CN111777053B - Polyvinyl chloride waste treatment method - Google Patents
Polyvinyl chloride waste treatment method Download PDFInfo
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- CN111777053B CN111777053B CN202010593429.1A CN202010593429A CN111777053B CN 111777053 B CN111777053 B CN 111777053B CN 202010593429 A CN202010593429 A CN 202010593429A CN 111777053 B CN111777053 B CN 111777053B
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- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1456—Removing acid components
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/68—Halogens or halogen compounds
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Abstract
The invention relates to a treatment method of polyvinyl chloride waste, which comprises the following steps: mixing polyvinyl chloride waste with a dechlorinating agent, sealing, heating and carrying out pyrolysis treatment to obtain a gas-phase product and a solid-phase product, wherein the gas-phase product is high-calorific-value pyrolysis gas, and the solid-phase product is soaked in acid liquor and washed with water to obtain a chloride solution and a carbon material. Compared with the prior art, the method has the advantages of simple treatment process, high production efficiency, high product value and no secondary pollution, and can simultaneously realize the harmless treatment and resource utilization of the polyvinyl chloride.
Description
Technical Field
The invention belongs to the technical field of waste treatment, and particularly relates to a treatment method of polyvinyl chloride waste.
Background
Polyvinyl chloride (PVC) is one of five general-purpose plastics, and is widely used in the fields of construction, packaging, electronic devices, automobile industry, and the like because of low price and excellent performance. According to statistics, the consumption of PVC in China in 2017 is 1780 ten thousand tons, and accounts for 16.24% of the total amount of resin (annual book of plastic industry in China, 2018). A large amount of PVC waste is also generated while mass-producing and using PVC. It is statistically estimated that in 2001-2015, the cumulative production of PVC waste is about 5480 ten thousand tons (Liu et al, Resources, consiservation & Recycling,154(2020) 104584). At present, the treatment and utilization modes of PVC are mainly landfill, incineration and pyrolysis, but PVC has the characteristic of difficult biodegradation, and can exist in landfill for hundreds of years; meanwhile, PVC contains a plasticizer, a stabilizer and the like, and toxic leachate is generated after leaching; PVC also contains a large amount of Cl elements, acid gas can be generated in the incineration process to corrode equipment, and meanwhile, the Cl elements can promote the chlorination migration of heavy metals and the generation of dioxin; the pyrolysis product of PVC has complex components and high tar content, is easy to be polluted by Cl, and has the defects of poor product quality, low value and lack of absorption channels.
The carbon material prepared by taking PVC as a raw material can solve the problem of PVC waste pollution and realize high-value utilization of the PVC waste, so the research direction is concerned. For example, the Chinese patent of invention "a method for synthesizing polyvinyl chloride-based carbon beads" (publication number: CN107381532A) prepares PVC into carbon beads through four steps of organic solvent dissolution, alkali liquor treatment dechlorination, heating crosslinking curing, high-temperature carbonization and the like. The document "Converting polyvinyl chloride foam procedure to carbon Materials via a high-performance purifying for high-performance superparameter" (Chang et al, ACS Applied Energy Materials,1(2018) 5685-; subsequently, the obtained product is dried and carbonized at high temperature to obtain a carbon material. These methods are complicated, time-consuming and labor-intensive, and require the consumption of large amounts of organic solvents and alkaline solutions. The Chinese invention patent 'a resource treatment method of organic waste' (publication number: CN110903836A) can convert various organic wastes into carbon materials by a closed heating method, but the method has no dechlorination operation, and the direct treatment of PVC waste has the problems of equipment corrosion and pollutant discharge and has potential environmental risks. Therefore, there is a need to develop a convenient, green, and economical PVC carbonization method.
Disclosure of Invention
The invention aims to provide a method for treating polyvinyl chloride waste for realizing green and efficient treatment and resource utilization of polyvinyl chloride, so as to realize high-value resource recycling of polyvinyl chloride waste, solve the problems of equipment corrosion and environmental pollution caused by polyvinyl chloride waste and generate products with high added values.
The purpose of the invention is realized by the following technical scheme:
a method for treating polyvinyl chloride waste specifically comprises the following steps: mixing polyvinyl chloride waste with a dechlorinating agent, sealing, heating and carrying out pyrolysis treatment to obtain a gas-phase product and a solid-phase product, soaking the solid-phase product in acid liquor, washing with water to obtain a chloride solution and a carbon material, drying the carbon material and using the carbon material, wherein the acid liquor is diluted acid. In the invention, the reaction is carried out in a reaction kettle, and the closed condition means that substances generated by the reaction cannot leave the reaction kettle, air or nitrogen can be filled in the reaction kettle before the closed condition, and the carbon material is spherical carbon, blocky carbon or flaky carbon with the particle size of 2-8 mu m.
Further, the polyvinyl chloride waste comprises a mixture of one or more of polyvinyl chloride resin or polyvinyl chloride plastic waste.
Further, the dechlorinating agent is a metal oxide or a metal hydroxide, and has the capacity of reacting with hydrogen chloride or polyvinyl chloride to generate soluble chloride salt.
Further, the dechlorination agent is selected from one or more of ZnO, KOH, CaO or NaOH.
Further, the mass ratio of the dechlorinating agent to the polyvinyl chloride waste is more than
Wherein n, M and cClRespectively represents the valence state of metal in the dechlorinating agent, the relative molecular mass of the dechlorinating agent and the mass percentage content of Cl element in the polyvinyl chloride waste. So as to ensure that the chlorine element in the polyvinyl chloride waste is completely converted into chlorine salt.
Further, the heating rate is 5-10 ℃/min.
Further, the pyrolysis temperature is 600-700 ℃, and the pyrolysis time is 20-40min, preferably 30 min.
Further, the pyrolysis treatment is carried out in a stainless steel reaction kettle, the highest working temperature of the reaction kettle is 800 ℃, and the maximum pressure resistance of the reaction kettle is 5 MPa.
Further, hydrochloric acid is used for soaking until the amount of the solid phase product is not changed any more (namely, the chlorine salt is dissolved in the hydrochloric acid, and the solid phase product in a solid state is all carbon material).
Further, the molar concentration of the hydrochloric acid is 1-6 mol/L.
Further, the gas phase product comprises one or more of methane, hydrogen, or carbon dioxide. When the gas phase product contains carbon dioxide, the residual gas phase product has high heat value after the carbon dioxide is removed, and can be used as synthetic natural gas for storage and transportation or directly combusted to supply energy to the system.
The invention adopts a one-pot method to treat the polyvinyl chloride waste, and in the reaction process, the polyvinyl chloride is decomposed at the temperature of 200 ℃ and 400 ℃ to release hydrogen chloride. The hydrogen chloride is then absorbed by the metal oxide or metal hydroxide and converted to the chloride salt. Certain metal oxides or metal hydroxides (e.g., ZnO) can be reacted directly with polyvinyl chloride to produce chloride salts and polyenes. The polyene obtained by dechlorinating the polyvinyl chloride is further pyrolyzed, and the pyrolysis product is converted into a carbon material and pyrolysis gas through cracking, aromatizing and polycondensation reactions.
Compared with the prior art, the invention has the following advantages:
(1) the products are soluble chlorine salt, carbon material and pyrolysis gas, and the polyvinyl chloride waste is recycled. The chloride salt can be used as a raw material for metallurgy or chlor-alkali industry; the carbon material can be widely used in the industrial fields of battery, rubber, pollutant purification and the like; the pyrolysis gas can be directly combusted to supply energy to the reaction system.
(2) The reaction of metal oxide or metal hydroxide with polyvinyl chloride can reduce the generation of hydrogen chloride or absorb the hydrogen chloride and other acidic gases released by polyvinyl chloride, thus avoiding the problems of reactor corrosion and atmospheric pollution.
(3) Organic solvent and alkali liquor are not needed in the reaction process, so that the method is more green and economical.
(4) The one-pot method realizes dechlorination, carbonization and gasification of the polyvinyl chloride, has simple and convenient process, shortens the reaction process and improves the production efficiency.
Drawings
FIG. 1 is the XRD spectrum of the solid phase product obtained in example 1;
FIG. 2 is an XRD spectrum of the carbon material obtained in example 1;
FIG. 3 is an SEM photograph of the carbon material obtained in example 1;
FIG. 4 is the XRD spectrum of the solid phase product obtained in example 2;
FIG. 5 is an XRD spectrum of the carbon material obtained in example 2;
FIG. 6 is an SEM photograph of the carbon material obtained in example 2;
FIG. 7 shows N in the carbon material obtained in example 22An adsorption isotherm diagram;
FIG. 8 is an XRD spectrum of the solid phase product obtained in comparative example 2.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
A treatment method of polyvinyl chloride waste is disclosed, wherein the polyvinyl chloride waste is polyvinyl chloride resin (the mass percentage content of Cl element in the polyvinyl chloride resin is 56.8%), and specifically comprises the following steps: ZnO and polyvinyl chloride resin are mixed according to the mass ratio of 0.9:1, and then added into a reactor (the reactor is a stainless steel reaction kettle, the maximum working temperature of the reaction kettle is 800 ℃, the maximum pressure resistance is 5MPa, the same below). After the reactor was closed, the temperature was raised to 700 ℃ at a rate of 5 ℃/min and held for 30 min. After cooling to room temperature, 7.71 wt.% of the gas phase product and 92.29 wt.% of the solid phase product were obtained. The XRD spectrum of the solid phase product is shown in figure 1, and it can be seen that the solid phase product is mainly ZnCl2And ZnOCl2·2H2O, i.e. conversion of Cl in polyvinyl chloride to ZnCl2And ZnOCl2·2H2And O. Soaking the solid phase product in dilute hydrochloric acid of 3mol/L (the same applies below) and distilled water, and separating to obtain ZnCl2Solution and carbon material. The XRD spectrum of the carbon material is shown in fig. 2, and it can be seen that only the diffraction peaks of amorphous graphite, specifically, the (002) diffraction peak at 26 ° and the (100) diffraction peak at 43 °, are contained in the XRD spectrum, and no other impurities are contained therein. SEM photographs of the carbon material are shown in FIG. 3, in which the carbon material is mainly spherical carbon of 2 to 8 μm and a small amount of bulk carbon. The gas phase product contains 59.40 vol.% of methane, 22.47 vol.% of hydrogen, 15.96 vol.% of carbon dioxide and a small amount of other gases such as ethylene and the like through gas chromatographic analysis, and the high calorific value of combustible gas components after the carbon dioxide is removed from the gas phase product is 30.11MJ/m3And the quality requirement of the natural gas of the second type is approached.
Example 2
A process for treating the waste polyvinyl chloride includes such steps as dechlorinating agent (KOH) whose mass ratio to polyvinyl chloride is 1.3:1, polymerizingThe kind of vinyl chloride waste and the operation procedure were the same as in example 1. 8.26 wt.% of gas phase product and 91.74 wt.% of solid phase product were finally obtained. The XRD pattern of the solid phase product is shown in FIG. 4, and it can be seen that the solid phase product is mainly KCl and K2CO3I.e. the Cl in the polyvinyl chloride is converted to KCl. K in the product2CO3Resulting from the activation reaction of excess KOH with the carbon material, the reaction equation is:
6KOH+2C→2K+3H2+2K2CO3
and soaking the solid phase product in dilute hydrochloric acid with the molar concentration of 5mol/L, washing the solid phase product with distilled water, and separating to obtain a KCl solution and a carbon material. The XRD spectrum of the carbon material is shown in fig. 5, and it can be seen that only the diffraction peaks of amorphous graphite, specifically, the (002) diffraction peak at 26 ° and the (100) diffraction peak at 43 °, are contained in the XRD spectrum, and no other impurities are contained therein. As shown in fig. 6, the SEM photograph of the carbon material showed that the carbon material was mainly flaky carbon and a pore structure was observed on the surface of the carbon material. Obtaining N at-196 ℃ by testing with a physical adsorption instrument2The adsorption isotherm diagram (shown in FIG. 7) shows that the specific surface area of the carbon material is as high as 1922m through the analysis of a BET method2A/g, much higher than commercial activated carbon (about 1000 m)2In terms of/g). The gas product contains 75.23 vol.% methane, 23.07 vol.% hydrogen and a small amount of other gases such as ethylene, and the high calorific value of the gas product is 31.88MJ/m3And the quality requirement of the second-class natural gas is met.
Example 3
A treatment method of polyvinyl chloride waste is the same as that of example 1 except that polyvinyl chloride waste is polyvinyl chloride plastic waste, a dechlorinating agent is CaO, the heating rate is 8 ℃/min, the pyrolysis temperature is 600 ℃, the pyrolysis time is 40min, and the molar concentration of hydrochloric acid is 1mol/L, and CaCl can be finally obtained2Solution, carbon material and high value pyrolysis gas.
Example 4
A treatment method of polyvinyl chloride waste is the same as that in example 1 except that polyvinyl chloride waste is polyvinyl chloride plastic waste, a dechlorinating agent is NaOH, the heating rate is 10 ℃/min, the pyrolysis temperature is 670 ℃, the pyrolysis time is 20min, and the molar concentration of hydrochloric acid is 6mol/L, and a NaCl solution, a carbon material and high-value pyrolysis gas can be finally obtained.
Comparative example 1
A method for treating non-sealed polyvinyl chloride waste was the same as in example 1, except that in this example, the reaction was carried out in an open autoclave. The final solid phase product yield obtained was only 28.59 wt.%, the carbon material yield was very low. Meanwhile, the volatile pyrolysis product is mainly liquid-phase hydrocarbon with complex components and has low value.
Comparative example 2
The waste polyvinyl chloride is treated by a step-by-step dechlorination-carbonization method, in the embodiment, the polyvinyl chloride is heated to 260 ℃ and kept for 30min, and thermal dechlorination is carried out. Subsequently, the dechlorinated product was charged into the reactor, and heat-treated in a closed state under the same conditions as in example 1. The XRD spectrum of the finally obtained solid phase product is shown in FIG. 8, and it can be seen that part of FeCl is present in the solid phase product2·4H2O, indicating that the process fails to completely dechlorinate, 0.2 to 1 wt.% of chlorine remains in the polyvinyl chloride waste after thermal dechlorination. In the subsequent pyrolysis process, the residual chlorine is released in the form of acid gas, which corrodes the stainless steel reaction kettle.
Comparing examples 1 and 2 with comparative examples 1 and 2, it can be seen that the invention maintains the temperature of 600-700 ℃ for 30min by adding dechlorinating agent (especially ZnO and KOH), pyrolyzes polyvinyl chloride waste, and then separates to obtain high-value carbon material, chlorine salt solution and pyrolysis gas, the treatment process is simple, the production efficiency is high, the product value is high, no secondary pollution is caused, and the harmless treatment and resource utilization of polyvinyl chloride can be realized at the same time.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (9)
1. A treatment method of polyvinyl chloride waste is characterized by comprising the following steps: mixing polyvinyl chloride waste with a dechlorinating agent, then sealing and heating for pyrolysis treatment to obtain a gas-phase product and a solid-phase product, and soaking and washing the solid-phase product with acid liquor to obtain a chloride solution and a carbon material;
the dechlorinating agent is metal oxide or metal hydroxide;
the pyrolysis temperature is 600-700 ℃;
the pyrolysis treatment is carried out in a stainless steel reaction kettle.
2. The method of claim 1, wherein the polyvinyl chloride waste comprises one or more of polyvinyl chloride resin or polyvinyl chloride plastic waste.
3. The method of claim 1, wherein the mass ratio of the dechlorinating agent to the polyvinyl chloride waste is greater than or equal to
Wherein n, M and cClRespectively represents the valence state of metal in the dechlorinating agent, the relative molecular mass of the dechlorinating agent and the mass percentage content of Cl element in the polyvinyl chloride waste.
4. The method of claim 1, wherein the heating rate is 5-10 ℃/min.
5. The method of claim 1, wherein the pyrolysis time is 20-40 min.
6. The method of claim 1, wherein the maximum operating temperature of the reaction vessel is 800 ℃ and the maximum pressure resistance is 5 MPa.
7. The method for treating polyvinyl chloride waste according to claim 1, wherein the soaking is performed using hydrochloric acid.
8. The method for treating polyvinyl chloride waste according to claim 7, wherein the hydrochloric acid has a molar concentration of 1 to 6 mol/L.
9. The method of claim 1, wherein the gas phase product comprises one or more of methane, hydrogen, or carbon dioxide.
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| CN104893147A (en) * | 2015-05-27 | 2015-09-09 | 福建工程学院 | Method for safely dechlorinating waste polyvinyl chloride and preparing high-purity ammonia chloride |
| CN106349500A (en) * | 2016-09-23 | 2017-01-25 | 苏州大学 | Dechlorination method for chlorine-containing plastic |
| CN106433724A (en) * | 2016-08-29 | 2017-02-22 | 石晓岩 | Continuous waste plastic cyclic cracking system and method |
| CN107381532A (en) * | 2016-05-17 | 2017-11-24 | 中国科学院大连化学物理研究所 | A kind of synthetic method of polyvinyl chloride-based charcoal bead |
| CN111112290A (en) * | 2019-12-20 | 2020-05-08 | 浙江巨化技术中心有限公司 | Dechlorination method for chlorinated hydrocarbon waste |
| CN111217353A (en) * | 2018-11-27 | 2020-06-02 | 中国科学院大连化学物理研究所 | Preparation method of polyvinyl chloride-based carbon powder |
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| UA109872C2 (en) * | 2015-06-22 | 2015-10-12 | DEVICES FOR THERMAL DESTRUCTION OF WASTES OF POLYETHYLENE AND POLYPROPYLENE |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104893147A (en) * | 2015-05-27 | 2015-09-09 | 福建工程学院 | Method for safely dechlorinating waste polyvinyl chloride and preparing high-purity ammonia chloride |
| CN107381532A (en) * | 2016-05-17 | 2017-11-24 | 中国科学院大连化学物理研究所 | A kind of synthetic method of polyvinyl chloride-based charcoal bead |
| CN106433724A (en) * | 2016-08-29 | 2017-02-22 | 石晓岩 | Continuous waste plastic cyclic cracking system and method |
| CN106349500A (en) * | 2016-09-23 | 2017-01-25 | 苏州大学 | Dechlorination method for chlorine-containing plastic |
| CN111217353A (en) * | 2018-11-27 | 2020-06-02 | 中国科学院大连化学物理研究所 | Preparation method of polyvinyl chloride-based carbon powder |
| CN111112290A (en) * | 2019-12-20 | 2020-05-08 | 浙江巨化技术中心有限公司 | Dechlorination method for chlorinated hydrocarbon waste |
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