CN114317998A - Method for treating impurity metal in waste palladium-carbon catalyst by micro-electric field coupling microorganism - Google Patents
Method for treating impurity metal in waste palladium-carbon catalyst by micro-electric field coupling microorganism Download PDFInfo
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Abstract
The invention discloses a method for treating impurity metals in a waste palladium-carbon catalyst by micro-electric field coupling microorganisms. Which comprises the following steps: (1) adding waste palladium-charcoal catalyst powder into acclimated acidophilic thiobacillus (B), (C)A.f+A.tMixed bacteria) culture solution, and proportionally mixing and culturing; (2) applying an external micro electric field in the culture system in the step (1) and continuously culturing; (3) and (3) filtering the mixture obtained in the step (2) to respectively obtain filtrate and filter residue. By adopting the method, the impurity metal in the waste palladium-carbon catalyst can be removed efficiently and mildly, so that the impurity interference in the subsequent palladium enrichment process is avoided; the invention adopts the coupling of direct current micro-electric field and microorganismThe method has the advantages that impurity metals of the palladium-carbon catalyst are removed, and high energy consumption, strong corrosivity and potential tail gas pollution risk caused by the traditional high-temperature roasting and strong acid treatment processes are replaced; the process provided by the invention can recycle the production water, and achieves the purpose of zero discharge of waste liquid.
Description
Technical Field
The invention belongs to the cross technical field of electrochemistry and biological metallurgy, and particularly relates to a method for treating impurity metals in a waste palladium-carbon catalyst by micro-electric field coupling microorganisms.
Background
Platinum group metals are strategic mineral resources and are widely applied to industries such as automobile exhaust catalysts, chemical catalysts, jewelry, electrical and electronic industries and the like. As the world countries with the largest platinum group metal consumption, the production and development of the industry in China cannot be met simply by the development of mineral resources, and the recycling of secondary mineral products containing platinum group metals must be increased.
Usually, the waste palladium-carbon catalyst contains 1-2% of palladium, and is an important raw material for extracting palladium powder. As for the recovery work of the waste palladium-carbon catalyst, Zhang Bao Ming mentions that most organic matters and carrier carbon in the waste palladium-carbon catalyst are removed by adopting a washing pretreatment and high-temperature roasting method (recovery of metal palladium in the palladium-containing waste activated carbon catalyst, Chinese resource comprehensive utilization, 2019, 37 (2): 27-29). Zhao Bei mentioned that the waste palladium carbon catalyst is washed by dilute hydrochloric acid to remove impurity metals (a recycling method of the waste palladium carbon catalyst, resource saving and environmental protection, No. 10, page 192-. In addition, studies have also shown that common methods for separating and recovering palladium from the waste palladium-carbon catalyst are incineration and leaching methods, including oxidative roasting, hydrochloric acid leaching, ammonia complexation separation, aqua regia dissolution, caustic soda leaching, and adsorption. The above methods are remarkably effective in recovering palladium from a supported palladium-containing catalyst, but each of them has drawbacks. For example, increased energy consumption during high temperature processing; the organic matter is decomposed in the high-temperature process, and potential dioxin risk is generated; the strong acid and strong alkali treatment process is easy to corrode equipment, and can generate secondary pollution and the like. Therefore, the development of an environment-friendly, green and environment-friendly technical process for separating and extracting palladium from the waste palladium-carbon catalyst is urgent and necessary.
Disclosure of Invention
The invention discloses a mild and efficient method for recovering impurity metals from waste palladium-carbon catalysts and improving the palladium concentration in the waste palladium-carbon catalysts, and aims to overcome the defects of high-temperature roasting and acid treatment in the prior art for treating the waste palladium-carbon catalysts. The invention adopts acidophilic thiobacillus mixed bacteria (namely acidophilic thiobacillus ferrooxidans (thiobacillus ferrooxidans)) domesticated based on waste palladium-carbon catalyst powderAcidithiobacillus ferrooxidans) Hereinafter, it is abbreviated asA. f，And Acidithiobacillus thiooxidans (A), (B), (C)Acidithiobacillus thiooxidans) Hereinafter, it is abbreviated asA. t) The method has the coupling effect with a direct current micro-electric field, and achieves the purposes of efficiently removing impurity metals (Cu, Ni, Pb, Cd and Al) in the waste palladium-carbon catalyst and further avoiding impurity interference in the subsequent palladium enrichment process. The whole recovery process is environment-friendly and pollution-free, the filtered filtrate can be recycled, the recovery rate is high, and resources are fully utilized.
The technical scheme of the invention is specifically introduced as follows.
A method for treating impurity metals in a waste palladium-carbon catalyst by micro-electric field coupling microorganisms comprises the following steps:
(1) subjecting to acclimatizationA. f + A. tThe mixed bacteria culture solution and the waste palladium-carbon catalyst powder are mixed and cultured according to a certain proportion, and the oxidation-reduction potential of the mixed bacteria culture solution is between 500 and 650 mV;
(2) applying an external micro-electric field in the culture system in the step (1), and continuously culturing for a period of time;
(3) and (3) filtering the mixture obtained in the step (2) to respectively obtain filtrate and filter residue, wherein the obtained filter residue contains active carbon and palladium and does not contain impurity metals, and the impurity metals comprise Cu, Ni, Pb, Cd and Al.
Preferably, in the step (1), before the mixed culture, the waste palladium catalyst powder is sieved by a nylon sieve, so that the particle size of the waste palladium catalyst powder is 0.5-1.5 mm.
Preferably, in step (1), theA. The domestication method of the f + A.t mixed bacteria comprises the following steps: by using a voltage of 1.5V, and the current is 0-100mA, and the addition amount of the waste palladium-carbon catalyst powder is 2g, 4g, 6g, 8g, 10g for A, f+ A. tContinuous domestication treatment is carried out to obtain bacteria liquid with the oxidation-reduction potential of 500-650 mV.
Preferably, in the step (2), the negative electrode material used by the micro electric field is one of a graphite carbon rod, graphite carbon cloth and a platinum electrode, the positive electrode material is a platinum electrode, the parameter of the micro electric field is voltage 1.5V, and direct current is 20-80 mA; the culture time is 4-6 days.
Preferably, the filtrate obtained in the step (3) is returned to the leaching system in the step (1) for recycling, and no waste liquid is discharged in the process.
Preferably, the filter residue obtained in the step (3) is further refined and purified by a wet process to obtain the metal palladium.
Compared with the prior art, the method has the following advantages:
1. the micro-electric field coupling microbial technology provided by the invention can realize the high-efficiency removal of impurity metals in the waste palladium-carbon catalyst, thereby avoiding the interference of impurities on the subsequent chemical separation of palladium;
2. the micro electric field releases heat in the reaction process, an additional heat source is not required to be provided, and the energy consumption is greatly reduced;
3. the filtrate generated after the micro-electric field and microorganism coupling treatment does not need further treatment, and the impurity metal is deposited on the negative electrode and can directly return to the front end leaching system to continue to participate in the reaction;
4. the method of the invention is adopted to pretreat the impurities of the waste palladium-carbon catalyst, and can replace the high energy consumption, high corrosivity and organic pollution hazards brought by high-temperature roasting and strong acid treatment.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in detail with reference to the following examples, which are not intended to limit the scope of the present invention, and all similar methods and similar variations using the present invention shall fall within the scope of the present invention.
The waste palladium-carbon catalyst is a noble metal-containing palladium catalyst taking activated carbon as a carrier, and the impurity metal mainly comprises Cu, Ni, Pb, Cd and Al.
A. f + A. tThe composition of the culture medium was as follows: (NH)4)2SO4 3g/L，MgSO4·7H2O 0.50g/L，KCl 0.10g/L，Ca(NO3)2 0.01g/L，K2HPO4 0.50g/L，FeSO4·7H2O44 g/L, initial pH2.0 of the culture solution.
Example 1
Continuously crushing the waste palladium-carbon catalyst for many times by using a handheld crusher, and sieving by using a national standard sieve (made of nylon material) to obtain waste palladium-carbon catalyst powder with the particle size of 1 mm. The direct current with the voltage of 1.5V and the current of 0-100mA is utilized, and the adding amount of the waste palladium-carbon catalyst powder is (2, 4, 6, 8, 10) g/50mLA. f + A. tAnd (4) carrying out continuous domestication treatment to obtain a bacterial liquid with the oxidation-reduction potential higher than 550 mV.
According to the waste palladium-carbon catalyst powder andA. f + A. tthe leaching experiment is carried out by adding 5g/50mL of the solution, and at the moment, the micro-electric field is applied: taking graphite carbon rod as negative electrode, platinum electrode as positive electrode, voltage of 1.5V, direct current of 40mA, continuously culturing for 5 days, monitoring pH, ORP and Fe of culture solution2+And (4) concentration. During the culture process, impurity metals (Cu, Ni, Pb, Cd, Al) are deposited on the negative electrode.
Treating the cultured mixed solution by using a sand core filtering device, respectively collecting filtrate and filter residue, analyzing by using an inductively coupled plasma atomic emission spectrometer, wherein impurity metals in the filtrate are not detected, only metal palladium is detected in the filter residue, and an X-ray diffractometer scans the phase of the filter residue, so that only an obvious and disordered carbon peak is displayed as a result.
Example 2
Continuously crushing the waste palladium-carbon catalyst for many times by using a handheld crusher, and sieving by using a national standard sieve (made of nylon material) to obtain waste palladium-carbon catalyst powder with the particle size of 0.5 mm. The direct current with the voltage of 1.5V and the current of 0-100mA is utilized, and the adding amount of the waste palladium-carbon catalyst powder is (2, 4, 6, 8, 10) g/50mLA. f + A. tAnd (4) carrying out continuous domestication treatment to obtain a bacterial liquid with the oxidation-reduction potential higher than 500 mV.
According to the waste palladium-carbon catalyst powder andA. f + A. tthe leaching experiment is carried out by adding 10g/50mL of the solution, and at the moment, the micro-electric field is applied: graphite carbon cloth as negative electrode, platinum electrode as positive electrode, voltage of 1.5V, direct current of 60mA, continuous culture for 4 days, and monitoring pH, ORP and Fe of culture solution2+And (4) concentration.
Treating the cultured mixed solution by using a sand core filtering device, respectively collecting filtrate and filter residue, analyzing by using an inductively coupled plasma atomic emission spectrometer, wherein impurity metals in the filtrate are not detected, only metal palladium is detected in the filter residue, and an X-ray diffractometer scans the phase of the filter residue, so that only an obvious and disordered carbon peak is displayed as a result.
Example 3
Continuously crushing the waste palladium-carbon catalyst for many times by using a handheld crusher, and sieving by using a national standard sieve (made of nylon material) to obtain waste palladium-carbon catalyst powder with the particle size of 1.5 mm. The direct current with the voltage of 1.5V and the current of 0-100mA is utilized, and the adding amount of the waste palladium-carbon catalyst powder is (2, 4, 6, 8, 10) g/50mLA. f + A. tAnd (4) carrying out continuous domestication treatment to obtain a bacterial liquid with the oxidation-reduction potential higher than 600 mV.
According to the waste palladium-carbon catalyst powder andA. f + A. tthe leaching experiment is carried out by adding 2g/50mL of the solution, and at the moment, the condition of applying a micro electric field is as follows: graphite carbon cloth as negative electrode, platinum electrode as positive electrode, voltage of 1.5V, direct current of 80mA, continuous culture for 4 days, and monitoring pH, ORP and Fe of culture solution2+And (4) concentration.
Treating the cultured mixed solution by using a sand core filtering device, respectively collecting filtrate and filter residue, analyzing by using an inductively coupled plasma atomic emission spectrometer, wherein impurity metals in the filtrate are not detected, only metal palladium is detected in the filter residue, and an X-ray diffractometer scans the phase of the filter residue, so that only an obvious and disordered carbon peak is displayed as a result.
Example 4
Continuously crushing the waste palladium-carbon catalyst for many times by using a handheld crusher, and sieving by using a national standard sieve (made of nylon material) to obtain waste palladium-carbon catalyst powder with the particle size of 1.0 mm. The direct current with the voltage of 1.5V and the current of 0-100mA is utilized, and the adding amount of the waste palladium-carbon catalyst powder is (2, 4, 6, 8, 10) g/50mLA. f + A. tAnd (4) carrying out continuous domestication treatment to obtain a bacterial liquid with the oxidation-reduction potential higher than 600 mV.
According to the waste palladium-carbon catalyst powder andA. f + A. tthe leaching experiment is carried out by adding 5g/50mL of the solution, and at the moment, the micro-electric field is applied: taking graphite carbon rod as negative electrode, platinum electrode as positive electrode, voltage of 1.5V, direct current of 80mA, continuously culturing for 6 days, monitoring pH, ORP and Fe of culture solution2+And (4) concentration.
Treating the cultured mixed solution by using a sand core filtering device, respectively collecting filtrate and filter residue, analyzing by using an inductively coupled plasma atomic emission spectrometer, wherein impurity metals in the filtrate are not detected, only metal palladium is detected in the filter residue, and an X-ray diffractometer scans the phase of the filter residue, so that only an obvious and disordered carbon peak is displayed as a result.
Comparative example 1
Continuously crushing the waste palladium-carbon catalyst for many times by using a handheld crusher, and sieving by using a national standard sieve (made of nylon material) to obtain waste palladium-carbon catalyst powder with the particle size of 1.0 mm. The direct current with the voltage of 1.5V and the current of 0-100mA is utilized, and the adding amount of the waste palladium-carbon catalyst powder is (2, 4, 6, 8, 10) g/50mLA. f + A. tAnd (4) carrying out continuous domestication treatment to obtain a bacterial liquid with the oxidation-reduction potential higher than 600 mV.
According to the waste palladium-carbon catalyst powder andA. f + A. tadding the solution in a proportion of 5g/50mL for leaching experiment, continuously culturing for 6 days without applying a micro electric field, and monitoring the pH, ORP and Fe of the culture solution in the process2+And (4) concentration.
And (2) treating the cultured mixed solution by using a sand core filtering device, respectively collecting filtrate and filter residue, analyzing by using an inductively coupled plasma atomic emission spectrometer, detecting impurity metals in the filtrate, detecting a large amount of impurity metals and palladium in the filter residue, scanning the phase of the filter residue by using an X-ray diffractometer, and displaying a relatively obvious and disordered carbon peak and inorganic compounds containing the impurity metals.
Comparative example 2
Continuously crushing the waste palladium-carbon catalyst for many times by using a handheld crusher, and sieving by using a national standard sieve (made of nylon material) to obtain waste palladium-carbon catalyst powder with the particle size of 1.0 mm. The direct current with the voltage of 1.5V and the current of 0-100mA is utilized, and the adding amount of the waste palladium-carbon catalyst powder is (2, 4, 6, 8, 10) g/50mLA. fAnd (4) carrying out continuous domestication treatment to obtain a bacterial liquid with the oxidation-reduction potential higher than 550 mV.
According to the waste palladium-carbon catalyst powder andA. fthe leaching experiment is carried out by adding 5g/50mL of the solution, and at the moment, the micro-electric field is applied: taking graphite carbon rod as negative electrode, platinum electrode as positive electrode, voltage of 1.5V, direct current of 40mA, continuously culturing for 5 days, monitoring pH, ORP and Fe of culture solution2+And (4) concentration.
And (3) treating the cultured mixed solution by using a sand core filtering device, respectively collecting filtrate and filter residue, analyzing by using an inductively coupled plasma atomic emission spectrometer, wherein impurity metals in the filtrate are not detected, a small amount of impurity metals and palladium are detected in the filter residue, and scanning the phase of the filter residue by using an X-ray diffractometer to show a relatively obvious and disordered carbon peak and inorganic compounds containing the impurity metals.
Comparative example 3
Continuously crushing the waste palladium-carbon catalyst for many times by using a handheld crusher, and sieving by using a national standard sieve (made of nylon material) to obtain waste palladium-carbon catalyst powder with the particle size of 1.0 mm. The direct current with the voltage of 1.5V and the current of 0-100mA is utilized, and the adding amount of the waste palladium-carbon catalyst powder is (2, 4, 6, 8, 10) g/50mLA. tAnd (4) carrying out continuous domestication treatment to obtain a bacterial liquid with the oxidation-reduction potential higher than 550 mV.
According to the waste palladium-carbon catalyst powder andA. tleaching experiment is carried out by adding 5g/50mL of the raw materialsAt this time, the condition of applying the micro electric field: taking graphite carbon rod as negative electrode, platinum electrode as positive electrode, voltage of 1.5V, direct current of 40mA, continuously culturing for 5 days, monitoring pH, ORP and Fe of culture solution2+And (4) concentration.
And (3) treating the cultured mixed solution by using a sand core filtering device, respectively collecting filtrate and filter residue, analyzing by using an inductively coupled plasma atomic emission spectrometer, wherein impurity metals in the filtrate are not detected, a small amount of impurity metals and palladium are detected in the filter residue, and scanning the phase of the filter residue by using an X-ray diffractometer to show a relatively obvious and disordered carbon peak and inorganic compounds containing the impurity metals.
The test results of examples 1 to 4 and comparative examples 1 to 3 are shown in Table 1:
TABLE 1
In summary, the invention providesA. f + A. tThe catalyst is coupled with a direct current micro-electric field to efficiently and selectively remove impurity metals in the waste palladium-carbon catalyst, thereby avoiding impurity interference in the subsequent palladium enrichment process. The whole recovery process is environment-friendly and pollution-free, the filtered filtrate can be recycled, the recovery rate is high, and resources are fully utilized. The micro electric field releases heat in the action process, and the whole reaction system does not need to provide an additional heat source, so that the energy consumption is greatly reduced; the filtrate generated after the micro-electric field and microorganism coupling treatment does not need further treatment, and the impurity metal is deposited on the negative electrode. Therefore, the invention has the advantages of higher environmental protection benefit and economic benefit, and the like.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A method for treating impurity metals in a waste palladium-carbon catalyst by micro-electric field coupling microorganisms is characterized by comprising the following steps:
(1) domesticated acidophilic thiobacillus ferrooxidans (B), (B)Acidithiobacillus ferrooxidansFor shortA.f) And Acidithiobacillus thiooxidans (A), (B), (C)Acidithiobacillus thiooxidansFor shortA.t) The mixed bacteria culture solution and the waste palladium-carbon catalyst powder are mixed and cultured according to a certain proportion, and the oxidation-reduction potential of the mixed bacteria culture solution is between 500 and 650 mV;
(2) applying an external micro-electric field in the culture system in the step (1), and continuously culturing for a period of time;
(3) and (3) filtering the mixture obtained in the step (2) to respectively obtain filtrate and filter residue, wherein the obtained filter residue contains active carbon and palladium and does not contain impurity metals, and the impurity metals comprise Cu, Ni, Pb, Cd and Al.
2. The method for treating impurity metals in the waste palladium-carbon catalyst by the micro-electric field coupling microorganism according to claim 1, which is characterized in that: in the step (1), before mixed culture, the waste palladium catalyst powder is screened by a nylon sieve, so that the particle size of the waste palladium catalyst powder is 0.5-1.5 mm.
3. The method for treating impurity metals in the waste palladium-carbon catalyst by the micro-electric field coupling microorganism according to claim 1, which is characterized in that: in step (1), theA. The domestication method of the f + A.t mixed bacteria comprises the following steps: with a voltage of 1.5V, the direct current with the current of 0-100mA, the addition amount of the waste palladium carbon catalyst powder is 2g, 4g, 6g, 8g, 10g to A, f+ A. tContinuous domestication treatment is carried out to obtain bacteria liquid with the oxidation-reduction potential of 500-650 mV.
4. The method for treating impurity metals in the waste palladium-carbon catalyst by the micro-electric field coupling microorganism according to claim 1, which is characterized in that: in the step (1), the waste palladium catalyst powder and the domesticated palladium catalyst powderA. f + A. tThe addition ratio of the mixed bacteria culture solution is (1-10) g/50 mL.
5. The method for treating impurity metals in the waste palladium-carbon catalyst by the micro-electric field coupling microorganism according to claim 1, which is characterized in that: in the step (2), the negative electrode material used by the micro electric field is one of a graphite carbon rod, graphite carbon cloth and a platinum electrode, the positive electrode material is a platinum electrode, the parameters of the micro electric field are voltage 1.5V and direct current 20-80 mA; the culture time is 4-6 days.
6. The method for treating impurity metals in the waste palladium-carbon catalyst by the micro-electric field coupling microorganism according to claim 1, which is characterized in that: and (4) returning the filtrate obtained in the step (3) to the leaching system in the step (1) for recycling, and discharging no waste liquid in the technical process.
7. The method for treating impurity metals in the waste palladium-carbon catalyst by the micro-electric field coupling microorganism according to claim 1, which is characterized in that: and (4) refining and purifying the filter residue obtained in the step (3) by a wet process to obtain the metal palladium.
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