CN112915963A - Method for preparing cobalt phosphide/biochar composite material by taking yeast nucleic acid as phosphorus source and carbon source - Google Patents
Method for preparing cobalt phosphide/biochar composite material by taking yeast nucleic acid as phosphorus source and carbon source Download PDFInfo
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Abstract
The invention discloses a method for preparing a cobalt phosphide/biochar composite material by taking yeast nucleic acid as a phosphorus source and a carbon source, which comprises the following steps: nucleic acid extracted from baker's yeast cells by a concentrated salt method is taken as a raw material, firstly, the nucleic acid is mixed with a cobalt nitrate solution, the generated complex precipitate is centrifugally washed and dried, mixed salt of sodium chloride and potassium chloride with the mass of 1-10 times is added, the mixture is uniformly ground, and the mixture is calcined under the protective atmosphere of 500-1000 ℃ to obtain the cobalt phosphide/biochar composite material. The material can adsorb bisphenol pollutants in water and activate potassium monopersulfate composite salt to effectively degrade the bisphenol pollutants. The invention not only recycles phosphorus and carbon resources in biomass, but also provides a preparation method of transition metal phosphide, and realizes the efficient removal of bisphenol pollutants in water.
Description
Technical Field
The invention belongs to the field of transition metal phosphide and carbon materials, and particularly relates to a method for preparing a cobalt phosphide/biochar composite material by using yeast nucleic acid as a phosphorus source and a carbon source.
Background
Advanced oxidation technologies (AOPs) based on the generation of strongly oxidizing radicals by activating potassium peroxymonosulfate complex salt (PMS) have the advantages of strong oxidizing ability, high selectivity, wide applicable pH range and the like, and are widely concerned about the treatment of organic matters in environmental wastewater. Transition metal activation, thermal activation, alkali activation, ultraviolet light activation and the like are all activation modes of PMS, transition metal ions are used as a homogeneous catalyst to activate PMS, external condition assistance is not needed, efficiency is high, reaction conditions are mild, and Co is used as a homogeneous catalyst to activate PMS2+PMS is the best match with high catalytic efficiency. However, the homogeneous catalyst has the disadvantages of difficult separation and recovery, potential harm of metal ion residues to the environment and the like in practical application. Therefore, the development of highly efficient heterogeneous catalysts is essential.
The transition metal phosphide is an important compound with P atoms doped in transition metal crystal lattices, has the characteristics of metal, is a good conductor of electricity and heat, and has high hardness, strength, thermal stability and chemical stability. In recent years, the use of transition metal phosphides as catalysts has become a focus of research. Progress has been sought in the synthesis of transition metal phosphides because the conventional synthesis methods mostly require harsh conditions of high temperature, high pressure, hazardous and expensive precursors. The synthesis of transition metal phosphide from elements such as carbon and phosphorus contained in biomass itself is a new method developed in recent years. However, most of the microbial cells have low phosphorus content, and the phosphorus content in the microbial cells from different sources has large difference. Considering that the content of phosphorus in nucleic acid is high and is one of main existing forms of phosphorus in cells, the invention selects cheap and easily available baker's yeast as a raw material for obtaining nucleic acid, extracts the nucleic acid in the baker's yeast by a concentrated salt method with simple and convenient operation and high extraction rate, obtains a complex precipitate by utilizing the chelation of metal ions and the nucleic acid, and converts a cobalt ion-nucleic acid complex into a cobalt phosphide/biochar composite material by molten salt activation and high-temperature pyrolysis. The material has a remarkable adsorption and removal effect on bisphenol pollutants in a water body, and can activate PMS to efficiently degrade the pollutants.
Disclosure of Invention
The cobalt phosphide/biochar composite material prepared by the technology can be used for catalytically activating potassium peroxymonosulfate composite salt to degrade environmental organic pollutants, solves the problems of high toxicity and high cost in the traditional chemical method for preparing transition metal phosphide, and simultaneously realizes the removal of the organic pollutants in water.
The purpose of the invention is realized by the following technical scheme.
A method for preparing a cobalt phosphide/biochar composite material by taking yeast nucleic acid as a phosphorus source and a carbon source comprises the following specific operations:
(1) uniformly dispersing nucleic acid extracted from baker's yeast cells by a concentrated salt method into 20-100 mL deionized water, slowly adding 0.1-0.2 mol/L cobalt nitrate hexahydrate solution while stirring, and continuously stirring for 5-12 h to obtain a complex suspension of the nucleic acid and cobalt ions;
(2) centrifuging the complex suspension obtained in the step (1), washing with deionized water for three times, and drying in a freeze dryer to obtain complex powder;
(3) grinding the complex powder obtained in the step (2) and mixed salt of sodium chloride and potassium chloride with the mass of 1-10 times, wherein the molar ratio of the sodium chloride to the potassium chloride in the mixed salt is 1: 1, and grinding to obtain mixed powder;
(4) transferring the mixed powder obtained in the step (3) into a corundum crucible, placing the corundum crucible into a tubular furnace, and calcining the mixed powder in a protective atmosphere at the calcining temperature of 500-1000 ℃, the calcining time of 3-6 h and the heating rate of 5 ℃/min to obtain a solid mixture powder material;
(5) dispersing the powder material obtained in the step (4) in deionized water, performing ultrasonic treatment for 30 min, filtering, washing for 3 times by using the deionized water, removing sodium chloride and potassium chloride, and drying a filter cake in a 60 ℃ drying oven to obtain a cobalt phosphide/biological carbon composite material;
(6) preparing 0.1 mmol/L bisphenol substance solution, taking the cobalt phosphide/biochar composite material obtained in the step (5) as an adsorbent and a catalyst under the conditions of room temperature and stirring, taking potassium hydrogen peroxymonosulfate composite salt as an oxidant, adding the cobalt phosphide/biochar composite material into the bisphenol substance solution, and sampling at regular time to detect the concentration of the bisphenol substance.
The product showed CoP by X-ray crystallography (XRD).
Optionally, in step (1), the transition metal used is cobalt.
Alternatively, in step (4), the atmosphere for the calcination of the complex is nitrogen or argon.
Optionally, in the step (6), the dosage of the cobalt phosphide/biochar composite material is 0.3-0.6 g/L, the dosage of the potassium monopersulfate composite salt is 0.3-0.6 g/L, the reaction temperature is 25 ℃, and the reaction stirring speed is 600 revolutions per minute.
The invention has the following innovation and beneficial effects:
(1) the invention firstly takes nucleic acid as a phosphorus source and a carbon source, prepares the cobalt phosphide/biological carbon composite material with high adsorbability and catalytic activity by two steps of coprecipitation and high-temperature calcination, is used for adsorbing and catalyzing potassium peroxymonosulfate composite salt to degrade organic pollutants, realizes the reutilization of phosphorus and carbon resources in biomass, simultaneously provides a preparation method of transition metal phosphide, and achieves the aim of efficiently removing bisphenol pollutants in water.
(2) The cobalt phosphide/biochar composite material prepared by the invention has the advantages of good adsorption performance, strong catalytic activity, wide application range and the like.
Description of the drawings:
FIG. 1 is an X-ray crystal diffraction analysis chart of a cobalt phosphide/biochar composite material prepared in example 1 of the present invention.
FIG. 2 is a schematic representation of bisphenol A removal of various materials obtained in example 2 of the present invention.
FIG. 3 is a schematic diagram of bisphenol removal of the material obtained in example 3 of the present invention.
The specific implementation mode is as follows:
for a better understanding of the invention, reference is made to the following detailed description of the invention in conjunction with the accompanying drawings. It should be specifically noted that the examples are provided only for the purpose of further illustrating the present invention, and the scope of the present invention as claimed should not be limited thereto.
Example 1 was carried out:
nucleic acid extracted from baker's yeast cells by a concentrated salt method is uniformly dispersed in 20-100 mL of deionized water, 0.1-0.2 mol/L cobalt nitrate hexahydrate solution is slowly added while stirring, the mixture is continuously stirred for 5-12 h, and the obtained complex is centrifugally washed by water and dried in a freeze dryer. Mixing the dried complex with 1-10 times of sodium chloride and potassium chloride by mass, grinding into powder, transferring to a corundum crucible, placing in a tubular furnace, calcining under a protective atmosphere at 800 ℃, 900 ℃, 1000 ℃ for 3-6 h at a heating rate of 5 ℃/min, cooling to room temperature, and taking out to obtain the material containing sodium chloride and potassium chloride. Dispersing the obtained material in deionized water, performing ultrasonic treatment, filtering, washing, removing sodium chloride and potassium chloride, drying in a 60 ℃ oven, grinding into fine powder to obtain the cobalt phosphide/biological carbon composite material, and respectively naming the cobalt phosphide/biological carbon composite material according to different calcination temperaturesCP-800，CP-900，CP-1000. The X-ray crystal diffraction analysis of the sample is shown in fig. 1.
Example 2 was carried out:
nucleic acid extracted from baker's yeast cells by a concentrated salt method is uniformly dispersed in 20-100 mL of deionized water, 0.1-0.2 mol/L cobalt nitrate hexahydrate solution is slowly added while stirring, the mixture is continuously stirred for 5-12 h, and the obtained complex is centrifugally washed by water and dried in a freeze dryer. Mixing the dried complex with 1-10 times of sodium chloride and potassium chloride, grinding into powder, transferring to a corundum crucible, calcining in a tubular furnace under a protective atmosphere at 800 ℃, 900 ℃, 1000 ℃ for 3-6 h at a heating rate of 5 ℃/min, cooling to room temperature, and taking out to obtain the sodium chloride-containing materialAnd potassium chloride. Dispersing the obtained material in deionized water, performing ultrasonic treatment, filtering, washing, removing sodium chloride and potassium chloride, drying in a 60 ℃ oven, grinding into fine powder to obtain the cobalt phosphide/biological carbon composite material, and respectively naming the cobalt phosphide/biological carbon composite material according to different calcination temperaturesCP-800，CP-900，CP-1000。
In order to examine the adsorption and degradation performance of the cobalt phosphide/biological carbon composite material, the experiment is as follows: preparing 0.1 mmol/L bisphenol A solution, stirring at 25 deg.C and 600 rpm, and mixing 40 mgCP- 800，CP-900OrCP-1000Adding a sample into the bisphenol A solution, sampling at regular time to determine the concentration of the residual bisphenol A in the system, stirring until the concentration of the bisphenol A in the liquid phase is unchanged, adding 40 mg of potassium peroxymonosulfate composite salt, and sampling at regular time to determine the concentration of the residual bisphenol A in the system. According to the measurement result, within 60 min of the system,CP-800，CP-900andCP-1000the adsorption removal rate of the sample to the bisphenol A reaches 48.6 percent, 75.5 percent and 73.8 percent respectively. After potassium hydrogen peroxymonosulfate composite salt is added,CP-800，CP-900andCP-1000the sample degrades the bisphenol A remained in the system within 45 min, 4 min and 15 min respectively. The comparative results of this experiment are shown in FIG. 2.
Example 3 of implementation:
nucleic acid extracted from baker's yeast cells by a concentrated salt method is uniformly dispersed in 20-100 mL of deionized water, 0.1-0.2 mol/L cobalt nitrate hexahydrate solution is slowly added while stirring, the mixture is continuously stirred for 5-12 h, and the obtained complex is centrifugally washed by water and dried in a freeze dryer. Mixing the dried complex with 1-10 times of sodium chloride and potassium chloride by mass, grinding into powder, transferring to a corundum crucible, placing in a tubular furnace, calcining under a protective atmosphere, wherein the calcining temperature is 900 ℃, the calcining time is 3-6 h, the heating rate is 5 ℃/min, cooling to room temperature, and taking out to obtain the material containing sodium chloride and potassium chloride. Dispersing the obtained material in deionized water, performing ultrasonic treatment, filtering, washing, removing sodium chloride and potassium chloride, drying in a 60 ℃ oven, and grinding into fine powder to obtain the cobalt phosphide/biological carbon composite material, which is named as cobalt phosphide/biological carbon composite materialCP-900。
In order to examine the adsorption and degradation performance of the cobalt phosphide/biochar composite material on bisphenol pollutants, 0.1 mmol/L of bisphenol F, bisphenol S and bisphenol AF solutions are respectively prepared and stirred at the temperature of 25 ℃ and the rotating speed of 600 r/min. Mixing 40 mgCP-900Adding a sample into the bisphenol F solution, sampling at regular time to determine the concentration of the residual bisphenol F in the system, stirring until the concentration of the bisphenol F in the liquid phase is unchanged, adding 40 mg of potassium peroxymonosulfate composite salt, and sampling at regular time to determine the concentration of the residual bisphenol F in the system. According to the measured result, the system isCP-900The adsorption removal rate of the sample to the bisphenol F within 60 min reaches 82.8%, and the bisphenol F can be completely degraded within 4 min after the potassium hydrogen peroxymonosulfate composite salt is added. Replacing bisphenol F with bisphenol S or bisphenol AF solution according to the same procedure as aboveCP-900The adsorption removal rates of the sample to bisphenol S and bisphenol AF within 60 min are respectively 84.2 percent and 62.5 percent, after potassium peroxymonosulfate composite salt is added, the degradation removal rates of the bisphenol S and the bisphenol AF within 10 min respectively reach 13.8 percent and 34.8 percent, and the total removal rates of the bisphenol S and the bisphenol AF in the whole process operation respectively reach 98.0 percent and 97.3 percent. The comparative results of this experiment are shown in FIG. 3.
Claims (5)
1. A method for preparing a cobalt phosphide/biochar composite material by taking yeast nucleic acid as a phosphorus source and a carbon source is characterized by comprising the following steps:
(1) uniformly dispersing nucleic acid extracted from baker's yeast cells by a concentrated salt method into 20-100 mL deionized water, slowly adding 0.1-0.2 mol/L cobalt nitrate hexahydrate solution while stirring, and continuously stirring for 5-12 h to obtain a complex suspension of the nucleic acid and cobalt ions;
(2) centrifuging the complex suspension obtained in the step (1), washing with deionized water for three times, and drying in a freeze dryer to obtain complex powder;
(3) grinding the complex powder obtained in the step (2) and mixed salt of sodium chloride and potassium chloride with the mass of 1-10 times, wherein the molar ratio of the sodium chloride to the potassium chloride in the mixed salt is 1: 1, and grinding to obtain mixed powder;
(4) transferring the mixed powder obtained in the step (3) into a corundum crucible, placing the corundum crucible into a tubular furnace, and calcining the mixed powder in a protective atmosphere at the calcining temperature of 500-1000 ℃, the calcining time of 3-6 h and the heating rate of 5 ℃/min to obtain a solid mixture powder material;
(5) dispersing the powder material obtained in the step (4) in deionized water, performing ultrasonic treatment for 30 min, filtering, washing for 3 times by using the deionized water, removing sodium chloride and potassium chloride, and drying a filter cake in a 60 ℃ drying oven to obtain a cobalt phosphide/biological carbon composite material;
(6) preparing 0.1 mmol/L bisphenol substance solution, taking the cobalt phosphide/biochar composite material obtained in the step (5) as an adsorbent and a catalyst under the conditions of room temperature and stirring, taking potassium hydrogen peroxymonosulfate composite salt as an oxidant, adding the cobalt phosphide/biochar composite material into the bisphenol substance solution, and sampling at regular time to detect the concentration of the bisphenol substance.
2. The method for preparing cobalt phosphide/biochar composite material by using yeast nucleic acid as phosphorus source and carbon source according to claim 1, wherein the transition metal in step (1) is cobalt, but not limited to cobalt, and other transition metals such as iron, nickel and the like are also suitable for the method.
3. The method for preparing cobalt phosphide/biochar composite material by using yeast nucleic acid as phosphorus source and carbon source according to claim 1, wherein the protective atmosphere used for calcination in step (4) is nitrogen or argon.
4. The method for preparing cobalt phosphide/biochar composite material by using yeast nucleic acid as phosphorus source and carbon source according to claim 1, wherein the organic pollutant used in step (6) is bisphenol, but is not limited to bisphenol, and any environmental organic pollutant existing in water body and capable of being adsorbed and catalytically degraded by the material, such as sulfamethoxazole, is included.
5. The method for preparing cobalt phosphide/biochar composite material by using yeast nucleic acid as phosphorus source and carbon source according to claim 1, wherein the dosage of cobalt phosphide/biochar material in the step (6) is 0.3-0.6 g/L, the dosage of potassium hydrogen peroxymonosulfate composite salt is 0.3-0.6 g/L, the reaction temperature is 25 ℃, and the reaction stirring speed is 600 r/min.
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| CN114011411A (en) * | 2021-11-08 | 2022-02-08 | 安徽科技学院 | CoO-Co3O4Preparation method and application of carbon composite |
| CN114335487A (en) * | 2022-01-10 | 2022-04-12 | 齐鲁工业大学 | Preparation method and application of cobalt phosphide/carbon composite electrode material |
| CN114956019A (en) * | 2022-01-14 | 2022-08-30 | 哈尔滨工业大学（深圳） | Method for one-step synthesis of cobalt phosphide by molten salt mediation and application thereof |
| CN115518614A (en) * | 2022-07-12 | 2022-12-27 | 山东大学 | Iron-copper bimetal modified biochar material and preparation method and application thereof |
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| CN114011411A (en) * | 2021-11-08 | 2022-02-08 | 安徽科技学院 | CoO-Co3O4Preparation method and application of carbon composite |
| CN114011411B (en) * | 2021-11-08 | 2023-05-26 | 安徽科技学院 | CoO-Co 3 O 4 Preparation method and application of carbon composite |
| CN114335487A (en) * | 2022-01-10 | 2022-04-12 | 齐鲁工业大学 | Preparation method and application of cobalt phosphide/carbon composite electrode material |
| CN114956019A (en) * | 2022-01-14 | 2022-08-30 | 哈尔滨工业大学（深圳） | Method for one-step synthesis of cobalt phosphide by molten salt mediation and application thereof |
| CN115518614A (en) * | 2022-07-12 | 2022-12-27 | 山东大学 | Iron-copper bimetal modified biochar material and preparation method and application thereof |
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