CN112284851A - Preparation method of nontoxic nano-scale plastic microparticles - Google Patents
Preparation method of nontoxic nano-scale plastic microparticles Download PDFInfo
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- CN112284851A CN112284851A CN202011151829.3A CN202011151829A CN112284851A CN 112284851 A CN112284851 A CN 112284851A CN 202011151829 A CN202011151829 A CN 202011151829A CN 112284851 A CN112284851 A CN 112284851A
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Abstract
The invention discloses a preparation method of nontoxic nano plastic microparticles. Dissolving plastics in high-concentration sulfuric acid aqueous solution, adding low-concentration sulfuric acid solution to separate out small-particle plastics, simultaneously stirring at high speed to prevent the plastic particles from forming flocculent precipitates, adding a biosurfactant to prevent the plastic nanoparticles from agglomerating and precipitating, and standing to take supernatant to obtain nano-scale particles. The method is suitable for plastics soluble in concentrated aqueous sulfuric acid, preferably polyethylene terephthalate (PET); the safe and nontoxic biosurfactant is used, so that the problem that the interference result caused by the overlarge toxicity of the surfactant is generated in the subsequent biological toxicology experiment is solved; the dissolution time is greatly reduced by using sulfuric acid as a solvent; the operation is simple, heating is not needed, and chemicals with volatile toxicity are not used as solvents.
Description
Technical Field
The invention relates to the field of environmental materials, in particular to a preparation method of a material required by quantitative detection and toxicological analysis of nano plastic particles.
Background
The plastic is widely applied to modern life and production, and the derived micro-plastic and nano-plastic are proved to be accumulated in various environmental media. Nano-plastics are a global pollution problem, and the negative effects of nano-plastics on the ecosystem and the toxicological effects on organisms are the research hotspots of the present school community. At present, the most extensive research on the toxicological effect is the Polystyrene (PS) plastic which can be industrially produced, and the research finds that the PS nano plastic has obvious toxicological effect on organisms such as zebra fish and the like due to the extremely small diameter and high cell adsorption capacity of the nano plastic, and has obvious effect on a lung cell line in an in vitro experiment. Polyethylene terephthalate (PET) is one of the most widely applied plastics, and the yield of PET in China in 2018 reaches 4542 ten thousand tons. PET (polyethylene terephthalate), also called terylene, is often used as a clothing material in daily life, and a certain amount of PET plastic is detected in indoor dust, but the toxic effect of nano PET plastic on human bodies is still unknown, so that the research on the toxicological effect of nano PET is urgent. Because no industrially produced nano PET plastic exists at present, chemical surfactants such as Sodium Dodecyl Sulfate (SDS) and the like are mostly used in the process of preparing the nano PET plastic in a laboratory, and the toxicity of the reagent can interfere with subsequent toxicology experiments, the development of the method for preparing the nano PET plastic, which is simple in operation and has no biological toxicity, is necessary.
Disclosure of Invention
The invention provides a preparation method of nontoxic nano plastic microparticles.
Dissolving plastics in high-concentration sulfuric acid aqueous solution at normal temperature, adding low-concentration sulfuric acid solution to separate out small-particle plastics, adding biosurfactant to prevent plastic nanoparticles from aggregating and precipitating, standing, and taking supernatant to obtain nano-particles. The method comprises the following specific steps:
(1) weighing 1g of plastic powder, placing the plastic powder in a 100mL round-bottom flask, adding a certain amount of high-concentration sulfuric acid aqueous solution, and stirring for 30min to completely dissolve the plastic powder; (2) adding a certain amount of low-concentration sulfuric acid aqueous solution while stirring to separate out massive plastic with a certain diameter, cooling the round-bottom flask to room temperature, and continuing stirring for 2 hours until white suspension appears in the round-bottom flask; (3) transferring the suspension into a 50mL centrifuge tube, centrifuging the centrifuge tube for 1h at 2800g in a low speed centrifuge, transferring the upper layer of plastic into another centrifuge tube, adding 30mL of ultrapure water, oscillating for 10min at 180r/min to resuspend the precipitate in water, centrifuging for 1h at 2800g again, removing the supernatant, and repeating the operation until the pH of the suspension is 7; (4) a certain amount of biosurfactant was weighed into a 250mL beaker, dissolved by adding 20mL of ultrapure water, and the neutral suspension obtained in the previous step was transferred to the beaker, to which 100mL of pure water was added. Stirring for 10min, performing ultrasonic treatment for 20min, oscillating for 20min at a speed of 180r/min, dividing 100mL of suspension into 4 parts on average, respectively transferring the 4 parts to a 50mL centrifuge tube, standing for 48h, taking the upper layer of suspension, performing ultrasonic treatment for 1h, and measuring the particle size distribution of the suspension by using a nanometer particle size and zeta potential molecular weight analyzer;
the preparation method of the nontoxic nano plastic microparticles comprises the steps of dissolving plastic in a high-concentration sulfuric acid aqueous solution at room temperature;
the plastics are soluble in concentrated sulfuric acid, such as polyethylene terephthalate (PET), Polyamide (PA), Polyacrylonitrile (PAN) and the like; preferably, the plastic is PET;
the concentration of the high-concentration sulfuric acid aqueous solution is 80-95% by volume;
the concentration of the low-concentration sulfuric acid aqueous solution is 5-20% by volume;
the biosurfactant is rhamnolipid;
the addition amount of the rhamnolipid is 0.0005-0.005 g;
the diameter of the precipitated massive plastic is 2-3 cm;
the rotating speed of the centrifuge is more than 2800g during centrifugal cleaning.
(2) The invention has the following positive effects:
the method does not need heating treatment and is simple to operate; the safe and nontoxic biosurfactant is used, so that the problem that the interference result caused by the overlarge toxicity of the surfactant is generated in the subsequent biological toxicology experiment is solved; the dissolution time is greatly reduced by using sulfuric acid as a solvent; no volatile toxic chemicals are used as solvents.
Drawings
FIG. 1 is a particle size distribution of nano PET plastic micro-particles prepared in example 1;
FIG. 2 is a particle size distribution of nano PET plastic micro-particles prepared in example 2;
FIG. 3 is a particle size distribution of nano PET plastic micro-particles prepared in example 3;
FIG. 4 is a particle size distribution of nano PET plastic micro-particles prepared in example 4.
Detailed Description
The following examples are further detailed descriptions of the present invention:
example 1:
weighing 1g of PET powder, placing the PET powder in a 100mL round-bottom flask, adding 10mL of sulfuric acid aqueous solution with the volume fraction of 90%, stirring until the solution is completely dissolved, adding 10mL of 20% sulfuric acid solution while stirring, cooling to room temperature, continuing to stir for 2h, transferring the suspension to a 50mL centrifuge tube, centrifuging for 1h 2800g, transferring the upper PET plastic to another centrifuge tube, centrifugally cleaning for 5 times, measuring the pH of the solution to be 7, transferring the precipitate to a 50mL centrifuge tube, dissolving 0.001g of rhamnolipid in 100mL of pure water, adding 25mL of rhamnolipid solution into the centrifuge tube of the precipitate, performing ultrasonic treatment for 20min, oscillating for 20min at 180r/min, standing for 48h, taking the upper suspension, performing ultrasonic treatment for 1h, taking 1.5mL of the upper suspension, analyzing the particle size of the suspension by using a nanometer particle size and zeta potential molecular weight analyzer, and measuring the particle size distribution to be 295-615nm as shown in FIG.
Example 2:
weighing 1g of PET powder, placing the PET powder in a 100mL round-bottom flask, adding 10mL of sulfuric acid aqueous solution with volume fraction of 90%, stirring until the solution is completely dissolved, adding 10mL of 10% sulfuric acid solution while stirring, cooling to room temperature, continuing to stir for 2h, transferring the suspension to a 50mL centrifuge tube, centrifuging for 1h 2800g, transferring the upper PET plastic to another centrifuge tube, centrifuging and cleaning for 4 times, measuring the pH of the solution to be 7, transferring the precipitate to a 50mL centrifuge tube, dissolving 0.001g of rhamnolipid in 100mL of pure water, adding 25mL of rhamnolipid solution into the centrifuge tube of the precipitate, performing ultrasonic treatment for 20min, oscillating for 20min at 180r/min, standing for 48h, taking the upper suspension, performing ultrasonic treatment for 1h, taking 1.5mL of the upper suspension, analyzing the particle size of the suspension by using a nanometer particle size and zeta potential molecular weight analyzer, and measuring the particle size distribution to be 459nm as shown in FIG..
Example 3:
weighing 1g of PET powder, placing the PET powder in a 100mL round bottom flask, adding 10mL of sulfuric acid aqueous solution with volume fraction of 85%, stirring until the solution is completely dissolved, adding 10mL of 10% sulfuric acid solution while stirring, cooling to room temperature, continuing to stir for 2h, transferring the suspension to a 50mL centrifuge tube, centrifuging for 1h 2800g, transferring the upper PET plastic to another centrifuge tube, centrifugally cleaning for 5 times, measuring the pH of the solution to be 7, transferring the precipitate to a 50mL centrifuge tube, dissolving 0.001g of rhamnolipid in 100mL of pure water, adding 25mL of rhamnolipid solution into the centrifuge tube of the precipitate, performing ultrasonic treatment for 20min, oscillating for 20min at 180r/min, standing for 48h, taking the upper suspension, performing ultrasonic treatment for 1h, taking 1.5mL of the upper suspension, analyzing the particle size of the upper suspension by using a nanometer particle size and zeta potential molecular weight analyzer, and measuring the particle size distribution to be 91-142nm as shown in FIG.
Example 4:
weighing 1g of PET powder, placing the PET powder in a 100mL round-bottom flask, adding 10mL of sulfuric acid aqueous solution with volume fraction of 90%, stirring until the solution is completely dissolved, adding 10mL of 10% sulfuric acid solution while stirring, cooling to room temperature, continuing to stir for 2h, transferring the suspension to a 50mL centrifuge tube, centrifuging for 1h 2800g, transferring the upper PET plastic to another centrifuge tube, centrifuging and cleaning for 5 times, measuring the pH of the solution to be 7, transferring the precipitate to a 50mL centrifuge tube, dissolving 0.005g of rhamnolipid in 100mL of pure water, adding 25mL of rhamnolipid solution into the centrifuge tube with the precipitate, performing ultrasonic treatment for 20min, oscillating for 20min at 180r/min, standing for 48h, taking the upper suspension, performing ultrasonic treatment for 1h, taking 1.5mL of the upper suspension, analyzing the particle size of the suspension by using a nanometer particle size and zeta potential molecular weight analyzer, and measuring the particle size distribution to be 459nm as shown in FIG. 4.
Although the method of the present invention has been described in terms of preferred embodiments, it will be apparent to those skilled in the art that modifications and rearrangements of the method described herein can be made to achieve the desired results without departing from the spirit and scope of the invention. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the scope and spirit of the invention.
Claims (10)
1. A method for preparing nontoxic nanometer plastic microparticles is characterized in that plastic is dissolved in high-concentration sulfuric acid aqueous solution at room temperature, then low-concentration sulfuric acid solution is added to separate out small-particle plastic, biosurfactant is added to avoid agglomeration and precipitation of plastic nanoparticles, and the mixture is stood to obtain supernate to obtain nanometer particles, and the method comprises the following specific steps:
(1) weighing 1g of plastic powder, placing the plastic powder in a round-bottom flask, adding a certain amount of high-concentration sulfuric acid aqueous solution, and stirring for 30min to completely dissolve the plastic powder; (2) adding a certain amount of low-concentration sulfuric acid aqueous solution while stirring to separate out massive plastic with a certain diameter, cooling the round-bottom flask to room temperature, and continuing stirring for 2 hours until white suspension appears in the round-bottom flask; (3) transferring the suspension into a 50mL centrifuge tube, centrifuging the centrifuge tube for 1h at 2800g in a low speed centrifuge, transferring the upper layer of plastic into another centrifuge tube, adding 30mL of ultrapure water, oscillating for 10min at 180r/min to resuspend the precipitate in water, centrifuging for 1h at 2800g again, removing the supernatant, and repeating the operation until the pH of the suspension is 7; (4) a certain amount of biosurfactant was weighed into a 250mL beaker, dissolved by adding 20mL of ultrapure water, and the neutral suspension obtained in the previous step was transferred to the beaker, to which 100mL of pure water was added. Stirring for 10min, performing ultrasonic treatment for 20min, oscillating for 20min at a speed of 180r/min, dividing 100mL of suspension into 4 parts on average, respectively transferring the 4 parts to a 50mL centrifuge tube, standing for 48h, taking the upper suspension, performing ultrasonic treatment for 1h, and measuring the particle size distribution of the suspension by using a nanometer particle size and zeta potential molecular weight analyzer.
2. The method according to claim 1, wherein the plastic is a kind of plastic soluble in concentrated sulfuric acid.
3. The method for preparing according to claim 2, wherein the plastic is polyethylene terephthalate (PET), Polyamide (PA), Polyacrylonitrile (PAN), or the like; preferably, the plastic is PET.
4. The method of claim 1, wherein the step of preparing the nontoxic nanoscale plastic microparticles comprises: the plastic was dissolved in a high-concentration aqueous sulfuric acid solution at room temperature.
5. The concentrated aqueous sulfuric acid solution according to claim 4, which has a concentration of 80 to 95% by volume.
6. The method of claim 1, wherein the step of preparing the nontoxic nanoscale plastic microparticles comprises: the concentration of the low-concentration sulfuric acid aqueous solution is 5-20% by volume fraction.
7. The method of claim 1, wherein the step of preparing the nontoxic nanoscale plastic microparticles comprises: the biosurfactant is rhamnolipid.
8. The rhamnolipid according to claim 7 is added in an amount of 0.0005-0.005 g.
9. The method of claim 1, wherein the step of preparing the nontoxic nanoscale plastic microparticles comprises: the diameter of the separated block-shaped plastic is 2-3 cm.
10. The method of claim 1, wherein the step of preparing the nontoxic nanoscale plastic microparticles comprises: the rotating speed of the centrifuge is more than 2800g during centrifugal cleaning.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113916729A (en) * | 2021-10-08 | 2022-01-11 | 连云港市沃鑫高新材料有限公司 | Superfine silicon carbide tailing particle size classification test method |
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