7. The method of claim 1, wherein: in the preparation process, the calcination temperature of the precursor is 550-650 ℃.
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CN1884088A (en) * 2005-06-21 2006-12-27 浙江师范大学 Technology for preparing ultrafine nano metal oxide materials
CN101717108A (en) * 2009-11-12 2010-06-02 济南大学 Industrial preparation method of rare earth hydrate and oxide nano-rod
CN105713610A (en) * 2015-06-14 2016-06-29 重庆品鉴光电工程有限公司 Preparation method of fluorescent powder for single-chip white LED
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