CN103183345A - Method for preparation of nitrogen doped activated carbon from chlorine-containing organic polymer waste - Google Patents
Method for preparation of nitrogen doped activated carbon from chlorine-containing organic polymer waste Download PDFInfo
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Abstract
Belonging to the technical field of carbon material preparation, the invention relates to a method for preparation of nitrogen doped activated carbon from chlorine-containing organic polymer waste. The method includes: subjecting chlorine-containing organic polymer waste and organic amine to a dechlorination reaction, and carrying out carbonization and activation treatment in an inert atmosphere, thus obtaining the nitrogen doped activated carbon. The method provided in the invention has the advantages that: the chlorine-containing organic polymer waste is taken as the carbon source, the organic amine is adopted as the nitrogen source, the dechlorination reaction temperature is low, and the preparation process is simple. The obtained activated carbon has a high specific surface area, and is suitable to serve as a supercapacitor electrode material, a catalyst carrier and an adsorbent. The invention provides a convenient and practicable method for utilization of chlorine-containing organic polymer waste.
Description
Technical field
The present invention relates to a kind ofly utilize chloride organic polymer waste material to prepare the method for nitrogen-dopped activated carbon, belong to raw material of wood-charcoal material preparing technical field.
Background technology
Chloride organic polymer waste material is the important component part in the synthetic macromolecular material waste, mainly comprises polyvinyl chloride copolymer, chlorinatedpolyolefins, chlorinated rubber, polyvinyl chloride, chlorinatedpolyethylene, chlorinated polyvinyl chloride, Chlorinated Polypropylene III, sovprene, polyvinylidene dichloride etc.Wherein polyvinyl chloride (PVC) is one of five big general-purpose plastics synthetic materialss, has characteristics such as output is big, purposes wide, good moldability, and from world wide, PVC has become second largest synthetic resins, and consumption is only second to polyethylene.
Chloride organic polymer waste is difficult to degraded at normal temperatures, and main treatment process has landfill method, burning method and reworked material method.Landfill method can take a large amount of arable lands, and burning method can produce a large amount of harmful smog and HCl, and the reworked material method can reduce quality product, and range of application is limited, and the offal treatment amount is also less.The annual waste plastic amount of China is about 2,000,000 tons, and the huge high molecular waste material of quantity has caused the waste of serious environmental pollution problem and natural resources.Therefore, the recovery of organic polymer waste material and recycling have great economic benefit and social benefit.The patent disclosure of publication number CN101050372A the method that chloride high molecular waste material resource utilization total composition utilizes in a kind of fluidized-bed.This patent successfully is converted into two PROCESS COUPLING of chlorine with decomposing the HCl that discharges in chloride organic polymer waste material cracking hydrocarbon oil and the cracking process, has solved the shortcoming of chlorine element underutilization in the chloride organic polymer hot resolution of waste material fuel oil technology processed.The patent disclosure of publication number CN101708842A a kind of polyvinyl chloride prepare the method for active carbon with high specific surface area, prepared gac has characteristics such as ash oontent is low, specific surface area is big, pore size distribution is narrow.
Characteristics such as gac has that pore texture prosperity, specific surface area are big, heat and chemical stability are good are a kind of sorbent material and support of the catalyst of high-quality, are widely used in fields such as industry, agricultural, national defence, medical and health, environment protection.But pore texture is not only depended in the adsorption of gac, but also depends on the chemical structure of carbon surface.Nitrogen-dopped activated carbon has not only improved the activated carbon surface group, and has increased the basic sites of activated carbon surface, and this makes nitrogen-dopped activated carbon have unique catalysis and characterization of adsorption.The preparation method of nitrogen-dopped activated carbon mainly contains two kinds: a kind of is to utilize nitrogenous precursor material to prepare nitrogen-dopped activated carbon through carbonization-activation; A kind of is to the gac nitriding treatment, as the patent disclosure of publication number CN1042481A and CN101352681A nitrogen-dopped activated carbon be used for removing the bitter taste of wine and peculiar smell and as the low-temperature SCR catalyst carrier.The patent disclosure of publication number CN1217394A a kind of preparation method of high nitrogen-containing polyacrylonitrile radical active carbon fiber, can be used for the absorption of sulphur system and compound nitrogen series.The patent disclosure of publication number CN10125996A the preparation method of nitrogenous asphalt-base spherical activated carbon.
The present invention utilizes the preparation of chloride organic polymer waste material and amine reactant to contain nitrogen precursor, prepares nitrogen-dopped activated carbon through carbonization-activation, and provides a kind of feasible method for the problem of utilizing that solves chloride organic polymer waste material.
Summary of the invention
It is simple to the invention provides a kind of technology, and activator level is few, effectively utilizes chloride organic polymer waste material to prepare the method for high-specific surface area nitrogen-dopped activated carbon.This method utilizes organic amine at low temperatures chloride organic polymer waste material to be carried out dechlorination reaction, has reduced the rotproofness requirement of equipment in the follow-up carbonization process.
The technical scheme that the present invention deals with problems is: a kind ofly utilize chloride organic polymer waste material to prepare the method for nitrogen-dopped activated carbon, chloride organic polymer waste material mixed with organic amine carry out dechlorination reaction, product after the dechlorination is carried out adopting physical activation method or chemical activation method that carbonizing production is carried out activation treatment after charing is handled under inert atmosphere, namely get nitrogen doping activated carbon.
The mass ratio of described chloride organic polymer waste material and organic amine is 1: 0.5～2, and the dechlorination reaction temperature is 100～300 ℃, and the reaction times is 3～48h.
Described chloride organic polymer waste material is synthetic macromolecular material waste, be two or more mixture of polyvinyl chloride copolymer, chlorinatedpolyolefins, chlorinated rubber, polyvinyl chloride, chlorinatedpolyethylene, chlorinated polyvinyl chloride, Chlorinated Polypropylene III, sovprene, polyvinylidene dichloride waste material or its, the particle diameter of chloride organic polymer waste material is less than 5mm.Described organic amine is n-Butyl Amine 99, hexahydroaniline, aniline, diethylamine, diethanolamine, quadrol, 1,6-hexanediamine, piperazine, O-Phenylene Diamine, mphenylenediamine, Ursol D, diethylenetriamine, triethylene tetramine, tetraethylene pentamine or polyethylene polyamine.
To carry out product behind the dechlorination reaction and carry out charing and handle, the charing treatment temp is 400～600 ℃, and temperature rise rate is 2～10 ℃/min, carbonization time 1～5h; Used rare gas element is nitrogen, argon gas or helium, and flow is 50～300sccm.
The product that charing is handled carries out activation treatment, and priming reaction can adopt physical activation method or chemical activation method, and wherein the processing step of physical activation method is:
Carbonizing production is heated to activation temperature under inert atmosphere, activation temperature is 400～1000 ℃, and temperature rise rate is 2～10 ℃/min; Feed activated gas and carry out activation treatment, described activated gas is water vapour, carbonic acid gas, oxygen, air or its mixture, and gas flow is 50～300sccm; Soak time is 0.5～6h; Under inert atmosphere, be cooled to room temperature then, namely get nitrogen-dopped activated carbon.Used rare gas element is nitrogen, argon gas or helium, and flow is 50～300sccm.
The processing step of chemical activation method is:
With the product after the charing and activator mix, used activator is phosphoric acid, zinc chloride, sodium hydroxide, potassium hydroxide or salt of wormwood, the mass ratio of raw material and activator 1: 0.5～4; Be heated to activation temperature and carry out activation treatment under inert atmosphere, temperature rise rate is 2～10 ℃/min, and activation temperature is 400～1000 ℃, and soak time is 0.5～6h; Under inert atmosphere, be cooled to room temperature then, through pickling, be washed to neutrality, filter, be drying to obtain gac.Wherein, when being activator with phosphoric acid, be washed till neutrality with deionized water; With zinc chloride, sodium hydroxide, potassium hydroxide, when salt of wormwood is activator, add hydrochloric acid to mixture pH less than 3, be washed till neutrality with deionized water again.Used rare gas element is nitrogen, argon gas or helium, and flow is 50～300sccm.
The invention has the beneficial effects as follows: utilize organic amine at low temperatures chloride organic polymer waste material to be carried out dechlorination, after charing, make and contain nitrogen precursor.Activator level is few in the subsequent activation process, and technology is easy, reasonably selects raw material and activation method, can prepare the high grade activated carbon of different specific surface areas and nitrogen content.Resulting nitrogen-dopped activated carbon can be used as the electrode materials of ultracapacitor, has better electrochemical performance.
Description of drawings
Accompanying drawing 4 width of cloth of the present invention,
Fig. 1 is the nitrogen adsorption desorption figure of embodiment 6 samples; (X-coordinate: relative pressure, ordinate zou: adsorptive capacity)
Fig. 2 is the nitrogen adsorption desorption figure of embodiment 12 samples; (X-coordinate: relative pressure, ordinate zou: adsorptive capacity)
Fig. 3 is the cyclic voltammetry curves of embodiment 14 samples under the 5mVs-1 sweep velocity; (X-coordinate: voltage, ordinate zou: current density)
Fig. 4 is the ratio capacitances of embodiment 14 samples under different current densities; (X-coordinate: current density, ordinate zou: than electric capacity)
Embodiment
Following non-limiting example can make those of ordinary skill in the art more fully understand the present invention, but does not limit the present invention in any way.
Embodiment 1
The polyvinyl chloride copolymer waste material is crushed to below the particle diameter 5mm; The mass ratio of polyvinyl chloride copolymer waste material and butylamine 1: 0.5; Under 140 ℃, carry out dechlorination reaction, reaction times 48h.With the reaction product drying, at nitrogen flow rate 50sccm, under the 2 ℃/min of heat-up rate, being heated to carbonization temperature is 400 ℃, treatment time 300min.At nitrogen flow rate 50sccm, under the 2 ℃/min of heat-up rate, being heated to activation temperature is 800 ℃.Activated gas water vapour flow is 300sccm.Soak time is 6h.Under nitrogen flow 50sccm, be cooled to room temperature.The main character of this gac as shown in Table 1.
Embodiment 2
The chlorinatedpolyethylene waste material is crushed to below the particle diameter 5mm; The mass ratio of chlorinatedpolyethylene waste material and diethanolamine 1: 2; Under 250 ℃, carry out dechlorination reaction, reaction times 3h.With the reaction product drying, at argon gas flow velocity 50sccm, under the 2 ℃/min of heat-up rate, being heated to carbonization temperature is 400 ℃, treatment time 300min.At argon gas flow velocity 50sccm, under the 2 ℃/min of heat-up rate, being heated to activation temperature is 900 ℃.Activated gas water vapour flow is 100sccm.Soak time is 4h.Under argon flow amount 50sccm, be cooled to room temperature.The main character of this gac as shown in Table 1.
Embodiment 3
The chlorinatedpolyolefins waste material is crushed to below the particle diameter 5mm; The mass ratio of chlorinatedpolyolefins waste material and hexahydroaniline 1: 1.5; Under 180 ℃, carry out dechlorination reaction, reaction times 6h.With the reaction product drying, at argon gas flow velocity 300sccm, under the 10 ℃/min of heat-up rate, being heated to carbonization temperature is 600 ℃, treatment time 60min.At argon gas flow velocity 300sccm, under the 10 ℃/min of heat-up rate, being heated to activation temperature is 1000 ℃.The activated gas carbon dioxide flow is 50sccm.Soak time is 0.5h.Under argon flow amount 300sccm, be cooled to room temperature.The main character of this gac as shown in Table 1.
Embodiment 4
The chlorinatedpolyolefins waste material is crushed to below the particle diameter 5mm; The mass ratio of chlorinatedpolyolefins waste material and tetraethylene pentamine 1: 0.5; Under 300 ℃, carry out dechlorination reaction, reaction times 12h.With the reaction product drying, at argon gas flow velocity 300sccm, under the 10 ℃/min of heat-up rate, being heated to carbonization temperature is 600 ℃, treatment time 60min.At argon gas flow velocity 300sccm, under the 10 ℃/min of heat-up rate, being heated to activation temperature is 900 ℃.The activated gas carbon dioxide flow is 50sccm.Soak time is 2h.Under argon flow amount 300sccm, be cooled to room temperature.The main character of this gac as shown in Table 1.
Embodiment 5
Chlorinated rubber is crushed to below the particle diameter 5mm; The mass ratio of chlorinated rubber waste material and aniline 1: 1; Under 200 ℃, carry out dechlorination reaction, reaction times 24h.With the reaction product drying, at helium flow velocity 150sccm, under the 5 ℃/min of heat-up rate, being heated to carbonization temperature is 500 ℃, treatment time 240min.At helium flow velocity 150sccm, under the 5 ℃/min of heat-up rate, being heated to activation temperature is 400 ℃.The activated gas oxygen flow is 50sccm.Soak time is 0.5h.Under helium gas flow 150sccm, be cooled to room temperature.The main character of this gac as shown in Table 1.
Embodiment 6
The polyvinyl chloride waste material is crushed to below the 5mm; The mass ratio of polyvinyl chloride waste material and diethylamine 1: 1; Under 100 ℃, carry out dechlorination reaction, reaction times 24h.With the reaction product drying, at nitrogen flow rate 100sccm, under the 3 ℃/min of heat-up rate, being heated to carbonization temperature is 500 ℃, treatment time 120min.At nitrogen flow rate 100sccm, under the 3 ℃/min of heat-up rate, being heated to activation temperature is 500 ℃.The activated gas air flow quantity is 150sccm.Soak time is 1h.Under nitrogen flow 100sccm, be cooled to room temperature.The main character of this gac as shown in Table 1.Nitrogen adsorption desorption figure as shown in Figure 1.
Embodiment 7
Chlorinated polyvinyl chloride is crushed to below the particle diameter 5mm; The mass ratio of chlorinated polyvinyl chloride waste material and quadrol 1: 1; Under 140 ℃, carry out dechlorination reaction, reaction times 12h.With the reaction product drying, at nitrogen flow rate 50sccm, under the 2 ℃/min of heat-up rate, being heated to carbonization temperature is 400 ℃, treatment time 300min.Carbonizing production is mixed by mass ratio with activator phosphoric acid at 1: 4.At nitrogen flow rate 50sccm, under the 2 ℃/min of heat-up rate, being heated to activation temperature is 400 ℃.Soak time is 6h.Under nitrogen flow 50sccm, be cooled to room temperature.Be washed till neutrality with deionized water, can make gac after the oven dry.The main character of this gac as shown in Table 1.
Embodiment 8
Chlorinated polyvinyl chloride is crushed to below the particle diameter 5mm; The mass ratio of chlorinated polyvinyl chloride waste material and diethylenetriamine 1: 1.5; Under 200 ℃, carry out dechlorination reaction, reaction times 48h.With the reaction product drying, at nitrogen flow rate 50sccm, under the 2 ℃/min of heat-up rate, being heated to carbonization temperature is 400 ℃, treatment time 300min.Carbonizing production is mixed by mass ratio with activator phosphoric acid at 1: 2.At nitrogen flow rate 50sccm, under the 2 ℃/min of heat-up rate, being heated to activation temperature is 600 ℃.Soak time is 2h.Under nitrogen flow 50sccm, be cooled to room temperature.Be washed till neutrality with deionized water, can make gac after the oven dry.The main character of this gac as shown in Table 1.
Embodiment 9
The Chlorinated Polypropylene III waste material is crushed to below the particle diameter 5mm; The mass ratio of Chlorinated Polypropylene III waste material and 1,6-hexanediamine 1: 1; Under 180 ℃, carry out dechlorination reaction, reaction times 16h.With the reaction product drying, at argon gas flow velocity 300sccm, under the 10 ℃/min of heat-up rate, being heated to carbonization temperature is 600 ℃, treatment time 60min.Carbonizing production is mixed by mass ratio with the activator zinc chloride at 1: 2.At argon gas flow velocity 300sccm, under the 10 ℃/min of heat-up rate, being heated to activation temperature is 700 ℃.Soak time is 1h.Under argon flow amount 300sccm, be cooled to room temperature.Add hydrochloric acid to mixture pH less than 3, be washed till neutrality with deionized water again.The main character of this gac as shown in Table 1.
Embodiment 10
The Chlorinated Polypropylene III waste material is crushed to below the particle diameter 5mm; The mass ratio of Chlorinated Polypropylene III waste material and triethylene tetramine 1: 1; Under 280 ℃, carry out dechlorination reaction, reaction times 24h.With the reaction product drying, at argon gas flow velocity 300sccm, under the 10 ℃/min of heat-up rate, being heated to carbonization temperature is 600 ℃, treatment time 60min.Carbonizing production is mixed by mass ratio with the activator zinc chloride at 1: 4.At argon gas flow velocity 300sccm, under the 10 ℃/min of heat-up rate, being heated to activation temperature is 600 ℃.Soak time is 2h.Under argon flow amount 300sccm, be cooled to room temperature.Add hydrochloric acid to mixture pH less than 3, be washed till neutrality with deionized water again.The main character of this gac as shown in Table 1.
Embodiment 11
The sovprene waste material is crushed to below the particle diameter 5mm; The mass ratio of sovprene waste material and O-Phenylene Diamine 1: 1; Under 250 ℃, carry out dechlorination reaction, reaction times 24h.With the reaction product drying, at helium flow velocity 100sccm, under the 5 ℃/min of heat-up rate, being heated to carbonization temperature is 500 ℃, treatment time 240min.Carbonizing production is mixed by mass ratio with activator sodium hydroxide at 1: 0.5.At helium flow velocity 100sccm, under the 5 ℃/min of heat-up rate, being heated to activation temperature is 700 ℃.Soak time is 6h.Under helium gas flow 100sccm, be cooled to room temperature.Add hydrochloric acid to mixture pH less than 3, be washed till neutrality with deionized water again.The main character of this gac as shown in Table 1.
Embodiment 12
The polyvinylidene dichloride waste material is crushed to below the particle diameter 5mm; The mass ratio of polyvinylidene dichloride waste material and Ursol D 1: 1; Under 250 ℃, carry out dechlorination reaction, reaction times 48h.With the reaction product drying, at nitrogen flow rate 300sccm, under the 10 ℃/min of heat-up rate, being heated to carbonization temperature is 600 ℃, treatment time 60min.Carbonizing production is mixed by mass ratio with activator potassium hydroxide at 1: 1.At nitrogen flow rate 300sccm, under the 10 ℃/min of heat-up rate, being heated to activation temperature is 750 ℃.Soak time is 1.5h.Under nitrogen flow 300sccm, be cooled to room temperature.Add hydrochloric acid to mixture pH less than 3, be washed till neutrality with deionized water again.The main character of this gac as shown in Table 1.Nitrogen adsorption desorption figure as shown in Figure 2.
Embodiment 13
Chlorinated rubber and sovprene waste material are crushed to below the particle diameter 5mm; The mass ratio of chlorinated rubber and sovprene waste material and mphenylenediamine 1: 1; Under 250 ℃, carry out dechlorination reaction, reaction times 6h.With the reaction product drying, at argon gas flow velocity 50sccm, under the 2 ℃/min of heat-up rate, being heated to carbonization temperature is 400 ℃, treatment time 300min.Carbonizing production is mixed by mass ratio with activator potassium hydroxide at 1: 2.At argon gas flow velocity 50sccm, under the 2 ℃/min of heat-up rate, being heated to activation temperature is 800 ℃.Soak time is 1h.Under argon flow amount 50sccm, be cooled to room temperature.Add hydrochloric acid to mixture pH less than 3, be washed till neutrality with deionized water again.The main character of this gac as shown in Table 1.
Embodiment 14
Polyvinyl chloride and polyvinylidene dichloride waste material are crushed to below the particle diameter 5mm; The mass ratio of polyvinyl chloride and polyvinylidene dichloride waste material and piperazine 1: 1; Under 250 ℃, carry out dechlorination reaction, reaction times 12h.With the reaction product drying, at helium flow velocity 100sccm, under the 5 ℃/min of heat-up rate, being heated to carbonization temperature is 500 ℃, treatment time 180min.Carbonizing production is mixed by mass ratio with activator salt of wormwood at 1: 1.At helium flow velocity 100sccm, under the 5 ℃/min of heat-up rate, being heated to activation temperature is 800 ℃.Soak time is 1h.Under helium gas flow 100sccm, be cooled to room temperature.Add hydrochloric acid to mixture pH less than 3, be washed till neutrality with deionized water again.The main character of this gac as shown in Table 1.
Embodiment 15
Chlorinated rubber, chlorinatedpolyolefins and chlorinated polyvinyl chloride waste material powder mix are broken to below the particle diameter 5mm; The mass ratio of chlorinated rubber, chlorinatedpolyolefins and chlorinated polyvinyl chloride waste material and polyethylene polyamine 1: 1; Under 250 ℃, carry out dechlorination reaction, reaction times 36h.With the reaction product drying, at nitrogen flow rate 100sccm, under the 5 ℃/min of heat-up rate, being heated to carbonization temperature is 600 ℃, treatment time 60min.Carbonizing production is mixed by mass ratio with activator salt of wormwood at 1: 1.5.At nitrogen flow rate 100sccm, under the 5 ℃/min of heat-up rate, being heated to activation temperature is 1000 ℃.Soak time is 0.5h.Under nitrogen flow 100sccm, be cooled to room temperature.Add hydrochloric acid to mixture pH less than 3, be washed till neutrality with deionized water again.The main character of this gac as shown in Table 1.
Application example 1
The sample of embodiment 14 is scattered in to stir in a small amount of dehydrated alcohol with mass ratio with tetrafluoroethylene and conductive carbon black respectively at 80: 10: 10 makes it to mix, behind the gained slurry drying, be pressed into sheet at tabletting machine, with punch tool carbon plate being cut into diameter again is the 1cm disk.Gained disk and nickel wire collector placed between two nickel foam be made into electrode of super capacitor.Utilize the chemical property of the electrical condenser of electrochemical workstation CHI660D test material assembling, testing method comprises cyclic voltammetry (as shown in Figure 3).Land system testing constant current charge-discharge (as shown in Figure 4).Three-electrode system is adopted in test: the carbon electrode of preparation is working electrode, and the Pt electrode is counter electrode, and mercury/mercuric oxide electrode is reference electrode.Ionogen is 6molL
-1KOH solution.Cyclic voltammetry curve-0.9～-test in the voltage range of 0.1V, the voltage range of Land system testing is-0.9～-0.1V.Cyclic voltammetric test shows, material have good electrostatic double layer characteristic.The constant current charge-discharge test shows is 50mAg in current density
-1The time, the quality of gained sample can reach 280Fg than electric capacity
-1
The microtexture of table one gac
Claims (10)
1. one kind is utilized chloride organic polymer waste material to prepare the method for nitrogen-dopped activated carbon, it is characterized in that: chloride organic polymer waste material is mixed with organic amine carry out dechlorination reaction, product after the dechlorination is carried out adopting physical activation method or chemical activation method that carbonizing production is carried out activation treatment after charing is handled under inert atmosphere, namely get nitrogen doping activated carbon.
2. according to claim 1ly a kind ofly utilize chloride organic polymer waste material to prepare the method for nitrogen-dopped activated carbon, it is characterized in that: the mass ratio of described chloride organic polymer waste material and organic amine is 1: 0.5～2, the dechlorination reaction temperature is 100～300 ℃, and the reaction times is 3～48h.
3. according to claim 1ly a kind ofly utilize chloride organic polymer waste material to prepare the method for nitrogen-dopped activated carbon, it is characterized in that: described chloride organic polymer waste material is two or more mixture of polyvinyl chloride copolymer, chlorinatedpolyolefins, chlorinated rubber, polyvinyl chloride, chlorinatedpolyethylene, chlorinated polyvinyl chloride, Chlorinated Polypropylene III, sovprene, polyvinylidene dichloride waste material or its, and the particle diameter of described chloride organic polymer waste material is less than 5mm.
4. according to claim 1ly a kind ofly utilize chloride organic polymer waste material to prepare the method for nitrogen-dopped activated carbon, it is characterized in that: described organic amine is n-Butyl Amine 99, hexahydroaniline, aniline, diethylamine, diethanolamine, quadrol, 1,6-hexanediamine, piperazine, O-Phenylene Diamine, mphenylenediamine, Ursol D, diethylenetriamine, triethylene tetramine, tetraethylene pentamine or polyethylene polyamine.
5. according to claim 1ly a kind ofly utilize chloride organic polymer waste material to prepare the method for nitrogen-dopped activated carbon, it is characterized in that: described charing treatment temp is 400～600 ℃, and temperature rise rate is 2～10 ℃/min, carbonization time 1～5h; Used rare gas element is nitrogen, argon gas or helium, and flow is 50～300sccm.
6. according to claim 1ly a kind ofly utilize chloride organic polymer waste material to prepare the method for nitrogen-dopped activated carbon, it is characterized in that: described activation method is physical activation method, its processing step is: carbonizing production is heated to activation temperature under inert atmosphere, feed activated gas and carry out activation treatment, under inert atmosphere, be cooled to room temperature then, namely get nitrogen-dopped activated carbon.
7. according to claim 6ly a kind ofly utilize chloride organic polymer waste material to prepare the method for nitrogen-dopped activated carbon, it is characterized in that: described activated gas is water vapour, carbonic acid gas, oxygen, air or its mixture; Gas flow is 50～300sccm; Used rare gas element is nitrogen, argon gas or helium, and flow is 50～300sccm; Described activation temperature is 400～1000 ℃, and temperature rise rate is 2～10 ℃/min, and soak time is 0.5～6h.
8. according to claim 1ly a kind ofly utilize chloride organic polymer waste material to prepare the method for nitrogen-dopped activated carbon, it is characterized in that: described activation method is chemical activation method, its processing step is: with the product after the charing and activator mix, under inert atmosphere, be heated to activation temperature and carry out activation treatment, under inert atmosphere, be cooled to room temperature then, through pickling, be washed to neutrality, filter, be drying to obtain gac.
9. according to claim 8ly a kind ofly utilize chloride organic polymer waste material to prepare the method for nitrogen-dopped activated carbon, it is characterized in that: used activator is phosphoric acid, zinc chloride, sodium hydroxide, potassium hydroxide or salt of wormwood; The mass ratio of raw material and activator 1: 0.5～4; Used rare gas element is nitrogen, argon gas or helium, and flow is 50～300sccm; Temperature rise rate is 2～10 ℃/min, and activation temperature is 400～1000 ℃, and soak time is 0.5～6h.
10. according to claim 8ly a kind ofly utilize chloride organic polymer waste material to prepare the method for nitrogen-dopped activated carbon, it is characterized in that: when being activator with phosphoric acid, be washed till neutrality with deionized water; With zinc chloride, sodium hydroxide, potassium hydroxide, when salt of wormwood is activator, add hydrochloric acid to mixture pH less than 3, be washed till neutrality with deionized water again.
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| CN109824029B (en) * | 2019-03-28 | 2022-05-27 | 桂林电子科技大学 | Nitrogen-doped porous carbon material based on polyvinylidene chloride and preparation method and application thereof |
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