CN112677368A - Plasma etching enhanced ternary mixed plastic flotation separation method - Google Patents
Plasma etching enhanced ternary mixed plastic flotation separation method Download PDFInfo
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- CN112677368A CN112677368A CN202011407273.XA CN202011407273A CN112677368A CN 112677368 A CN112677368 A CN 112677368A CN 202011407273 A CN202011407273 A CN 202011407273A CN 112677368 A CN112677368 A CN 112677368A
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Abstract
The invention belongs to the technical field of pollution prevention and recycling of solid wastes, and provides a plasma etching enhanced ternary mixed plastic flotation separation method. The method comprises seven core process links including pretreatment 1, pretreatment 2, plasma etching 1, flotation unit 1, pretreatment 3, plasma etching 2 and flotation unit 2; the seven process links are sequentially connected in series and can be continuously operated on line; the ternary mixed plastic fed by the pretreatment 1 comprises PMMA, PTFE and ABS which are from different sources; the sinking tailing 1 of the flotation unit 1 is the separated PMMA; the sinking tailing 2 of the flotation unit 2 is the separated PTFE; the floating product 2 of the flotation unit 2 is the separated ABS. The method has the advantages of simple flow, relatively mild process, no high-temperature pressurizing link, and high separation safety and efficiency.
Description
Technical Field
The invention belongs to the technical field of pollution prevention and recycling of solid wastes, particularly relates to a flotation separation technology of a plastic mixture, and particularly relates to a method for selectively enhancing the flotation separation capacity of mixed plastics by utilizing low-temperature plasma etching as pretreatment.
Background
At present, the economic and environmental losses caused by waste plastics are increasingly serious, the proportion of the waste plastics in common solid wastes is continuously increased, and the recycling treatment is widely concerned. The single kind of mixed plastics can realize material circulation through a simple remolding process or be cracked until monomers participate in chemical circulation. However, waste plastics collected from common solid waste streams often have an obvious associated relationship, and if the waste plastics are not separated and enter a recycling stage, heterogeneous components cause negative problems of main body polymerization cracking, decoloration, embrittlement and the like in a recovery process, so that the quality of regenerated plastics or pyrolysis oil is seriously reduced. Therefore, the effective separation of the waste plastic mixture has extremely important environmental and economic values for the recycling of the waste plastic mixture.
Polymethyl methacrylate (PMMA), Polytetrafluoroethylene (PTFE) and acrylonitrile/butadiene/styrene copolymer (ABS) are important engineering polymer materials, widely used in the manufacturing industry of automobiles, electronics and electrical equipment, and have a high proportion in solid waste streams such as automobile crushing residues (ASR) and waste electrical equipment (WEEE). For ternary mixed plastics consisting of PMMA, PTFE and ABS, no effective automatic separation method is reported except for manual sorting, and the recycling process of the waste plastics is greatly limited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for enhancing ternary mixed plastic flotation separation by plasma etching, so as to solve the problem of low efficiency of manual sorting, and further realize quick and efficient separation and recovery of common ternary mixed plastic wastes.
In order to achieve the technical objects, the present inventors have conducted extensive experimental studies and diligent research, and as a result, have obtained a method for selectively enhancing the flotation separation capability of mixed plastics by using low-temperature plasma etching as a pretreatment. Specifically, the technical scheme of the invention is summarized as follows:
a method for enhancing ternary mixed plastic flotation separation by plasma etching comprises the following steps:
(1) pretreatment 1: collecting mixed plastics as a feeding material, wherein the sources of the mixed plastics are common PMMA, PTFE and ABS products in various solid waste streams, cleaning to remove stains, then crushing, and controlling the feeding thickness to be less than or equal to 10mm to finish the sheeting of the feeding material;
(2) and (3) pretreatment 2: finely grinding the laminated mixed plastic in the step (1), and controlling the equivalent diameter to be 3-5 mm by using a particle size sieve to finish feeding fine particles;
(3) plasma etching 1: carrying out plasma positive electrode etching on the mixed plastic after the fine granulation in the step (2) under the atmospheric pressure, wherein plasma is generated in the atmospheric atmosphere by corona discharge, and the unit activation energy generated on the plasma etching surface is controlled to be 9-10 kJ/m in the process2；
(4) A flotation unit 1: adding the mixed plastic particles etched by the plasma in the step (3) into a flotation container, adding tap water as a solution medium, wherein the solid-to-liquid ratio is as follows: m is3Adding a foaming agent, namely pine oil, according to the ratio of (16-25) to 1, operating for 4-6 min under the condition of air aeration of 180-220L/h, and collecting sinking tailing 1 to finish the separation of PMMA;
(5) and (3) pretreatment: further transferring the floating product 1 in the step (4) into a closed container, wherein the solid-liquid ratio is as follows: m is3Adding a mixed solvent of ethanol and tert-butyl alcohol into the mixture according to the ratio of (40-60) to 1, soaking for 25-40 min to complete solubilization of low-molecular-weight oxidation substances and quenching of redundant free radicals generated in the step (4), performing solid-liquid separation after soaking, and naturally drying;
(6) plasma etching 2: feeding the mixed plastic particles air-dried in the step (5) intoPerforming secondary etching on plasma in the closed container, wherein the plasma is generated in an oxygen atmosphere by a radio frequency plasma torch generator, and the unit activation energy generated on the etching surface of the plasma is controlled to be 13-14 kJ/m in the process2；
(7) A flotation unit 2: adding the mixed plastic particles subjected to the secondary plasma etching in the step (6) into a flotation container, adding tap water as a solution medium, wherein the solid-to-liquid ratio is as follows: m is3Adding a foaming agent, namely pine oil, according to the ratio of (16-25) to 1, operating for 2-4 min under the condition of 140-160L/h of air aeration, collecting sinking tailings 2 to finish the separation of PTFE, and collecting floating products 2 to finish the separation of ABS.
Further preferably, the method for separating ternary mixed plastics by flotation through plasma etching enhanced as described above, wherein the mass ratio of PMMA, PTFE and ABS in the feed in the step (1) is (1-3): (1-3): (1-3). Still further preferably, the mass ratio of PMMA, PTFE and ABS in the feeding in the step (1) is (1-3): (1-2): (1-3).
Further preferably, the plasma etching enhances the ternary mixed plastic flotation separation method as described above, wherein the cleaning process in the step (1) is as follows: soaking in tap water containing detergent (preferably cleaning powder), stirring, washing with tap water, and separating solid from liquid.
Further preferably, in the method for performing flotation separation on ternary mixed plastics by plasma etching enhanced as described above, the crushing process in step (1) is coarse crushing, and is performed by using a small crusher, and the coarse crushing is controlled by using a thickness screen to ensure that the minimum size thickness in three dimensions of the coarse crushed material is less than or equal to 10 mm.
Further preferably, the plasma etching enhances the ternary mixed plastic flotation separation method as described above, wherein the fine grinding in step (2) is a ball milling treatment.
Further preferably, the plasma etching enhances the ternary mixed plastic flotation separation method as described above, wherein the corona discharge in the step (3) adopts a corona machine, parameters of a working electrode in the corona machine are 500mm in length, 1mm in width, 1.5mm in spacing, a sinusoidal alternating voltage of 220VAC/50Hz is supplied, the output power is 300W, and the average linear velocity of a feeding roller is 3.78 m/min.
Further preferably, in the method for flotation separation of ternary mixed plastics by plasma etching enhanced flotation, the flotation container in the step (4) is columnar, the diameter-depth ratio is 1:4, and the addition amount of the foaming agent pine oil is 20-30 mg/L.
Further preferably, the method for flotation separation of ternary mixed plastics by plasma etching enhanced flotation separation is as described above, wherein the volume ratio of ethanol to tert-butyl alcohol in the mixed solvent in the step (5) is (2.5-3.5): 1.
Further preferably, the plasma etching enhances the ternary mixed plastic flotation separation method as described above, wherein the operating parameters of the plasma torch in the step (6) are radio frequency 13.56MHz, the parallel electrode distance and the diameter are 110mm and 200mm respectively, and the oxygen serving as the carrier gas is supplied to the gas flow of 10 sccm.
Further preferably, in the method for flotation separation of ternary mixed plastics by plasma etching enhanced flotation, the flotation container in the step (7) is columnar, the diameter-depth ratio is 1:5, and the addition amount of the foaming agent pine oil is 8-12 mg/L.
Compared with the prior art, the method for enhancing the ternary mixed plastic flotation separation by plasma etching has the following advantages and remarkable progress:
(1) the invention provides an effective sorting method for PMMA, PTFE and ABS ternary mixed plastics, which is simple to operate and beneficial to industrial large-scale application.
(2) The method has the advantages of simple flow, relatively mild process, no high-temperature pressurizing link, and high separation safety and efficiency.
(3) The invention can realize the on-line automatic operation in all links by depending on the conveying device, and is convenient to be popularized and applied by combining the existing large-scale flotation equipment.
Drawings
FIG. 1 is a flow diagram of a continuous separation process of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments. It will be understood by those skilled in the art that the following examples are illustrative of the present invention only and should not be taken as limiting the scope of the invention. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
As shown in fig. 1, the process of the method of the present invention comprises seven core process links including pretreatment 1, pretreatment 2, plasma etching 1, flotation unit 1, pretreatment 3, plasma etching 2 and flotation unit 2; the seven process links are sequentially connected in series and can be continuously operated on line; the ternary mixed plastics fed to the pretreatment 1 comprise polymethyl methacrylate (PMMA), Polytetrafluoroethylene (PTFE) and acrylonitrile/butadiene/styrene copolymer (ABS) with different sources and mass ratios; the sinking tailing 1 of the flotation unit 1 is the separated PMMA; the sinking tailing 2 of the flotation unit 2 is the separated PTFE; and the floating product 2 of the flotation unit 2 is the separated ABS.
The feeding composition of the embodiment is ternary mixed plastic of PMMA, PTFE and ABS, the sources of the ternary mixed plastic are automobile, building and electrical fittings, different mass ratios of the PMMA, the PTFE and the ABS are taken as a plurality of groups of feeding materials, and the following separation operation methods are uniformly executed:
(1) pretreatment 1: firstly, soaking, stirring and feeding tap water containing a detergent (cleaning powder) for 10min to remove stains, then re-washing and removing the detergent by using the tap water, performing simple solid-liquid separation by using a centrifugal machine, then crushing in a small crusher, and controlling the minimum three-dimensional size thickness of coarse crushed materials to be less than 10mm by using a thickness sieve to finish feeding sheeting;
(2) and (3) pretreatment 2: finely grinding the laminated mixed plastic in the step (1) by using a ball mill, and controlling the equivalent diameter (more than 90% of the mass) of a fine grinding material to be 3-5 mm by using a particle size sieve to finish fine granulation;
(3) plasma etching 1: carrying out plasma positive electrode etching on the mixed plastic after the fine granulation in the step (2) under the atmospheric pressure, wherein plasma is generated in the atmospheric atmosphere by corona discharge, and the unit activation energy generated on the plasma etching surface is controlled to be 9.5kJ/m in the process2(ii) a Working electrode of corona machine (length, width and distance) 500mm, 1mm, 1.5mm, sineThe alternating voltage is 220VAC/50Hz for power supply, the output power is 300W, and the average linear speed of the feeding roller is 3.78 m/min;
(4) a flotation unit 1: adding the mixed plastic particles etched by the plasma in the step (3) into a columnar flotation container, wherein the diameter-depth ratio (inner diameter: height) of the mixed plastic particles is 1:4, adding tap water as a solution medium, and the solid-liquid ratio (kg: m)3) Controlling the ratio to be 20: 1, adding foaming agent pinitol oil (25mg/L), operating for 5min under the condition of air aeration of 200L/h, and collecting sinking tailing 1 for later use;
(5) and (3) pretreatment: further transferring the floating product 1 in the step (4) into a closed container according to the solid-liquid ratio (kg: m)3) Adding a mixed solvent of EtOH and TBA (volume ratio of 3:1) according to a ratio of 50:1, soaking for 30min to complete solubilization of low-molecular-weight oxidation substances and quenching of redundant free radicals generated in the step (4), then performing solid-liquid separation by using a centrifugal machine, and naturally air-drying;
(6) plasma etching 2: performing secondary plasma etching on the air-dried mixed plastic particles in the step (5) in a closed container, wherein plasma is generated by a radio frequency plasma torch generator in an oxygen atmosphere, and the unit activation energy generated on the plasma etching surface is controlled to be 13.5kJ/m in the process2(ii) a The distance between parallel electrodes of the radio frequency (13.56MHz) plasma torch and the diameter are respectively 110mm and 200 mm; the flow rate of oxygen as carrier gas is about 10 sccm;
(7) a flotation unit 2: adding the mixed plastic particles etched by the plasma in the step (6) into a columnar flotation container, wherein the diameter-depth ratio (inner diameter: height) of the mixed plastic particles is 1:5, adding tap water as a solution medium, and the solid-liquid ratio (kg: m)3) Controlling the ratio to be 20: 1, adding a foaming agent, namely pinitol oil (10mg/L), operating for 3min under the condition of air aeration of 150L/h, and respectively collecting sinking tailing 2 and floating product 2 for later use;
finally, after drying the sinking tails 1, sinking tails 2 and floating products 2 to be used, carefully selecting and distinguishing different components according to the color, texture and reflection factors, wherein the mass of a single plastic is divided by the mass of the corresponding kind of plastic in the feeding material to be used as the recovery rate (in%) and the mass of a single plastic is divided by the mass of the corresponding tails or products to be used as the purity (in%), and the results are shown in table 1.
TABLE 1 comparison of the recovery and purity of ternary mixed plastics of different mass ratios after separation by the process of the invention
As can be seen from Table 1, the recovery rate of PMMA separated by the embodiment of the invention is more than 90%, the purity of PMMA is more than 85%, the recovery rate and purity of PTFE separated are more than 77%, the recovery rate and purity of ABS separated are more than 73%, and the PMMA has better adaptability to different feed composition mass ratios. Therefore, the method has high separation stability and wide application range.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (9)
1. A method for enhancing ternary mixed plastic flotation separation by plasma etching is characterized by comprising the following steps:
(1) pretreatment 1: collecting mixed plastics as feeding materials, wherein the mixed plastics comprise PMMA, PTFE and ABS from different sources, cleaning to remove stains, then crushing, and controlling the feeding thickness to be less than or equal to 10mm to finish the sheeting of the feeding materials;
(2) and (3) pretreatment 2: finely grinding the laminated mixed plastic in the step (1), and controlling the equivalent diameter to be 3-5 mm by using a particle size sieve to finish feeding fine particles;
(3) plasma etching 1: carrying out plasma positive electrode etching on the mixed plastic after the fine granulation in the step (2) under the atmospheric pressure, wherein plasma is generated in the atmospheric atmosphere by corona discharge, and the unit activation energy generated on the plasma etching surface is controlled to be 9-10 kJ/m in the process2；
(4) A flotation unit 1: adding the mixed plastic particles etched by the plasma in the step (3) into a flotation container, and addingTap water is used as a solution medium, and the solid-liquid ratio is as follows: m is3Adding a foaming agent, namely pine oil, according to the ratio of (16-25) to 1, operating for 4-6 min under the condition of air aeration of 180-220L/h, and collecting sinking tailing 1 to finish the separation of PMMA;
(5) and (3) pretreatment: further transferring the floating product 1 in the step (4) into a closed container, wherein the solid-liquid ratio is as follows: m is3Adding a mixed solvent of ethanol and tert-butyl alcohol into the mixture according to the ratio of (40-60) to 1, soaking for 25-40 min, separating solid from liquid after soaking, and naturally drying;
(6) plasma etching 2: performing secondary plasma etching on the air-dried mixed plastic particles in the step (5) in a closed container, wherein plasma is generated in an oxygen atmosphere by a radio frequency plasma torch generator, and the unit activation energy generated on the plasma etching surface is controlled to be 13-14 kJ/m in the process2；
(7) A flotation unit 2: adding the mixed plastic particles subjected to the secondary plasma etching in the step (6) into a flotation container, adding tap water as a solution medium, wherein the solid-to-liquid ratio is as follows: m is3Adding a foaming agent, namely pine oil, according to the ratio of (16-25) to 1, operating for 2-4 min under the condition of 140-160L/h of air aeration, collecting sinking tailings 2 to finish the separation of PTFE, and collecting floating products 2 to finish the separation of ABS.
2. The method for plasma etching enhanced ternary mixed plastic flotation separation as claimed in claim 1, wherein the cleaning process in step (1) is as follows: soaking in tap water containing detergent while stirring, re-washing with tap water to remove detergent, and separating solid from liquid.
3. The method for flotation separation of ternary mixed plastics through plasma etching enhancement according to claim 1, wherein the crushing process in the step (1) is coarse crushing, and the coarse crushing is performed by a small crusher, and the coarse crushing is controlled by a thickness screen to ensure that the thickness of the three-dimensional minimum size of the coarse crushed material is less than or equal to 10 mm.
4. The method for flotation separation of ternary mixed plastics through plasma etching enhancement according to claim 1, wherein the fine grinding in the step (2) is ball milling treatment.
5. The method for flotation separation of ternary mixed plastics through plasma etching enhancement according to claim 1, characterized in that corona discharge in the step (3) adopts a corona machine, parameters of a working electrode in the corona machine are 500mm in length, 1mm in width and 1.5mm in distance, a sinusoidal alternating voltage is 220VAC/50Hz for power supply, the output power is 300W, and the average linear speed of a feeding roller is 3.78 m/min.
6. The method for flotation separation of ternary mixed plastics through plasma etching enhancement according to claim 1, wherein the flotation container in the step (4) is columnar, the diameter-depth ratio is 1:4, and the addition amount of the foaming agent pine oil is 20-30 mg/L.
7. The method for separating ternary mixed plastics by flotation through plasma etching enhancement according to claim 1, wherein the volume ratio of ethanol to tertiary butanol in the mixed solvent in the step (5) is (2.5-3.5) to 1.
8. The method for flotation separation of ternary mixed plastics through plasma etching enhancement according to claim 1, wherein the working parameters of the plasma torch in the step (6) are radio frequency 13.56MHz, the parallel electrode distance and the diameter are respectively 110mm and 200mm, and the gas supply flow rate of oxygen as the carrier gas is 10 sccm.
9. The method for flotation separation of ternary mixed plastics through plasma etching enhancement according to claim 1, wherein the flotation container in the step (7) is columnar, the diameter-depth ratio is 1:5, and the addition amount of the foaming agent pine oil is 8-12 mg/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113618966A (en) * | 2021-08-30 | 2021-11-09 | 陕西师范大学 | Method for separating micro plastic and biochar |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5566832A (en) * | 1994-08-05 | 1996-10-22 | Daimler-Benz Ag | Method for sorting plastics from a particle mixture composed of different plastics |
| CN106881782A (en) * | 2017-02-21 | 2017-06-23 | 长安大学 | A kind of method of FLOTATION SEPARATION high density polyethylene (HDPE), polypropylene and polyethylene terephthalate in mixed plastic from multicomponent |
| CN111873246A (en) * | 2020-07-21 | 2020-11-03 | 长安大学 | Flotation separation method for multi-component waste plastic |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5566832A (en) * | 1994-08-05 | 1996-10-22 | Daimler-Benz Ag | Method for sorting plastics from a particle mixture composed of different plastics |
| CN106881782A (en) * | 2017-02-21 | 2017-06-23 | 长安大学 | A kind of method of FLOTATION SEPARATION high density polyethylene (HDPE), polypropylene and polyethylene terephthalate in mixed plastic from multicomponent |
| CN111873246A (en) * | 2020-07-21 | 2020-11-03 | 长安大学 | Flotation separation method for multi-component waste plastic |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113618966A (en) * | 2021-08-30 | 2021-11-09 | 陕西师范大学 | Method for separating micro plastic and biochar |
| CN113618966B (en) * | 2021-08-30 | 2022-12-27 | 陕西师范大学 | Method for separating micro plastic and biochar |
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