CN108480647B - Recycling method of nano-silver particle waste liquid - Google Patents
Recycling method of nano-silver particle waste liquid Download PDFInfo
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- CN108480647B CN108480647B CN201810064851.0A CN201810064851A CN108480647B CN 108480647 B CN108480647 B CN 108480647B CN 201810064851 A CN201810064851 A CN 201810064851A CN 108480647 B CN108480647 B CN 108480647B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
- C22B11/021—Recovery of noble metals from waste materials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/005—Separation by a physical processing technique only, e.g. by mechanical breaking
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a recycling method of nano silver particle waste liquid, which comprises the following steps: a waste liquid collecting step: centrifuging the nano silver particle stock solution, pouring out supernatant liquor, and collecting turbid liquid at the middle and bottom layers to obtain waste liquid; stirring: uniformly stirring the waste liquid, and calculating the content of silver in the waste liquid; the reaction steps are as follows: putting the waste liquid in a fume hood, adding ammonia water with the concentration of 5% while stirring, stirring after adding the ammonia water, and then standing to obtain a reaction liquid; a centrifugation step: centrifuging the reaction solution to obtain a centrifugate; and (3) drying: drying the centrifugate to obtain silver blocks; grinding: and grinding and crushing the silver blocks to obtain micron silver particles. The method can simply, conveniently and effectively recycle the silver in the nano silver particle waste liquid, reduce the waste of the silver, avoid the pollution to the environment, greatly reduce the usage amount of oxidants such as hydrogen peroxide and the like, and has the characteristics of high recovery rate, low cost and convenient operation.
Description
Technical Field
The invention relates to a resource recycling method, in particular to a recycling method of nano silver particle waste liquid.
Background
The recovery and utilization of the nano silver particle waste liquid refers to that the nano silver particles, which are main components in the waste liquid, are recovered after a large amount of waste liquid generated in the processes of purification, extraction and the like of the nano silver particles is subjected to certain treatment. The processed nano silver is gathered into irregular agglomerates with the grain diameter of micron and above, and the recovered silver blocks are ground into micron silver particles. The micron silver particles are silver particles with the particle diameter of micron level, have lasting antibacterial effect, and are suitable for the fields of personal care, medical use, medicine, animal health products and the like.
The rapid development of nano material technology and the wide application in various fields are known, but a lot of nano materials are inevitableThe material is released into the environment, such as waste liquid from the preparation of the nanomaterial, and then enriched in the organism through the food chain, producing toxic effects. At present, the nano materials are used in the world, wherein the usage amount of nano silver is the highest, and correspondingly, waste liquid generated during preparation in factories and laboratories is large. The related research shows that Ag+The background concentration in the environment is extremely low, and the concentration range in the natural water body only reaches 0.03-500 ng.L-1However, Ag + has a lasting and bioaccumulating effect in the environment and has strong toxicity to aquatic organisms, such as 50-100 ng.L of micro phytoplankton-1After Ag is contaminated, the reproductive capacity of the product is inhibited. The content of Ag in the waste liquid for preparing AgNPs is 1-4 g.L-1The present invention is necessary for the recovery of nano silver particles, since the effect of discharging to the environment cannot be expected. Studies by Choi et al indicate that AgNPs are able to inhibit the growth of nitrifying bacteria at 1 mg.L-1At the concentration of (A), the respiratory inhibition rate of the AgNPs to autotrophic nitrifying bacteria is as high as about 86%; miao et al demonstrated through studies that the artificially synthesized AgNPs severely inhibit cell growth, photosynthesis and chlorophyll synthesis of marine diatoms (Thalasiosis weissflogii); jang et al exposed carp in (0.62 + -0.12) mg/L nano silver suspension for 7 days, and found that the amount of silver distributed in different organs of the fish varies from large to small, such as liver, gill, gastrointestinal tract, skeletal muscle, brain, blood; after 2 weeks of decontamination, the silver concentrations in the liver, gill and gastrointestinal tract were still high. AgNPs existing in fish bodies can further inhibit the activity of certain enzymes in the fish bodies, interfere normal ion regulation and nerve regulation, even cause malformation of fish embryos, reduce the survival rate of the embryos and the like. Then the fishes are transmitted through a food chain, are biologically enriched and the like, and are enriched in a human body after being eaten by human beings so as to generate a series of toxic effects. Research shows that the toxic effect of the nano silver particles is mainly caused by silver ions dissolved and released when the particle size is 20-80 nm, and the nano silver particles with smaller particle size, such as 10nm, are more easily utilized by organisms compared with the silver ions, so that the toxic effect is larger. In the current preparation process of nano silver particles at home and abroad, the nano silver particles remained in the waste liquid are mainly below 30nm,because the separation and purification of nano silver particles with the particle size of less than 30nm are still difficult in the prior art. It is necessary to reduce the content of the smaller nano silver particles in the waste liquid by using the method of the invention to agglomerate the smaller nano silver particles into larger agglomerates.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a method for recycling the nano-silver particle waste liquid, which can simply, conveniently and effectively recycle the silver in the nano-silver particle waste liquid, reduce the waste of the silver, avoid the pollution to the environment, greatly reduce the usage amount of oxidants such as hydrogen peroxide and the like, and has the characteristics of high recovery rate, low cost and convenient operation.
The purpose of the invention is realized by adopting the following technical scheme:
a method for recycling nano silver particle waste liquid is characterized by comprising the following steps:
a waste liquid collecting step: centrifuging the nano silver particle stock solution in a centrifuge of 4000-7000r/mind for 30-60min, wherein the obvious layering phenomenon can occur in the centrifugal solution, pouring the upper transparent solution, and collecting the bottom turbid solution, namely the waste solution;
stirring: uniformly stirring the waste liquid, measuring the solid content of the waste liquid, weighing the total weight of the waste liquid, and calculating the content of silver in the waste liquid;
the reaction steps are as follows: placing the waste liquid in a ventilation cabinet, adding 5% ammonia water while stirring, stirring after adding the ammonia water, wherein the stirring speed is 100-;
a centrifugation step: centrifuging the reaction solution to obtain a centrifugate;
and (3) drying: drying the centrifugate to obtain silver blocks;
grinding: and grinding and crushing the silver blocks to obtain micron silver particles.
Further, in the step of collecting the waste liquid, the centrifugation is performed for 5 times, the waste liquid obtained by each centrifugation is integrated, and 0.5-1L of the waste liquid is recovered from every 10L of the nano silver particle stock solution.
Further, in the stirring step, the stirring speed is 100-300r/min, and the stirring time is 5-15 min.
Further, in the reaction step, the mass volume ratio of the silver in the waste liquid to the ammonia water is (7-21): 20-50) g/ml.
Further, in the reaction step, the stirring speed is 200r/min, the stirring time is 10min, and then the mixture is kept still for 2 days.
Further, in the reaction step, ammonia water with the concentration of 5% is obtained by adopting a field preparation method, and the specific preparation method comprises the following steps: diluting a certain amount of 28% ammonia water to 5% ammonia water.
Further, in the centrifugation step, the centrifugation speed is 5000-7000r/min, and the centrifugation time is 40-50 min.
Further, in the centrifugation step, the centrifugation speed is 6000r/min, and the centrifugation time is 45 min.
Further, in the drying step, the drying temperature is 120-150 ℃, and the drying time is 1-2 h.
Further, in the drying step, the drying temperature is 130 ℃, and the drying time is 1.5 h.
Compared with the prior art, the invention has the beneficial effects that:
the recycling method of the invention obtains the micron silver particles through the steps of waste liquid collection, stirring, reaction, centrifugation, drying and grinding in sequence, can simply, conveniently and effectively recycle the silver in the nano silver particle waste liquid, reduces the waste of the silver, avoids the pollution to the environment, greatly reduces the usage amount of oxidants such as hydrogen peroxide and the like, and has the characteristics of high recovery rate, low cost and convenient operation.
In general, the release of AgNPs, directly or indirectly, into the environment would have an unpredictable effect. The method of the invention enables AgNPs to be agglomerated into agglomerates with particle sizes of micron and above, thereby eliminating the special physical and chemical characteristics of the AgNPs at the nanometer level, greatly reducing the toxicity of silver to the environment and the like, and simultaneously increasing the utilization rate and the additional application value of the silver by recycling.
Detailed Description
The present invention is further described below with reference to specific embodiments, and it should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment. The materials used in this example are all commercially available.
A recycling method of nano silver particle waste liquid comprises the following steps:
a waste liquid collecting step: centrifuging the nano silver particle stock solution in a centrifuge of 4000-7000r/mind for 30-60min, wherein the obvious layering phenomenon can occur in the centrifugal solution, pouring the upper transparent solution, and collecting the bottom turbid solution, namely the waste solution; because the highest rotating speed of 6 x 1000ml of the high-speed large-capacity refrigerated centrifuge at home and abroad is 8000r/min at present, and nano silver particles with relatively low particle size (the particle size is less than 30nm) are difficult to centrifuge out, unless the rotating speed of the centrifuge reaches 13000r/min or above, the stock solution which can be processed by the centrifuge with the centrifugal rotating speed is very little, about 6 x 10ml, and the centrifuge has no great application value when being used in an enterprise factory. However, the loss of some nano silver particles with small particle size can be caused by using large capacity, and the nano silver particles are mainly distributed on the bottom layer of the centrifugal bottle, so that the nano silver particles can be recycled, and the influence caused by accidental discharge to the environment is avoided;
stirring: uniformly stirring the waste liquid, measuring the solid content of the waste liquid, weighing the total weight of the waste liquid, and calculating the content of silver in the waste liquid; this step is mainly to roughly understand the content of silver in the waste liquid, and certainly there may be some PVP, etc., by which the recovery percentage of silver in the recovered waste liquid can be understood.
The reaction steps are as follows: placing the waste liquid in a ventilation cabinet, adding 5% ammonia water while stirring, stirring after adding the ammonia water, wherein the stirring speed is 100-;
a centrifugation step: centrifuging the reaction solution to obtain a centrifugate;
and (3) drying: and drying the centrifugate to obtain silver blocks.
Grinding: and grinding and crushing the silver blocks to obtain micron silver particles.
In a preferred embodiment, in the step of collecting the waste liquid, the number of times of centrifugation is 5, the waste liquid obtained by each centrifugation is integrated, and 0.5-1L of waste liquid is recovered per 10L of the nano silver particle stock solution. In the step, the centrifugation times are 5, the waste liquid obtained by each centrifugation is integrated, so that about 15L or more of solvent is consumed, and the turbid liquid is concentrated to 0.5-1L through the process of collecting the turbid liquid, so that the subsequent treatment work is greatly reduced.
As a preferred embodiment, in the stirring step, the stirring speed is 100-300r/min, and the stirring time is 5-15 min.
In a preferred embodiment, in the reaction step, the mass-to-volume ratio of the silver in the waste liquid to the ammonia water is (7-21): 20-50) g/ml.
In a preferred embodiment, in the reaction step, the stirring speed is 200r/min, the stirring time is 10min, and then the mixture is allowed to stand for 2 days.
In a preferred embodiment, the ammonia water with a concentration of 5% is prepared in situ in the reaction step by the following specific preparation method: diluting a certain amount of 28% ammonia water to 5% ammonia water.
As a preferred embodiment, in the centrifugation step, the centrifugation speed is 7000r/min 5000-.
In a preferred embodiment, in the centrifugation step, the centrifugation speed is 6000r/min and the centrifugation time is 45 min.
In a preferred embodiment, in the drying step, the drying temperature is 120-.
In a preferred embodiment, in the drying step, the drying temperature is 130 ℃ and the drying time is 1.5 h.
Example 1:
a recycling method of nano silver particle waste liquid comprises the following steps:
a waste liquid collecting step: centrifuging 10L of nano silver particle stock solution in a centrifuge of 4000-7000r/mind for 30-60min, at the moment, obviously layering in the centrifugal solution, pouring out the upper transparent solution, and collecting the bottom turbid solution to obtain 1.2L of waste solution;
stirring: uniformly stirring the waste liquid, measuring the solid content of the waste liquid, weighing the total weight of the waste liquid, and calculating the silver content in the waste liquid to be 20.1080 g; stirring at 100r/min for 15 min;
the reaction steps are as follows: placing the waste liquid in a fume hood, adding 20mL of 5% ammonia water while stirring, stirring after adding the ammonia water, wherein the stirring speed is 100r/min, the stirring time is 15min, and then standing for 2 days to obtain a reaction liquid; wherein the mass volume ratio of the silver in the waste liquid to the ammonia water is 20.1080g:20 mL;
the ammonia water with the concentration of 5% is obtained by adopting a field preparation method, and the specific preparation method comprises the following steps: diluting a certain amount of 28% ammonia water to 5% ammonia water.
A centrifugation step: and centrifuging the reaction solution at the speed of 5000r/min for 50min to obtain a centrifugate.
And (3) drying: and drying the centrifugate at 120 ℃ for 2h to obtain the silver blocks.
Grinding: and grinding and crushing the silver blocks to obtain micron silver particles.
Example 2:
a recycling method of nano silver particle waste liquid comprises the following steps:
a waste liquid collecting step: centrifuging 10L of nano silver particle stock solution in a centrifuge of 4000-7000r/mind for 30-60min, at the moment, obviously layering in the centrifugal solution, pouring out the upper transparent solution, and collecting the bottom turbid solution to obtain 1.2L of waste solution;
stirring: uniformly stirring the waste liquid, measuring the solid content of the waste liquid, weighing the total weight of the waste liquid, and calculating the silver content in the waste liquid to be 8.2711 g; stirring at 300r/min for 5 min; (ii) a
The reaction steps are as follows: placing the waste liquid in a fume hood, adding 30mL of 5% ammonia water while stirring, stirring after adding the ammonia water, wherein the stirring speed is 100r/min, the stirring time is 10min, and then standing for 1 day to obtain a reaction liquid; wherein the mass volume ratio of the silver in the waste liquid to the ammonia water is 8.2711g:30 mL;
the ammonia water with the concentration of 5% is obtained by adopting a field preparation method, and the specific preparation method comprises the following steps: diluting a certain amount of 28% ammonia water to 5% ammonia water.
A centrifugation step: and centrifuging the reaction solution at 7000r/min for 40min to obtain a centrifugate.
And (3) drying: and drying the centrifugate at 150 ℃ for 1h to obtain silver blocks.
Grinding: and grinding and crushing the silver blocks to obtain micron silver particles.
Example 3:
a recycling method of nano silver particle waste liquid comprises the following steps:
a waste liquid collecting step: centrifuging 10L of nano silver particle stock solution in a centrifuge of 4000-7000r/mind for 30-60min, at the moment, obviously layering in the centrifugal solution, pouring out the upper transparent solution, and collecting the bottom turbid solution to obtain 1.2L of waste solution;
stirring: uniformly stirring the waste liquid, measuring the solid content of the waste liquid, weighing the total weight of the waste liquid, and calculating the silver content in the waste liquid to be 7.5900 g; stirring at 300r/min for 5 min; (ii) a
The reaction steps are as follows: placing the waste liquid in a fume hood, adding 30mL of 5% ammonia water while stirring, stirring after adding the ammonia water, wherein the stirring speed is 200r/min, the stirring time is 10min, and then standing for 2 days to obtain a reaction liquid; wherein the mass volume ratio of the silver in the waste liquid to the ammonia water is 7.5900g:30 mL;
the ammonia water with the concentration of 5% is obtained by adopting a field preparation method, and the specific preparation method comprises the following steps: diluting a certain amount of 28% ammonia water to 5% ammonia water.
A centrifugation step: and centrifuging the reaction solution at the speed of 6000r/min for 45min to obtain a centrifugate.
And (3) drying: and drying the centrifugate at the temperature of 130 ℃ for 1.5h to obtain the silver blocks.
Grinding: and grinding and crushing the silver blocks to obtain micron silver particles.
Example 4:
a recycling method of nano silver particle waste liquid comprises the following steps:
a waste liquid collecting step: centrifuging 10L of nano silver particle stock solution in a centrifuge of 4000-7000r/mind for 30-60min, at the moment, obviously layering in the centrifugal solution, pouring out the upper transparent solution, and collecting the bottom turbid solution to obtain 1.2L of waste solution;
stirring: uniformly stirring the waste liquid, measuring the solid content of the waste liquid, weighing the total weight of the waste liquid, and calculating the silver content in the waste liquid to be 19.866 g; stirring at 200r/min for 15 min;
the reaction steps are as follows: placing the waste liquid in a fume hood, adding 50ml of 5% ammonia water while stirring, stirring after adding the ammonia water, wherein the stirring speed is 200r/min, the stirring time is 10min, and then standing for 1 day to obtain a reaction liquid; wherein the mass volume ratio of the silver in the waste liquid to the ammonia water is 19.866g:50 ml;
the ammonia water with the concentration of 5% is obtained by adopting a field preparation method, and the specific preparation method comprises the following steps: diluting a certain amount of 28% ammonia water to 5% ammonia water.
A centrifugation step: and centrifuging the reaction solution at the speed of 6000r/min for 50min to obtain a centrifugate.
And (3) drying: and drying the centrifugate at 150 ℃ for 1h to obtain silver blocks.
Grinding: and grinding and crushing the silver blocks to obtain micron silver particles.
Comparative example 1:
a method for treating nano silver particle waste liquid by hydrogen peroxide comprises the following steps:
1) pouring 10L of waste liquid generated in the production process of the nano silver particles into a waste liquid tank;
2) adding hydrogen peroxide into a waste liquid tank, wherein 3000ml of hydrogen peroxide 2000-containing solution with the concentration of 30% needs to be added;
3) and discharging the waste liquid in the waste liquid tank after the waste liquid in the waste liquid tank becomes clear and transparent from turbidity.
Effect testing
Take the waste liquid generated by 10L of the original liquid of the nano silver particles as an example. 3000ml of hydrogen peroxide 2000-with a consumption concentration of 30% is needed in the comparative example 1, while 20-50ml of ammonia water with a concentration of 5% is needed in the treatment of the method of the examples 1-4, so that the use amount of the raw materials is greatly reduced. And recycling the silver particles also reduces their potential threat to the environment and adds additional revenue.
After the nano silver particle waste liquid is treated in the embodiments 1 to 4 of the invention, the following data in table 1 are obtained through measurement and calculation:
TABLE 1
| Recover silver quality (g) | Measuring the content (g) of silver in the waste liquid | Recovery (%) | |
| Example 1 | 10.3677 | 20.1080 | 51.56 |
| Example 2 | 5.7370 | 8.2711 | 69.36 |
| Example 3 | 6.5028 | 7.5900 | 85.67 |
| Example 4 | 15.1769 | 19.866 | 76.39 |
As can be seen from Table 1, the recovery rates of examples 1 to 4 reached 50% or more, and particularly, the recovery rate of example 3 reached the highest 85.67%.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (9)
1. A method for recycling nano silver particle waste liquid is characterized by comprising the following steps:
a waste liquid collecting step: centrifuging the nano silver particle stock solution in a centrifuge with the speed of 4000-7000r/min for 30-60min, pouring out the transparent liquid on the upper layer, and collecting the turbid liquid on the bottom layer, namely the waste liquid;
stirring: uniformly stirring the waste liquid, measuring the solid content of the waste liquid, weighing the total weight of the waste liquid, and calculating the content of silver in the waste liquid;
the reaction steps are as follows: placing the waste liquid in a ventilation cabinet, adding 5% ammonia water while stirring, stirring after adding the ammonia water, wherein the stirring speed is 100-; the mass volume ratio of the silver in the waste liquid to the ammonia water is (7-21) to (20-50) g/ml;
a centrifugation step: centrifuging the reaction solution to obtain a centrifugate;
and (3) drying: drying the centrifugate to obtain silver blocks;
grinding: and grinding and crushing the silver blocks to obtain micron silver particles.
2. The method for recycling silver nanoparticle waste liquid according to claim 1, wherein in the step of collecting the waste liquid, the number of times of centrifugation is 5, the waste liquid obtained by each centrifugation is integrated, and 0.5-1L of the waste liquid is recovered per 10L of the silver nanoparticle stock solution.
3. The recycling method of the silver nanoparticle waste liquid as claimed in claim 1, wherein in the stirring step, the stirring speed is 100-300r/min, and the stirring time is 5-15 min.
4. The method for recycling the nano silver particle waste liquid as claimed in claim 1, wherein in the reaction step, the stirring speed is 200r/min, the stirring time is 10min, and then the reaction solution is allowed to stand for 2 days.
5. The recycling method of the nano silver particle waste liquid as claimed in claim 1, wherein in the reaction step, the ammonia water with the concentration of 5% is obtained by adopting a field preparation method, and the specific preparation method is as follows: diluting a certain amount of 28% ammonia water to 5% ammonia water.
6. The method for recycling the waste liquid of silver nanoparticles as claimed in claim 1, wherein in the centrifugation step, the centrifugation speed is 5000-7000r/min, and the centrifugation time is 40-50 min.
7. The recycling method of the nano silver particle waste liquid as claimed in claim 6, wherein in the centrifugation step, the centrifugation speed is 6000r/min, and the centrifugation time is 45 min.
8. The recycling method of the nano silver particle waste liquid as claimed in claim 1, wherein in the drying step, the drying temperature is 120-.
9. The recycling method of the nano silver particle waste liquid according to claim 8, wherein in the drying step, the drying temperature is 130 ℃ and the drying time is 1.5 h.
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