CN114669281B - PEI modified yeast residue-based platinum-palladium-rhodium adsorption material, preparation method and industrial wastewater treatment method - Google Patents

PEI modified yeast residue-based platinum-palladium-rhodium adsorption material, preparation method and industrial wastewater treatment method Download PDF

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CN114669281B
CN114669281B CN202210340486.8A CN202210340486A CN114669281B CN 114669281 B CN114669281 B CN 114669281B CN 202210340486 A CN202210340486 A CN 202210340486A CN 114669281 B CN114669281 B CN 114669281B
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CN114669281A (en
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谢建平
王国祯
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Central South University
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Abstract

The PEI modified yeast residue based platinum-palladium-rhodium adsorption material comprises yeast residue, PEI and glutaraldehyde, PEI is crosslinked on the yeast residue, and the crosslinked yeast residue and PEI are crosslinked and fixed through the glutaraldehyde to form the PEI modified yeast residue platinum-palladium-rhodium adsorption material. The invention takes yeast fermentation waste residues as raw materials, and prepares the PEI-modified platinum-palladium-rhodium biological adsorbent with high adsorption capacity on platinum ions, palladium ions and rhodium ions by crosslinking PEI on the surface of biomass, and the PEI-modified platinum-palladium-rhodium biological adsorbent is used for recovering the platinum ions, the palladium ions and the rhodium ions from an aqueous solution. Meanwhile, the platinum-palladium-rhodium adsorption material of the PEI modified yeast residues can be kept stand to separate the adsorption material from an adsorption system, so that the cost of the traditional immobilization mode and the potential loss of adsorption active sites after immobilization are reduced.

Description

PEI modified yeast residue-based platinum-palladium-rhodium adsorption material, preparation method and industrial wastewater treatment method
Technical Field
The invention relates to the field of industrial wastewater treatment or platinum group metal recovery, in particular to a PEI (polyethyleneimine) modified yeast residue-based platinum, palladium and rhodium adsorption material, a preparation method and an industrial wastewater treatment method.
Background
Platinum group metals palladium, platinum and rhodium are widely used in the fields of chemical catalysis, electronic and electrical equipment, automobile industry, jewelry, medical equipment and the like because of their excellent physicochemical properties such as oxidation resistance, corrosion resistance, high melting point, excellent electrical conductivity, catalytic performance and the like. However, platinum group metals are extremely rare in the earth's crust, and palladium content is more scarce, on the order of 1-10 parts per trillion. The quantity of high-grade ores is gradually reduced along with mining, and the grade of residual natural ores is continuously reduced, so that the mining cost is increased. Compared with natural ore (10 g/t), the method has the advantages that the method is more efficient and economical in extracting the platinum group metals from secondary resources such as waste catalysts (2 kg/t) and waste electronic equipment (130 g/t). Therefore, in order to protect the environment, save mineral resources, and meet future market demands, it is necessary to recover platinum group metals.
Ion exchange, membrane separation, solvent extraction and other methods are commonly used to recover metals from aqueous solutions, and these methods are generally expensive, have limited removal efficiency, and have poor recovery effect at low concentration, which is likely to cause secondary pollution. Compared with other methods, the biological adsorption adopts biomass as a biological adsorbent to adsorb metal ions in solution, and has the advantages of simple operation, low cost and no harm to the environment. Therefore, the method has a great development prospect in the field of metal ion recovery and removal. Although biomass that can be used as an adsorbent is widely available, the adsorption capacity of the original biomass is generally low and solid-liquid separation is inconvenient, limiting commercial application.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an adsorbing material based on PEI modified yeast residues, a preparation method and a treatment method of industrial wastewater, wherein the adsorbing material has high adsorption rate on platinum ions, palladium ions and rhodium ions.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: the PEI is crosslinked on the yeast residues, and the crosslinked yeast residues and the PEI are crosslinked and fixed through glutaraldehyde to form the PEI modified platinum-palladium-rhodium adsorbing material of the yeast residues.
Preferably, when the PEI modified yeast residues and the PEI are crosslinked, the yeast residues are subjected to shaking culture in a PEI aqueous solution with the mass concentration of 0.5% -8% for more than 12 hours.
Preferably, the PEI modified yeast residue based platinum palladium rhodium adsorption material is subjected to constant temperature oscillation at the temperature of 25-35 ℃ when being cultured in a PEI aqueous solution.
Preferably, the steps of cross-linking and fixing the PEI and the yeast residues which are cross-linked together through glutaraldehyde are as follows: adding glutaraldehyde with the mass concentration of 0.1-2% into the yeast residue and PEI solution which are crosslinked together for crosslinking and fixing.
Preferably, the platinum-palladium-rhodium adsorbing material based on the PEI modified yeast residues is shaken up for more than 1 hour when the glutaraldehyde is subjected to cross-linking and fixing.
A preparation method of a PEI modified yeast residue-based platinum-palladium-rhodium adsorption material comprises the following steps;
1) Cleaning the yeast residue with clear water for more than 3 times, drying, and storing in a sealed container;
2) Adding 1 weight part of yeast dregs into 80-120 weight parts of PEI aqueous solution, and carrying out constant temperature shaking culture at the temperature of 25-35 ℃ for more than 12 hours; the mass concentration of the PEI aqueous solution is 0.5-8%;
3) Adding 3-10 parts by weight of glutaraldehyde aqueous solution into the solution obtained in the step 2), and shaking up for more than 1 hour; the mass concentration of the glutaraldehyde water solution is 0.1-2%.
4) Centrifuging to obtain a cross-linked product, washing with deionized water, and freeze-drying; thus obtaining PEI modified yeast dregs.
According to the preparation method of the PEI modified yeast residue-based platinum-palladium-rhodium adsorption material, the mass concentration of the PEI aqueous solution is preferably 5%.
According to the preparation method of the PEI modified yeast residue-based platinum-palladium-rhodium adsorption material, the mass concentration of the glutaraldehyde aqueous solution is preferably 1.25%.
A method for treating industrial wastewater by using a PEI modified yeast residue-based platinum-palladium-rhodium adsorption material comprises the following steps;
1) Adjusting the pH value of the industrial wastewater to 1.0 to 3.0; the industrial wastewater contains one or more of platinum ions, palladium ions and rhodium ions; so that the concentration sum of platinum ions, palladium ions and/or rhodium ions in the industrial wastewater is less than 800 mg/L;
2) Adding the PEI modified yeast residue-based platinum-palladium-rhodium adsorption material into the industrial wastewater obtained in the step 1); adsorbing at 25-35 deg.C for more than 4 hr;
3) And standing for more than 3 hours to separate the platinum-palladium-rhodium adsorption material of the PEI modified yeast dregs from the industrial wastewater.
Preferably, the method for treating the industrial wastewater by using the PEI modified yeast residue based platinum-palladium-rhodium adsorption material uses 0.3 mol/L-1 mol/L dilute hydrochloric acid solution of 0.3 mol/L-1 mol/L thiourea to elute the PEI modified yeast residue treated in the step 3) so as to recover the PEI modified yeast residue platinum-palladium-rhodium adsorption material.
Compared with the prior art, the invention has the advantages that: the invention takes yeast fermentation waste residues as raw materials, and prepares the PEI-modified platinum-palladium-rhodium biological adsorbent with high adsorption capacity on platinum ions, palladium ions and rhodium ions by crosslinking PEI on the surface of biomass, and the PEI-modified platinum-palladium-rhodium biological adsorbent is used for recovering the platinum ions, the palladium ions and the rhodium ions from an aqueous solution. Meanwhile, the platinum, palladium and rhodium adsorbing material of the PEI modified yeast residues can be kept still to separate the adsorbing material from an adsorbing system, so that the cost of the traditional immobilization mode and the potential loss of adsorption active sites after immobilization are reduced.
Drawings
FIG. 1 is an SEM image of the original Pichia pastoris bacterial residue.
FIG. 2 is an SEM image of the PEI-modified Pichia pastoris based bacterial slag adsorption material of example 1.
FIG. 3 is a diagram showing the results of elemental analysis of the original Pichia pastoris bacterial slag adsorption material.
FIG. 4 is a graph of elemental analysis results of a PEI-modified Pichia pastoris bacterial slag adsorption material.
FIG. 5 is an SEM image of Pd adsorbed by the PEI-modified Pichia pastoris bacterial slag adsorbing material in example 1.
FIG. 6 is a graph showing the results of elemental analysis of the PEI-modified Pichia pastoris bacterial slag adsorption material after adsorption of Pd in example 1.
FIG. 7 is a graph showing the relationship between the number of reuses and the adsorption amount of the PEI-modified Pichia pastoris bacterial slag adsorption material in example 1.
Detailed Description
In order to facilitate an understanding of the invention, the invention will now be described more fully and in detail with reference to the preferred embodiments, but the scope of the invention is not limited to the specific embodiments described below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Example 1
A PEI modified yeast residue-based platinum-palladium-rhodium adsorption material is prepared by the following steps;
1) Cleaning the Pichia pastoris residues with clear water for 5 times to remove residual chemical reagents and metabolites. Then, the mixture was dried at 55 ℃ and stored in a sealed container. The Pichia pastoris slag is a fermentation waste slag, the yeast is a fungus, the outer layer of the cell wall is mannan, the inner layer is glucan, the middle layer is a layer of protein molecules, and a small amount of lipoid and chitin are contained. Compared with the structure of common bacteria, the structure of the yeast is higher, complex and richer in surface groups, so that more crosslinking sites are provided for crosslinking with PEI.
2) Adding 1 weight part of pichia pastoris bacterial residues into 100 weight parts of PEI aqueous solution, and carrying out shake culture in a constant temperature incubator at 30 ℃ and 150 rpm for 24 hours; the mass concentration of the PEI aqueous solution is 5 percent, and the molecular weight of the PEI is 10000.
3) Adding 5 parts by weight of glutaraldehyde aqueous solution into the solution obtained in the step 2), and shaking up for 2 hours; the mass concentration of the glutaraldehyde aqueous solution was 1.25%.
4) Centrifuging to obtain a cross-linked product, washing with deionized water, and freeze-drying; and grinding the mixture through a 200-mesh screen to obtain the PEI modified yeast dregs.
In this embodiment, if the amounts of the PEI aqueous solution and the glutaraldehyde aqueous solution are too large, agglomeration may occur, resulting in a decrease in the adsorption amount of the finally prepared adsorption material.
FIG. 1 shows an SEM image of the original Pichia pastoris bacterial residues, from which it can be seen that there are many fragments of different sizes stacked. FIG. 2 is an SEM image of the PEI-modified Pichia pastoris bacterial slag-based adsorbing material of the present example, from which it can be seen that the surface becomes rough after modification. FIGS. 3 and 4 are diagrams illustrating elemental analysis results of the original Pichia pastoris bacterial slag and PEI-based modified Pichia pastoris bacterial slag adsorption material, respectively; as can be seen from FIGS. 3 and 4, the weight ratio of C and N of the Pichia pastoris slag, modified by PEI, increased from 49.58% and 13.03% to 55.33% and 31.05%, respectively.
The PEI-modified Pichia pastoris bacterial slag adsorption material prepared in the embodiment is prepared by crosslinking PEI on Pichia pastoris bacterial slag and then performing crosslinking and solidification through glutaraldehyde. The content of imino on the surface of the PEI modified Pichia pastoris bacterial residues is increased, so that the electrostatic adsorption effect of the PEI modified Pichia pastoris bacterial residue adsorption material on negatively charged platinum complexes, palladium complexes and rhodium complexes in a solution is enhanced, and the adsorption capacity of platinum ions, palladium ions and rhodium ions is greatly improved.
The PEI-modified-based Pichia pastoris bacterial slag adsorption material prepared in the embodiment is used for adsorbing Pd-containing industrial wastewater, and the specific steps are as follows;
1) Adjusting the pH value of the industrial wastewater to 1.0 to 3.0; the industrial wastewater contains palladium ions; so that the concentration of platinum ions and palladium ions in the industrial wastewater is 500 mg/L.
2) Adding the PEI modified Pichia pastoris bacterial slag adsorption material prepared in the embodiment into the industrial wastewater in the step 1); adsorption was carried out at 30 ℃ for 6 hours. In this example, the PEI-modified Pichia pastoris bacterial slag based adsorption material was added in an amount of 1.0 g/L.
3) And standing for 6 hours to separate the platinum, palladium and rhodium adsorbing material of the PEI modified yeast dregs from the industrial wastewater. The adsorbing material of the embodiment can be removed from the solution through natural sedimentation, and the effect of standing for 240 min is even better than that of 12000 Xg centrifugation, so that the microbial adsorbent can be separated from the adsorbing system through standing, and the cost of the traditional immobilization mode and the potential loss of adsorption active sites after immobilization are reduced.
The content of palladium ions in the industrial wastewater is detected, and the result shows that the adsorption of the PEI-modified Pichia pastoris bacterial slag adsorption material on the palladium ions reaches 587.67 mg/g. Fig. 5 is an SEM image of the PEI modified pichia pastoris bacterial residue-based adsorbing material of the present example after adsorbing Pd, and it can be seen from the figure that the distribution of palladium is very uniform. Fig. 6 is a graph of the element analysis result of the PEI modified based pichia pastoris bacterial residue adsorbing material adsorbing Pd according to the embodiment.
In this embodiment, after the content of imino groups on the surface of the PEI modified pichia pastoris bacterial residue adsorbing material is increased, the isoelectric point is changed from 4.64 to 9.46, the imino groups are protonated when the pH is lower than the isoelectric point, and the surface of the PEI modified pichia pastoris bacterial residue adsorbing material is positively charged when the pH is lower than the isoelectric point.
In this embodiment, pH is a key factor affecting the adsorption, and when the adsorption is performed, the pH of the industrial wastewater needs to be adjusted to 1.0 to 3.0. In the pH range of 1-3, the adsorbing capacity of the PEI-modified Pichia pastoris slag-based adsorbing material for Pd (II) increases with the increase of the pH value of the solution. After PEI modification, a large amount of amino groups are introduced to the surface of the biomass, namely pichia pastoris, so that the surface of the biomass has a large amount of positive charges. In addition, the presence of palladium also affects adsorption, which is affected by the pH of the solution and the chloride ion concentration. The stable palladium ion is an anionic chloride complex (PdCl) at a pH of 3 4 2- ) Therefore, the protonated amine groups on the surface of the biomass modified by the palladium anion complex and the PEI have stronger electrostatic attraction and coordination. In the pH range of 1-3, the adsorption capacity of the biosorbent is increased rather than decreased due to the ratio PdCl of certain anions to positively charged biosorbent 4 2- Has stronger competition. The pH range of 3 is selected in this example in view of the precipitation of hydroxides of metal ions occurring in high pH solutions.
In this example, the PEI-modified Pichia pastoris slag adsorption material can be recycled, eluting with 60 mL of 0.5 mol/L dilute hydrochloric acid solution containing 0.5 mol/L thiourea prior to recycling. The regenerated adsorbing material can be used for adsorbing industrial wastewater containing platinum ions, palladium ions and rhodium ions again. Fig. 7 is a graph showing the relationship between the number of times of repeated use and the adsorption amount of the PEI modified pichia pastoris bacterial residue adsorbing material in the present embodiment. In the embodiment, after the regenerated PEI-modified Pichia pastoris bacterial slag adsorption material is repeatedly used for 5 times, the adsorption capacity of palladium ions is reduced from 488.75 mg/g to 451.75 mg/g; this is probably because part of Pd (II) after adsorption is reduced to Pd (0) and cannot be eluted by thiourea, resulting in reduction of adsorption sites.
The PEI modified Pichia pastoris slag-based platinum-palladium-rhodium adsorption material prepared in the embodiment is used for respectively adsorbing industrial wastewater containing platinum ions and rhodium ions, and the initial solubility of the platinum ions and the initial solubility of the rhodium ions are both 500 mg/L; the amount of PEI-modified Pichia pastoris bacterial residue-based adsorption material added was 1.0 g/L. The other steps are the same as the steps for adsorbing the industrial wastewater containing Pd. Finally, the PEI modified Pichia pastoris slag adsorption material achieves 277.24 mg/g of platinum ions and 235.64 mg/g of rhodium ions.
From the above, the PEI modified pichia pastoris bacterial residue-based adsorption material of the embodiment has the following advantages.
1. According to the research, yeast fermentation waste residues are used as raw materials, and PEI is crosslinked on the surface of biomass to prepare the PEI modified biological adsorbent with high Pd (II) adsorption capacity. The addition amount of PEI and glutaraldehyde significantly influences the adsorption capacity of the modified Pichia pastoris bacterial residues, namely the proportion of imino groups generated through a crosslinking reaction influences the adsorption performance of PEI modified biomass.
2. The highest PEI-PR adsorption was obtained using 5% PEI (M = 10000) and 1.25% glutaraldehyde, which was a 301% increase over 146.39 mg/g adsorption before modification. The adsorption performance of 90.35 percent can be still maintained after 5 times of recycling.
3. Compared with the PEI-PR before modification, the PEI-PR can be removed from the solution through natural sedimentation, the effect of standing for 240 min is even better than that of 12000 Xg centrifugation, and therefore, the microbial adsorbent can be separated from the adsorption system through standing, and the cost of the traditional immobilization mode and the potential loss of adsorption active sites after immobilization are reduced.
4. Interaction between various amino groups and amide groups and Pd (II) plays an important role in the adsorption process, the modification greatly increases the content of imino groups, and the electrostatic adsorption effect of PEI-PR on negatively charged palladium complexes in the solution is enhanced, so that the adsorption amount of Pd (II) is greatly improved.

Claims (6)

1. A PEI modified yeast slag-based platinum palladium rhodium adsorption material is characterized in that: the PEI modified yeast residue platinum palladium rhodium adsorption material comprises yeast residue, PEI and glutaraldehyde, wherein the PEI is crosslinked on the yeast residue, and the crosslinked yeast residue and the PEI are crosslinked and fixed through the glutaraldehyde to form the PEI modified yeast residue platinum palladium rhodium adsorption material; when the yeast dregs and the PEI are crosslinked, the yeast dregs are subjected to shaking culture for more than 12 hours in PEI aqueous solution with the mass concentration of 0.5% -8%; the yeast dregs are oscillated at constant temperature between 25 ℃ and 35 ℃ when being cultured in PEI aqueous solution; the steps of crosslinking and fixing the yeast dregs and the PEI together through glutaraldehyde are as follows: adding glutaraldehyde with the mass concentration of 0.1-2% into the yeast residue and PEI solution which are crosslinked together for crosslinking and fixing.
2. The PEI modified yeast dreg based platinum palladium rhodium adsorption material as claimed in claim 1, wherein: the glutaraldehyde is shaken up for more than 1 hour when the cross-linking fixation is carried out.
3. A preparation method of a platinum-palladium-rhodium adsorption material based on PEI modified yeast residues is characterized by comprising the following steps: comprises the following steps;
1) Cleaning yeast residue with clear water for more than 3 times, drying, and storing in a sealed container;
2) Adding 1 weight part of yeast dregs into 80-120 weight parts of PEI aqueous solution, and carrying out constant temperature shaking culture at the temperature of 25-35 ℃ for more than 12 hours; the mass concentration of the PEI aqueous solution is 0.5-8%;
3) Adding 3-10 parts by weight of glutaraldehyde aqueous solution into the solution obtained in the step 2), and shaking up for more than 1 hour; the mass concentration of the glutaraldehyde water solution is 0.1-2%;
4) Centrifuging to obtain a cross-linked product, washing with deionized water, and freeze-drying; thus obtaining PEI modified yeast dregs.
4. The method for preparing the PEI modified yeast dreg based platinum-palladium-rhodium adsorbing material according to claim 3, which is characterized by comprising the following steps: the mass concentration of the PEI aqueous solution is 5%.
5. The method for preparing the PEI modified yeast residue based platinum palladium rhodium adsorption material according to claim 3, which is characterized by comprising the following steps: the mass concentration of the glutaraldehyde aqueous solution was 1.25%.
6. A method for treating industrial wastewater by using a PEI modified yeast residue-based platinum-palladium-rhodium adsorption material is characterized by comprising the following steps: comprises the following steps;
1) Adjusting the pH value of the industrial wastewater to 1.0 to 3.0; the industrial wastewater contains one or more of platinum ions, palladium ions and rhodium ions; so that the concentration sum of platinum ions, palladium ions and/or rhodium ions in the industrial wastewater is less than 800 mg/L;
2) Adding the PEI modified yeast slag based platinum palladium rhodium adsorption material of any one of claims 1-3 to the industrial wastewater in step 1); adsorbing at 25-35 deg.C for more than 4 hr;
3) And standing for more than 3 hours to separate the platinum-palladium-rhodium adsorption material of the PEI modified yeast dregs from the industrial wastewater.
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