CN114408920A - Solid waste recycling method for preparing aperture-adjustable activated carbon by using waste membrane material and product thereof - Google Patents
Solid waste recycling method for preparing aperture-adjustable activated carbon by using waste membrane material and product thereof Download PDFInfo
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Abstract
The invention provides a solid waste recycling method for preparing active carbon with adjustable pore diameter by using waste membrane materials and a product thereof, wherein the method comprises the following steps: (1) mixing the waste membrane material with an activating agent, and drying to obtain a mixture; (2) and carrying out pyrolysis carbonization on the mixture under the protection of inert gas to obtain the activated carbon material. The invention creatively provides a method for resource utilization of waste membrane materials, an activated carbon adsorption material with high specific surface area, developed pores and adjustable pore diameter can be prepared by one-step activation and high-temperature carbonization, and the prepared activated carbon material has excellent adsorption performance in the aspect of removing organic pollutants. The invention utilizes the waste membrane material as resources, effectively reduces the resource waste and reduces the treatment cost of the waste membrane as solid waste. And the preparation method is easy to operate, easy to realize large-scale industrial production and good in application prospect.
Description
Technical Field
The invention belongs to the field of solid waste recycling, and relates to a solid waste recycling method for preparing active carbon with adjustable pore diameter by using waste membrane materials and a product thereof.
Background
The membrane materials represented by the hollow fiber membrane and the plate-type membrane have the advantages of large filtration area, relatively low manufacturing cost and the like, and become the membrane products with the largest scale and the highest production value in the field of membrane separation. PVDF, PP and other organic material membrane materials are widely applied in the field of environmental protection, particularly water treatment. However, due to the unavoidable nature of membrane pollution, the membrane module is out of service and becomes solid waste after 3-5 years of use in the water treatment process. Therefore, the problems of a large amount of solid wastes generated by decommissioning the membrane module of tens of millions of square meters every year and great resource waste are urgently solved.
The activated carbon is a general name of carbon materials which are prepared by pyrolyzing and activating carbon-containing raw materials such as wood, coal, petroleum coke and the like, have developed pore structures, larger specific surface areas, abundant surface chemical groups and stronger specific adsorption capacity. Due to its good adsorption performance, activated carbon has been widely used in the fields of wastewater treatment, catalysis or supported catalyst, clinical medicine (blood purification, cancer treatment, etc.), flue gas treatment, etc.
The PVDF and other organic polymer membrane materials have polymer skeletons containing abundant carbon elements and can be used as precursors of active carbon materials. Therefore, if the waste hollow fiber membrane can be prepared into the activated carbon material with additional value, the activated carbon material has important application value and conforms to the national green and sustainable development guiding idea.
However, currently, activated carbon in the prior art is generally made of raw materials such as wood, coal, petroleum coke, and the like, and it is unknown whether the assumption of preparing activated carbon from waste membrane materials such as PVDF is feasible and how to prepare the activated carbon is specific, so how to provide a waste recycling method for preparing waste hollow fiber membranes into activated carbon materials with added values becomes a problem to be solved in the field.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a solid waste recycling method for preparing active carbon with adjustable pore diameter by using waste membrane materials and a product thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a solid waste recycling method for preparing activated carbon with adjustable pore diameter by using waste membrane materials, which comprises the following steps:
(1) mixing the waste membrane material with an activating agent, and drying to obtain a mixture;
(2) and carrying out pyrolysis carbonization on the mixture under the protection of inert gas to obtain the activated carbon material.
Preferably, the waste film material includes any one of polyvinylidene fluoride (PVDF), polyethylene terephthalate (PET), or polypropylene (PP), or a combination of at least two thereof. Examples of the combination of at least two of them include a combination of polyvinylidene fluoride and polyethylene terephthalate, a combination of polyethylene terephthalate and polypropylene, and a combination of polyvinylidene fluoride and polypropylene, and any other combination may be used.
Preferably, the step (1) further comprises cleaning and drying the waste membrane material before mixing.
Preferably, the solvent used for the washing comprises absolute ethanol and/or water.
Preferably, the cleaning comprises mixing the waste membrane material with absolute ethyl alcohol, and after cleaning, mixing with water again for cleaning.
Preferably, the activating agent in step (1) comprises any one or a combination of at least two of potassium hydroxide, sodium hydroxide, ferric chloride or zinc chloride. The combination of at least two of them may be, for example, a combination of potassium hydroxide and sodium hydroxide, a combination of sodium hydroxide and ferric chloride, a combination of ferric chloride and zinc chloride, or the like, and any other combination may be used.
Preferably, the mass ratio of the waste membrane material to the activating agent in the step (1) is 1 (0.5-4).
Specific values in (0.5-4) are, for example, 0.5, 0.7, 1, 1.2, 1.5, 1.7, 2, 2.2, 2.5, 2.7, 3, 3.2, 3.5, 3.7, 4, etc.
Preferably, the mixing in step (1) is carried out at 40-120 ℃, such as 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 105 ℃, 110 ℃, 115 ℃, 120 ℃ and the like, and the mixing time is 8-24h, such as 8h, 10h, 12h, 14h, 16h, 18h, 20h, 22h, 24h and the like.
Preferably, the inert gas of step (2) comprises nitrogen or argon.
Preferably, the temperature of the pyrolysis carbonization in the step (2) is 600-.
Preferably, the pyrolytic carbonization in step (2) comprises temperature programming at a rate of 2-5 deg.C/min, such as 2 deg.C/min, 2.5 deg.C/min, 3 deg.C/min, 3.5 deg.C/min, 4 deg.C/min, 4.5 deg.C/min, 5 deg.C/min, etc.
Preferably, the step (2) further comprises a step (3) after the pyrolysis carbonization: and crushing, washing and drying the material subjected to pyrolysis carbonization.
Preferably, the means of comminution comprises grinding.
Preferably, the washing comprises acid washing and water washing.
Preferably, the detergent used in the acid washing comprises 0.1-1mol/L of acid solution.
Specific values of the above-mentioned 0.1 to 1mol/L are, for example, 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, 0.7mol/L, 0.8mol/L, 0.9mol/L, 1mol/L and the like.
Preferably, the acid includes any one of hydrochloric acid, sulfuric acid or nitric acid or a combination of at least two of the hydrochloric acid and the sulfuric acid, the sulfuric acid and the nitric acid, the hydrochloric acid and the nitric acid, and the like, and any other combination can be used.
Preferably, the drying of step (3) is carried out at 40-80 ℃, such as 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃ and the like, and the drying time is longer than 10h, such as 10h, 12h, 14h, 16h, 18h, 20h, 24h, 30h, 36h, 40h and the like.
In a second aspect, the invention provides an activated carbon material, which is prepared by the solid waste recycling method for preparing the activated carbon with adjustable pore diameter by using the waste membrane material according to the first aspect.
The recitation of numerical ranges herein includes not only the above-recited values, but also any values between any of the above-recited numerical ranges not recited, and for brevity and clarity, is not intended to be exhaustive of the specific values encompassed within the range.
Compared with the prior art, the invention has the following beneficial effects:
the invention creatively provides a method for resource utilization of waste membrane materials, which can prepare an activated carbon adsorption material with high specific surface area and developed and adjustable aperture by one-step activation and high-temperature carbonization of alkali solution or metal salt (the waste membrane reacts with an activating agent in the high-temperature carbonization process and simultaneously completes activation, namely carbonization and activation are simultaneously carried out and completed by one step). The prepared activated carbon material has excellent adsorption performance in the aspect of removing organic pollutants. The invention utilizes the waste membrane material as resources, effectively reduces the resource waste and reduces the treatment cost of the waste membrane as solid waste. And the preparation method is easy to operate, easy to realize large-scale industrial production and good in application prospect.
In the method, the waste film and the activating agent are mixed and dried in the first step, and the aim is to fully and uniformly distribute the activating agent on the surface and pore passages of the waste film. And a second step of pyrolysis carbonization, wherein in the high-temperature carbonization process, the waste film reacts with an activating agent and is activated simultaneously. The conventional activated carbon preparation method generally includes secondary activation, i.e., firstly carbonizing the raw material at a high temperature, and then physically or chemically activating the raw material again at a high temperature. The method is a one-step activation method, and the waste membrane material and the activating agent are fully mixed and impregnated, and then are subjected to one-step high-temperature activation to obtain the activated carbon, so that a secondary high-temperature treatment process is avoided. In addition, the raw materials for preparing the conventional activated carbon are generally shells, woods, coals and the like, while the waste membrane materials belong to polymers, the yield of the activated carbon prepared by the method of the invention reaches more than 20 percent, and if the activated carbon is prepared according to the conventional steps of pyrolysis and activation, the yield is lower (lower than 15 percent).
In the method, the active carbon materials with different pore structures can be prepared by selecting waste membranes with different materials and different types of activating agents, so that the preparation of the active carbon with adjustable pore diameters is realized, and the prepared active carbon material has high specific surface area and strong adsorption capacity, and can be used as an adsorbent to be applied to the fields of water treatment and the like again to realize the high-efficiency removal of organic pollutants. The waste recycling method for preparing the activated carbon material with the added value by using the waste membrane material conforms to the national green and sustainable development guiding idea and has important application value.
Drawings
FIG. 1a is a scanning electron micrograph of the activated carbon prepared in example 1.
FIG. 1b is a scanning electron micrograph of the activated carbon prepared in example 2.
Fig. 2a is a nitrogen adsorption-desorption curve of activated carbons with different pore size characteristics prepared in example 1 and example 2.
FIG. 2b is a graph of pore size distribution for activated carbons with different pore size characteristics prepared in examples 1 and 2.
FIG. 3 is a graph showing the results of adsorption removal of methylene blue by the activated carbon prepared in example 1 and example 2.
FIG. 4a is a scanning electron micrograph of the activated carbon prepared in example 3.
FIG. 4b is a scanning electron micrograph of the activated carbon prepared in example 4.
FIG. 4c is a scanning electron micrograph of the activated carbon prepared in example 5.
Fig. 5a is a nitrogen adsorption-desorption curve of activated carbons having different pore size characteristics prepared in example 3, example 4 and example 5.
Fig. 5b is a graph of pore size distribution for activated carbons with different pore size characteristics prepared in example 3, example 4, and example 5.
FIG. 6 is a graph showing the results of toluene adsorption removal by the activated carbon prepared in example 3, example 4 and example 5.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention. The waste membrane made of the single PVDF material related to the following embodiment is an MBR flat membrane of a sewage treatment plant; the hollow fiber membrane according to the following examples, which contains both PVDF and PET, is a hollow fiber membrane used in a deep treatment unit of a sewage treatment plant.
Example 1
The embodiment provides a solid waste recycling method for preparing active carbon with adjustable pore diameter by using waste membrane materials, which comprises the following steps:
(1) crushing a waste film made of a single PVDF material into small sections, stirring in absolute ethyl alcohol and deionized water, ultrasonically cleaning, and then drying;
(2) 50 ml of 10 wt% potassium hydroxide solution is prepared as an activating agent, 5g of dried waste membrane is weighed and put into the activating agent, the waste membrane is soaked for 10 hours at the temperature of 80 ℃, and then the waste membrane is dried for 12 hours at the same temperature, and the mass ratio of the waste membrane to the solute of the activating agent is 1: 1.
(3) And (3) placing the waste film which is impregnated by the activating agent and dried into a tubular furnace, heating to 800 ℃ at a heating rate of 3.5 ℃/min under the protection of argon, preserving heat for 2 hours, and performing high-temperature pyrolysis carbonization.
(4) And grinding the pyrolysis carbonization material, soaking and washing the material by using 0.1mol/L hydrochloric acid solution, washing the material to be neutral by using deionized water, and performing vacuum drying at the temperature of 60 ℃ for 12 hours to finally obtain the activated carbon.
Example 2
The present example provides a method for recycling solid waste by using waste membrane materials to prepare activated carbon with controllable pore size, which is different from example 1 only in that "waste membrane made of single PVDF material" is replaced with "hollow fiber membrane containing both PVDF and PET with equal quality", and the other conditions refer to example 1.
Example 3
The embodiment provides a solid waste recycling method for preparing active carbon with adjustable pore diameter by using waste membrane materials, which comprises the following steps:
(1) crushing the waste hollow fiber membrane containing PVDF and PET into small sections, stirring in absolute ethyl alcohol and deionized water, ultrasonically cleaning, and drying;
(2) 50 ml of 10 wt% sodium hydroxide solution is prepared as an activating agent, 5g of dried waste membrane is weighed and put into the activating agent, the waste membrane is soaked for 10 hours at the temperature of 80 ℃, and then the waste membrane is dried for 12 hours at the same temperature, and the mass ratio of the waste membrane to the solute of the activating agent is 1: 1.
(3) And (3) placing the waste film which is impregnated by the activating agent and dried into a tubular furnace, heating to 800 ℃ at a heating rate of 3.5 ℃/min under the protection of argon, preserving heat for 2 hours, and performing high-temperature pyrolysis carbonization.
(4) And grinding the pyrolysis carbonization material, soaking and washing the material by using 0.1mol/L hydrochloric acid solution, washing the material to be neutral by using deionized water, and performing vacuum drying at the temperature of 60 ℃ for 12 hours to finally obtain the activated carbon.
Example 4
The embodiment provides a solid waste recycling method for preparing pore diameter controllable activated carbon by using waste membrane materials, which is different from the embodiment 3 only in that an activating agent is changed into a 10 wt% zinc chloride solution, the mass ratio of the waste membrane to a solute zinc chloride is ensured to be 1:1, and the other conditions refer to the embodiment 3.
Example 5
This example provides a method for recycling solid waste, in which a waste membrane material is used to prepare activated carbon with controllable pore size, which is different from example 3 only in that an activating agent is changed to a 10 wt% ferric chloride solution, and the mass ratio of the waste membrane to a solute ferric chloride is ensured to be 1:1, and the other conditions refer to example 3.
Experimental example 1
Pore diameter and adsorption capacity test of activated carbon prepared from waste films of different materials
(1) The pore diameters of the activated carbons obtained in examples 1 and 2 were characterized and shown in FIG. 1a, FIG. 1b, FIG. 2a and FIG. 2b (in which AC represents activated carbon).
As can be seen from the scanning electron microscope image, the surface of the activated carbon prepared from the single PVDF waste membrane has no obvious macropore (figure 1a), while the activated carbon prepared from the hollow fiber membrane containing PVDF and PET has an obvious macropore structure (figure 1 b). From FIG. 2a, it can be seen that the adsorption capacity of the activated carbon prepared from the single PVDF waste membrane is increased abruptly in the low-pressure region, indicating that a large number of micropores exist; when the adsorption pressure is continuously increased, the adsorption capacity is slightly increased, which indicates that the pore diameter is mainly microporous. The activated carbon prepared from the waste membrane containing PVDF and PET materials has larger adsorption capacity in a low-pressure area and a high-pressure area, and the combination of more intuitive pore size distribution (figure 2b) shows that the activated carbon has wider pore size distribution range from mesopores to macropores while containing abundant micropores. In FIG. 2a, the BET specific surface area of AC-PVDF + PET is 1364m2BET specific surface area of 2207 m/g, AC-PVDF2/g。
(2) Methylene blue is selected as a target pollutant, a methylene blue solution of 200mg/L is prepared, a static adsorption method is adopted, the activated carbon prepared in the embodiment 1 and the embodiment 2 is adopted as an adsorbent, and the adding amount is 0.5 g/L. The adsorption results are shown in fig. 3, the two activated carbons have faster adsorption rate to methylene blue, and the adsorption capacities exceed 400mg/g, which indicates that the two activated carbons have stronger adsorption capacity.
Experimental example 2
Activated carbon prepared by using different activating agents for activation and testing pore diameter and adsorption performance
(1) The pore diameters of the activated carbons obtained in examples 3-5 were characterized and are shown in FIG. 4a, FIG. 4b and FIG. 5.
As can be seen from the scanning electron microscope image, the surfaces of the activated carbon prepared by using sodium hydroxide as an activating agent (figure 4a) and the activated carbon prepared by using zinc chloride as an activating agent (figure 4b) also have macropores, and the surface pore channels of the activated carbon prepared by using ferric chloride as an activating agent (figure 4c) are irregular. ByIt can be further confirmed from the nitrogen adsorption-desorption curve of fig. 5a and the pore size distribution of fig. 5b that sodium hydroxide and ferric chloride as activators can obtain porous carbon having a wide pore size distribution from micropores to mesopores to macropores, and zinc chloride as an activator can obtain activated carbon having a pore size mainly of micropores. In FIG. 5a, the BET specific surface area of AC-NaOH is 791m2/g、AC-FeCl3BET specific surface area of 816m2/g、AC-ZnCl2BET specific surface area of 583m2/g。
(2) Toluene is selected as a target adsorption substance, 400mg/L high-concentration toluene solution is prepared, a static adsorption method is adopted, and the adding amount of an adsorbent is 0.5 g/L. The adsorption effect is shown in figure 6, and the result shows that the activated carbon prepared by three different activating agents can have a good removal effect on the toluene solution in water, and the adsorption performance is excellent.
The applicant states that the present invention is illustrated by the above examples, but the present invention is not limited to the above examples, i.e. the present invention is not limited to the above examples, which means that the present invention must be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
Claims (10)
1. A solid waste recycling method for preparing active carbon with adjustable pore diameter by using waste membrane materials is characterized by comprising the following steps:
(1) mixing the waste membrane material with an activating agent, and drying to obtain a mixture;
(2) and carrying out pyrolysis carbonization on the mixture under the protection of inert gas to obtain the activated carbon material.
2. The method for recycling solid waste generated in the preparation of pore size-controllable activated carbon by using the waste membrane material as claimed in claim 1, wherein the waste membrane material comprises any one or a combination of at least two of polyvinylidene fluoride, polyethylene terephthalate or polypropylene.
3. The method for recycling solid waste in the preparation of pore-size-controllable activated carbon by using the waste membrane material as claimed in claim 1 or 2, wherein the step (1) further comprises cleaning and drying the waste membrane material before mixing;
preferably, the solvent used for the washing comprises absolute ethanol and/or water.
4. The method for recycling solid waste in the preparation of pore-size-controllable activated carbon by using the waste membrane material as claimed in any one of claims 1 to 3, wherein the activating agent in the step (1) comprises any one or a combination of at least two of potassium hydroxide, sodium hydroxide, ferric chloride and zinc chloride.
5. The method for recycling solid waste generated in the process of preparing activated carbon with adjustable pore size by using waste membrane material as claimed in any one of claims 1 to 4, wherein the mass ratio of the waste membrane material to the activating agent in the step (1) is 1 (0.5-4).
6. The method for recycling solid waste in the preparation of pore-size-controllable activated carbon using waste membrane materials as claimed in any one of claims 1 to 5, wherein the mixing in step (1) is performed at 40 to 120 ℃ for 8 to 24 hours.
7. The method for recycling solid waste in the preparation of pore size-controllable activated carbon using waste membrane materials as claimed in any one of claims 1 to 6, wherein the inert gas in the step (2) comprises nitrogen or argon;
preferably, the temperature of the pyrolysis carbonization in the step (2) is 600-900 ℃, and the time of the pyrolysis carbonization is 1-4 h.
8. The resource utilization method of solid waste for preparing activated carbon with adjustable pore diameter by using waste membrane materials as claimed in any one of claims 1 to 7, wherein the pyrolysis carbonization in the step (2) comprises temperature programming, and the temperature raising rate is 2-5 ℃/min.
9. The method for recycling solid waste in the preparation of pore-size-controllable activated carbon by using the waste membrane material as claimed in any one of claims 1 to 8, wherein the pyrolysis carbonization in the step (2) further comprises a step (3): crushing, washing and drying the material subjected to pyrolysis carbonization;
preferably, the means of comminution comprises grinding;
preferably, the washing comprises acid washing and water washing;
preferably, the detergent used in the acid washing comprises 0.1-1mol/L acid solution;
preferably, the acid comprises any one of hydrochloric acid, sulfuric acid or nitric acid or a combination of at least two thereof;
preferably, the drying of step (3) is carried out at 40-80 ℃ and the drying time is longer than 10 h.
10. An activated carbon material, which is prepared by the solid waste recycling method for preparing the pore-size-controllable activated carbon by using the waste membrane material according to any one of claims 1 to 9.
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| CN115322076A (en) * | 2022-08-18 | 2022-11-11 | 华北电力大学 | Electronic waste plastic pyrolysis CO-production of phenolic chemicals and CO 2 Method for adsorbing carbon material |
| CN116409786A (en) * | 2023-03-24 | 2023-07-11 | 安徽师范大学 | Method for manufacturing porous carbon material by recycling waste filter membrane |
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