CN115025747B - High-performance PH 3 Preparation method, product and application of adsorbent - Google Patents
High-performance PH 3 Preparation method, product and application of adsorbent Download PDFInfo
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- 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
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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Abstract
The invention discloses a high-performance PH 3 A preparation method, a product and application of an adsorbent relate to the technical field of air pollution control. The method comprises the following steps: carrying out hydrothermal reaction on the mixed aqueous solution of Cu salt and Ce salt to obtain CuO-CeO 2 A precursor; for the CuO-CeO 2 Calcining the precursor to obtain the high-performance PH 3 An adsorbent. The method has the advantages of simple operation, rich raw materials, wide sources, easy realization of industrial application and good application prospect. The bi-component CuO-CeO prepared by the method of the invention 2 High performance PH 3 The adsorbent has the appearance similar to walnut shape and the surface of the adsorbent is rough, so that more pores are generated, the specific surface area and active sites are increased, the adsorption of phosphine molecules is facilitated, and the PH can be realized under the condition of low temperature oxygen-free atmosphere 3 Is removed with high efficiency and stability and PH 3 The penetration capacity is high.
Description
Technical Field
The invention relates to the technical field of air pollution control, in particular to a high-performance PH 3 Preparation method, product and application of adsorbent.
Background
Yellow phosphorus is a chemical industryIn the industry, the important products are 2500-3000 m in theory when 1t yellow phosphorus is produced by using an electric furnace method 3 The yellow phosphorus tail gas mainly consists of CO (85% -90%), and has higher heat value. But because the yellow phosphorus tail gas contains PH besides CO 3 Equal impurity, PH 3 The existence of the catalyst is extremely easy to cause poisoning and deactivation of various catalysts in the carbon chemical industry, in particular to noble metal catalysts such as palladium, rhodium, ruthenium and the like. In addition, pH 3 The combined mechanism of toxicity is still unclear, and no effective antidote or therapeutic method is found. PH value 3 Enters the human body mainly through the respiratory tract and is then distributed throughout the body through the blood. Inhalation pH 3 Can affect the heart, respiratory system, kidney, intestines and stomach, nervous system, liver, etc. Long-term exposure to low pH 3 Symptoms such as dizziness, headache, insomnia, general weakness, inappetence, nausea and the like can occur, and the PH with higher concentration is contacted 3 Can directly lead to death of the adult. Yellow phosphorus tail gas, domestic methane, landfill gas, semiconductor photoelectric industry tail gas and the like are PH 3 Is the main source of (a). However, in the last few decades, pH 3 Emission problems are still lacking in importance in some areas. Therefore, in order to fully implement the cyclic economy concept and construct the resource efficient cyclic utilization system, and to fully ensure human health and solve the ecological environment problem, the PH existing in each tail gas must be treated 3 And (5) effectively removing.
For PH at home and abroad 3 The related art researches on high-efficiency removal are also deficient, and the gas-solid adsorption method, the adsorption-oxidation method and the catalytic decomposition method are representative PH at present 3 A purifying and removing method. However, the present representative purification and removal methods still have larger defects and shortages, such as higher working temperature of the catalytic decomposition method>420 ℃ and the catalyst is easy to be poisoned and deactivated. Also, the adsorption-oxidation method, although considered as a very potential and effective solution, has major problems (poor adsorption performance, long preparation period, etc.) in developing and using the adsorbent currently studied, and the adsorbent developed based on the adsorption-oxidation method is difficult to meet the current practical industrial application demands.
Thus, a pH having a short preparation period and excellent adsorption performance is provided 3 The preparation method of the adsorbent has important significance for the technical field of air pollution control.
Disclosure of Invention
Based on the foregoing, the present invention provides a high performance PH 3 Preparation method, product and application of adsorbent. The method firstly utilizes a simple hydrothermal method to synthesize the precursor, then the precursor is calcined to finally obtain the CuO-CeO 2 High performance PH 3 An adsorbent. The preparation process uses pure water as a solvent, so that the environmental protection and economic benefits of the preparation process are further ensured. Has the characteristics of short preparation period and good adsorption performance.
In order to achieve the above object, the present invention provides the following solutions:
one of the technical schemes of the invention is a high-performance PH 3 The preparation method of the adsorbent comprises the following steps:
carrying out hydrothermal reaction on the mixed aqueous solution of Cu salt and Ce salt to obtain CuO-CeO 2 A precursor;
for the CuO-CeO 2 Calcining the precursor to obtain the high-performance PH 3 An adsorbent.
Further, cu in the mixed aqueous solution 2+ With Ce 3+ The molar ratio of (2) is 15:1-25:1. The purpose is to add a proper amount of rare earth element cerium on the surface of the adsorbent to further enhance the adsorption performance of the adsorbent.
Further, cu in the mixed aqueous solution 2+ The concentration of (C) is 0.05mol/L to 0.15mol/L.
Further, the Cu salt is Cu (CH) 3 COO) 2 The method comprises the steps of carrying out a first treatment on the surface of the The Ce salt is Ce (CH) 3 COO) 3 。
Further, a carbonate solution is added to the mixed aqueous solution before the hydrothermal reaction is performed.
Further, CO in carbonate solution 2 3 - The concentration of (2) is 0.2-0.5mol/L; CO in solution 2 3 - With Cu 2+ The molar ratio of (2) is 4:5-3:2. The carbonate solution is added to provide CO 2 3 - The purpose is to ensure adequate synthesis of the precursor.
Further, the carbonate solution is Na 2 CO 3 Solution, K 2 CO 3 One of the solutions.
Further, the temperature of the hydrothermal reaction is 120-160 ℃ and the time is 10-13 h.
Further, after the hydrothermal reaction is finished, the method further comprises the steps of centrifugally separating, washing the generated precursor for 2-3 times by using distilled water and absolute ethyl alcohol, and drying at 50-80 ℃ for 7-9 hours.
Further, the calcination treatment specifically includes: calcining in air at 300-600 deg.c for 3-4 hr. Aims to fully synthesize the bi-component CuO-CeO 2 High performance PH 3 The adsorbent is used for further enhancing the specific surface area of the adsorbent and improving the adsorption performance.
In the second technical scheme of the invention, the high-performance PH prepared by the preparation method 3 An adsorbent.
In a third aspect of the present invention, the high-performance PH 3 Adsorption-oxidation removal of PH from adsorbents 3 Is used in the field of applications.
Further, the conditions of the adsorption-oxidation removal are as follows: an oxygen-free atmosphere at 30-150deg.C.
The invention discloses the following technical effects:
the method synthesizes the precursor by a simple hydrothermal method, and then calcines the precursor. The addition of Ce salt can lead the CuO to be dispersed more uniformly, prevent the aggregation of single CuO particles, lead the specific surface area of single copper oxide particles to be smaller, lead the aggregation phenomenon to directly influence the specific surface area of the adsorbent, and lead the addition of Ce to play an important role in the uniform dispersion of copper. At the same time, due to CuO and CeO 2 The strong interaction between the two components finally leads the prepared adsorbent to be walnut-like in shape, and the special spherical coarse structure of the adsorbent can generate more pores and active sites, thereby being beneficial to the adsorption of phosphine molecules. The method of the invention uses pure water as solvent, which takes account ofEnvironmental protection and economy. The method has the advantages of simple operation, rich raw materials, wide sources, easy realization of industrial application and good application prospect.
The bi-component CuO-CeO prepared by the method of the invention 2 High performance PH 3 The adsorbent has walnut-like appearance and rough surface, so that more pores are generated, the specific surface area and active sites of the adsorbent are increased, the adsorption of phosphine molecules is facilitated, and the PH can be realized under the condition of low-temperature oxygen-free atmosphere 3 Is removed with high efficiency and stability and PH 3 The penetration capacity is high. The test results of test example 2 show that the high performance PH prepared by the invention 3 The adsorbent is used for PH under low temperature and oxygen-free condition 3 The removal efficiency is maintained above 97%, the time is up to 360min, and the phosphorus content is up to 272.8mg (PH) 3 ) Per g (adsorbent), illustrating the high performance pH provided by the present invention 3 The adsorbent is used for PH under low temperature and oxygen-free condition 3 The method has the advantages of high removal efficiency, long penetration time, large phosphorus capacity and excellent overall adsorption performance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 shows the high performance pH of example 1 3 Microcosmic topography of the adsorbent;
FIG. 2 shows the high performance pH of example 1 3 Microcosmic topography of the adsorbent;
FIG. 3 shows the high performance pH of example 1 3 Adsorbent, conventional solid copper oxide adsorbent prepared in example 2 and conventional solid CuO-CeO prepared in example 3 2 Adsorbent pair pH 3 Is a graph of the removal effect of (c).
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
As used herein, the term "room temperature" refers to 20-25℃unless otherwise specified.
EXAMPLE 1 high Performance PH 3 Preparation of adsorbents
(1) Cu (CH) was disposed at a concentration of 0.1mol/L 3 COO) 2 ·H 2 O solution, ce (CH) 3 COO) 3 Controlling Cu in solution 2+ With Ce 3+ The molar ratio of (2) was 20:1.
(2) Adding 0.3mol/LNa to the solution of step (1) 2 CO 3 Solution, control CO in solution 2 3 - With Cu 2+ The molar ratio of (2) is 1:1.
(3) And (3) placing the solution obtained in the step (2) into a reaction kettle, reacting for 12 hours at 140 ℃, centrifuging after the reaction is finished and cooling, washing the generated precursor with distilled water and absolute ethyl alcohol for 3 times, and drying for 8 hours at 60 ℃.
(4) Calcining the product obtained after the drying in the step (3) for 3 hours in air at 400 ℃, and cooling to room temperature to obtain CuO-CeO 2 High performance PH 3 An adsorbent.
CuO-CeO prepared in this example 2 High performance PH 3 The specific surface area of the adsorbent was 41.93m 2 ·g -1 ) Pore volume of 0.16cm 3 ·g -1 。
EXAMPLE 2 preparation of a conventional copper oxide configuration adsorbent
The nano copper oxide powder (99.5 percent, 40nm, shanghai Michelia Biochemical technology Co., ltd.) is subjected to tabletting treatment (15 MPa,45 s) to prepare the pure copper oxide adsorbent with the particle diameter of 40-60 meshes.
EXAMPLE 3 traditional solid CuO-CeO 2 Preparation of adsorbents
In this example, a grinding method was used to prepare the conventional solid CuO-CeO 2 An adsorbent. Nanometer cerium oxide (99.9%, 50nm, shanghai Meilin Biochemical Co., ltd.) and nanometer copper oxide (99.5%, 40nm, shanghai Meilin Biochemical Co., ltd.) were mixed according to Cu 2+ With Ce 3+ The molar ratio of CuO to CeO is 20:1 2 After mixing together, the mixture was thoroughly ground to homogeneity in an agate mortar. And then CuO and CeO are added 2 Calcining the mixture in air at 400 ℃ for 3 hours, cooling to room temperature, tabletting the product (15 MPa,45 s) to obtain the traditional solid CuO-CeO with the particle diameter of 40-60 meshes 2 An adsorbent.
EXAMPLE 4 high Performance PH 3 Preparation of adsorbents
(1) Cu (CH) was disposed at a concentration of 0.05mol/L 3 COO) 2 ·H 2 O solution, ce (CH) 3 COO) 3 Controlling Cu in solution 2+ With Ce 3+ The molar ratio of (2) was 15:1.
(2) Adding 0.25mol/LNa to the solution of step (1) 2 CO 3 Solution, control CO in solution - 3 2 With Cu 2+ The molar ratio of (2) was 4:5.
(3) And (3) placing the solution obtained in the step (2) into a reaction kettle, reacting for 13 hours at the temperature of 100 ℃, centrifuging after the reaction is finished and cooling, washing the generated precursor for 2 times by using distilled water and absolute ethyl alcohol, and drying for 9 hours at the temperature of 50 ℃.
(4) Calcining the product obtained after the drying in the step (3) for 4 hours in air at the temperature of 300 ℃, and cooling to room temperature to obtain CuO-CeO 2 High performance PH 3 An adsorbent.
CuO-CeO prepared in this example 2 High performance PH 3 The specific surface area of the adsorbent was 26.28m 2 ·g -1 Pore volume of 0.082cm 3 ·g -1 . For PH 3 The removal efficiency was maintained at 97% or more for 150min, and the phosphorus content was 113.6mg (pH 3 ) /g (adsorbent).
EXAMPLE 5 high Performance PH 3 Preparation of adsorbents
(1) Cu (CH) was disposed at a concentration of 0.15mol/L 3 COO) 2 ·H 2 O solution, ce (CH) 3 COO) 3 Controlling Cu in solution 2+ With Ce 3+ The molar ratio of (2) was 25:1.
(2) Adding 0.5mol/LNa to the solution of step (1) 2 CO 3 Solution, control CO in solution - 3 2 With Cu 2+ The molar ratio of (2) was 6:5.
(3) And (3) placing the solution obtained in the step (2) into a reaction kettle, reacting for 10 hours at 160 ℃, centrifuging after the reaction is finished and cooling, washing the generated precursor for 3 times by using distilled water and absolute ethyl alcohol, and drying for 7 hours at 80 ℃.
(4) Calcining the product obtained after the drying in the step (3) for 3 hours in air at 600 ℃, and cooling to room temperature to obtain CuO-CeO 2 High performance PH 3 An adsorbent.
CuO-CeO prepared in this example 2 High performance PH 3 Specific surface area of adsorbent 30.15m 2 ·g -1 Pore volume of 0.13cm 3 ·g -1 . For PH 3 The removal efficiency was maintained at 97% or more for 240min, and the phosphorus content was 159.2mg (pH 3 ) /g (adsorbent).
EXAMPLE 6 high Performance PH 3 Preparation of adsorbents
(1) Cu (CH) was disposed at a concentration of 0.1mol/L 3 COO) 2 ·H 2 O solution, ce (CH) 3 COO) 3 Controlling Cu in solution 2+ With Ce 3+ The molar ratio of (2) was 22:1.
(2) Adding 0.3mol/LNa to the solution of step (1) 2 CO 3 Solution, control CO in solution 2 3 - With Cu 2+ The molar ratio of (2) was 13:10.
(3) And (3) placing the solution obtained in the step (2) into a reaction kettle, reacting for 12 hours at 150 ℃, centrifuging after the reaction is finished and cooling, washing the generated precursor for 3 times by using distilled water and absolute ethyl alcohol, and drying for 8 hours at 60 ℃.
(4) Calcining the product obtained after the drying in the step (3) for 3 hours in air at 500 ℃, and cooling to room temperature to obtain CuO-CeO 2 High performance PH 3 An adsorbent.
CuO-CeO prepared in this example 2 High performance PH 3 The specific surface area of the adsorbent was 36.74m 2 ·g -1 Pore volume of 0.14cm 3 ·g -1 . For PH 3 The removal efficiency was maintained at 97% or more for 300min, and the phosphorus content was 227.4mg (pH 3 ) /g (adsorbent).
Test example 1
For the CuO-CeO prepared in example 1 2 High performance PH 3 The adsorbents were subjected to physicochemical characterization analysis, wherein the high performance pH was obtained by scanning electron microscopy (Gemini 300, zeiss, germany) 3 Microcosmic morphology information of the adsorbent. 5-10 mg of the adsorbent prepared in example 1 is weighed each time, the adsorbent particles to be tested are stuck on the conductive adhesive for sample preparation, and all samples are subjected to Pt metal spraying treatment before the test so as to enhance the surface conductivity, and the operation voltage is 3.00kV.
FIGS. 1 and 2 show CuO-CeO prepared in example 1 2 High performance PH 3 Microcosmic topography of the adsorbent. As can be seen from fig. 1 and fig. 2, the material prepared in example 1 has a walnut-like morphology and a rough surface of the adsorbent, so that more pores are generated, the specific surface area and active sites are increased, the adsorption of phosphine molecules is facilitated, and the adsorption performance of the phosphine molecules is obviously improved.
Test example 2
For the high performance pH prepared in example 1 3 Adsorbent (Walnut-shaped CuO-CeO) 2 ) Conventional Solid copper oxide adsorbent (Solid CuO) prepared in example 2 and conventional Solid CuO-CeO prepared in example 3 2 Adsorbent (Solid CuO-CeO) 2 ) Performance testing is carried out, wherein the testing conditions are as follows: PH value 3 The concentration of the adsorbent is 1000ppm, only nitrogen is used as carrier gas, the prepared adsorbent is placed in a fixed bed reactor under the condition of no oxygen atmosphere, and the space velocity is 30000h -1 The reaction temperature is 60 ℃; the reactor inlet and outlet concentrations were measured by gas chromatography.
As shown in FIG. 3, it can be seen from FIG. 3 that the high performance pH of example 1 3 Adsorbent (Walnut-shaped CuO-CeO) 2 ) Conventional solid CuO-CeO prepared in example 3 2 Adsorbent (Solid CuO-CeO) 2 ) And conventional Solid copper oxide adsorbent (Solid CuO) vs pH prepared in example 2 3 The removal efficiency of (C) was maintained at 97% or more for 360min, 180min and 120min, respectively, and the phosphorus content was 272.8mg (pH) 3 ) /g (adsorbent), 135.9mg (pH) 3 ) /g (adsorbent) and 90.5mg (pH) 3 ) /g (adsorbent). Wherein the two-component CuO-CeO 2 Walnut shaped adsorbent (i.e. high performance PH) 3 Adsorbent) propertyCan be obviously higher than solid CuO-CeO 2 Adsorbents and solid copper oxide adsorbents.
Test example 3
PH for examples 4 to 6 3 And (3) testing adsorption performance, wherein the test conditions are as follows: PH value 3 The concentration of the adsorbent is 1000ppm, only nitrogen is used as carrier gas, the prepared adsorbent is placed in a fixed bed reactor under the condition of no oxygen atmosphere, and the space velocity is 30000h -1 The reaction temperature is 60 ℃; the reactor inlet and outlet concentrations were measured by gas chromatography.
As is clear from the results of the adsorption performance test of test example 3, examples 4 to 6 were specific to pH 3 The removal efficiency of the catalyst is maintained for more than 97 percent for 150min, 240min and 300min respectively; phosphorus contents of 113.6mg (pH) 3 ) /g (adsorbent), 159.2mg (pH) 3 ) Per g (adsorbent) and 227.4mg (pH) 3 ) /g (adsorbent). It can be seen that when the conditions for preparing the adsorbent are in accordance with the ranges set forth in the claims of the present invention, the prepared high-performance adsorbent has a specific pH 3 All have relatively excellent adsorptivity; however, when the conditions for the preparation do not meet the ranges of the present invention, the prepared adsorbent has a pH value 3 The adsorption performance of (2) is obviously reduced. For example, in comparison to examples 5 and 6, example 4, the hydrothermal temperature at which the sorbent precursor is synthesized results in example 4 versus pH due to the non-compliance with the hydrothermal temperature range (120-160 ℃) referred to in the claims of the present invention 3 Is inferior in adsorption performance even lower than the conventional solid CuO-CeO prepared in example 3 2 Adsorbent pair pH 3 Is used for the adsorption performance of the catalyst.
The results of each test example show that the invention provides the bi-component CuO-CeO 2 Walnut-shaped high-performance PH 3 The adsorbent has good adsorption activity and can realize PH under the condition of low temperature and no oxygen 3 High-efficiency stable removal and solving of PH in industrial tail gas 3 Is a problem of emissions. Meanwhile, the preparation method provided by the invention is simple to operate, the preparation time of the adsorbent is relatively short, and meanwhile, pure water is used as a solvent, so that the environmental protection and the economical efficiency are both considered. The high-performance PH prepared by the invention 3 Adsorbents of similar morphologyThe walnut-shaped adsorbent has rough surface, generates more pores and increases specific surface area and active sites, so that the adsorbent has excellent adsorption activity and adsorption selectivity and can be used for PH in various systems 3 Is stable and efficient in removing and purifying. At pH of 3 Compared with the traditional adsorbent, the high-efficiency removal and purification of the double-component CuO-CeO prepared by the invention 2 High performance PH 3 The adsorbent has better adsorption performance due to high specific surface area and high active site, so that the adsorbent has better practical application potential.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (3)
1. Walnut-like adsorbent for removing PH by low-temperature oxidation 3 The application is characterized in that the walnut-like adsorbent is CuO-CeO 2 An adsorbent;
the CuO-CeO 2 The preparation method of the adsorbent comprises the following steps:
carrying out hydrothermal reaction on the mixed aqueous solution of Cu salt and Ce salt to obtain CuO-CeO 2 A precursor;
for the CuO-CeO 2 Calcining the precursor to obtain the CuO-CeO 2 An adsorbent;
cu in the mixed aqueous solution 2+ With Ce 3+ The molar ratio of (2) is 15:1-25:1;
the Cu salt is Cu (CH) 3 COO) 2 The method comprises the steps of carrying out a first treatment on the surface of the The Ce salt is Ce (CH) 3 COO) 3 ；
Adding a carbonate solution to the mixed aqueous solution before performing a hydrothermal reaction;
the temperature of the hydrothermal reaction is 140 ℃ and the time is 10-13 hours;
the CuO-CeO 2 The adsorbent is in oxygen-free atmosphere at 60deg.C and pH 3 The concentration is 1000ppm,Space velocity of 30000h -1 Under the condition of PH 3 The removal efficiency is maintained at 97% or more for 360min, and the phosphorus content is 272.8mg PH 3 /g adsorbent.
2. The walnut-like adsorbent of claim 1 for removal of PH at low temperature oxidation 3 Is characterized in that in the carbonate solutionThe concentration of (2) is 0.2-0.5mol/L; in solution->With Cu 2+ The molar ratio of (2) is 4:5-3:2.
3. The walnut-like adsorbent of claim 1 for removal of PH at low temperature oxidation 3 The application of (3) is characterized in that the calcination treatment is specifically as follows: and calcining for 3-4 hours in air at the temperature of 300-600 ℃.
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