CN106672966A - Preparation method of ethylene tar-based porous carbon with narrow aperture distribution - Google Patents
Preparation method of ethylene tar-based porous carbon with narrow aperture distribution Download PDFInfo
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Abstract
The invention provides a method for preparing porous carbon from ethylene tar, and belongs to the field of advanced processing of petrochemical byproducts. The method comprises the following steps: preprocessing and pre-oxidizing ethylene tar, and uniformly dispersing the pre-oxidized ethylene tar in an alkali solution with a certain concentration; dropwise adding a magnesium precursor to the above obtained colloid, standing the obtained mixture overnight, carrying out centrifuge and drying to obtain a carbon precursor and template agent coprecipitate, and carrying out high-temperature charring and pickling in inert atmosphere to obtain the target product. The in-situ template synthesis method provided by the invention realizes homogeneous mixing of the precursor and the template and regeneration of the pickled template and also realizes the material circulation of the whole technology, and the prepared porous carbon has narrow aperture distribution, has a specific surface area reaching 1620 m<2>/g, has a specific capacitance reaching 260 F/g, can be used as an energy storage material and an electrode material, and realizes high-added value utilization of the ethylene tar.
Description
Technical field
The present invention relates to a kind of preparation method of ethylene bottom oil base porous charcoal, belongs to Some Petrochemical Byproducts field of deep.
Background technology
Porous charcoal has larger specific surface area, and complicated pore-size distribution, good electric conductivity, stable physicochemical properties are often used as absorption, energy storage and electrode material.Preparation process and presoma are the principal elements for affecting porous charcoal quality.For raw material, the biomass class raw material such as rice husk, lignin and coal tar, Colophonium, needle coke, the mineral nitrogen class raw material such as petroleum coke was all once reported as the presoma for preparing porous charcoal.Raw material-ethylene bottom oil selected by the present invention is a kind of by-product of ethylene industry, and wide material sources, carbon content is high.At present only seldom part is used for extracting naphthalene, the chemical products such as methyl naphthalene, prepare Petropols, production white carbon black etc., most of ethylene bottom oil is directly burnt as fuel, and calorific value is low and pollutes environment, compared to raw material such as Colophonium, needle coke etc. for commonly using in electrode material, its price is more cheap, is transformed into both having solved the environmental problem that its burning causes with compared with the porous carbon material of high added value, also achieves the high added value processing and utilization of waste resource.
Traditional preparation technology mainly includes the step such as carbonization, activation, and physical activation method and chemical activation method are two kinds of conventional activation methods.Physical activation method is a kind of activation method of comparative maturity, and especially for coal-tar base activated carbon, but longer soak time, relatively low specific surface area limits the application of this activation method.Alkali activation is a kind of preparation method of the activated carbon for generally adopting, and the activated carbon prepared by alkaline etching has the characteristics of specific surface area is big, and Carbon yield is high.However, substantial amounts of alkali input causes equipment corrosion, impurity to be also difficult to remove.Additionally, this synthesis path can cause a relatively wide pore-size distribution, its chemical property is limited.The appearance of template compensate for these deficiencies, and orderly mesoporous carbon can be obtained by template charing method.Conventional template has silicon template and alumina formwork etc., but these templates remove difficulty, complex operation high cost.The present invention synthesizes the steps such as template, Co carbonization and is transformed into a kind of electrode porous carbon material with high added value and narrow pore-size distribution by pretreatment.Be co-precipitated by template in situ and presoma, it is ensured that they mix and carbonization rear pattern plate agent is easily removed.Template after pickling is renewable, reduces production cost, realizes the recycling of material.
The content of the invention
It is an object of the invention to provide a kind of preparation method for preparing the porous charcoal with narrow pore-size distribution as raw material with ethylene bottom oil, using the template in situ and presoma Co carbonization method of chemosynthesis, the porous carbon material for having compared with Large ratio surface and good chemical property is obtained, the deep processing and utilization to waste resource ethylene bottom oil is realized.The present invention is realized that by the following technical programs specific implementation step is as follows:
（1）Pretreatment：A certain amount of ethylene bottom oil is dissolved in normal heptane and being flowed back 5 hours in 120 DEG C, after completion of the reaction, filters, and takes filter cake and is placed in baking oven 80 DEG C of dryings 2 hours；
The quality (g) of described ethylene bottom oil and the volume ratio of normal heptane（ml）For 1:50-1:80
（2）Pre-oxidation：By step（1）In solid dissolving be under conditions of being stirred at room temperature, to add the concentrated nitric acid that mass fraction is 65%, 60 minutes response time to mass fraction in 98% concentrated sulphuric acid.Liquid after oxidation is transferred in a large amount of water, is filtered, 70 DEG C of dryings 3 hours, and the oxidation product for obtaining is the presoma of porous carbon material；
Described concentrated sulphuric acid is 3 with the volume ratio of concentrated nitric acid:7, pretreated raw materials quality（g）Volume (ml) ratio with nitration mixture is 1：10；
（3）Precursor solution situ synthesizes chemical template：By step（2）In the presoma that obtains be distributed in certain density aqueous slkali and form colloid, 5-8 hours are stirred under room temperature；Under conditions of being stirred vigorously, the precursor water solution for taking magnesium is slowly dropped in above-mentioned colloid solution.Stand overnight, pour out supernatant, then by centrifugation, be dried, obtain carbonaceous presoma and template Mg (OH)2Coprecipitated thing；
Described aqueous slkali is the one kind in potassium hydroxide solution, sodium hydroxide solution and ammonia, and the concentration of aqueous slkali is 0.01-5
Mol/L, the quality of carbon precursor（g）With the volume of aqueous slkali（L）Than for：0.067-50:1.The precursor solution of above-mentioned magnesium is magnesium sulfate, magnesium nitrate, and one kind of magnesium chloride, the concentration of magnesium presoma is 0.01-3
Mol/L, the quality of carbon precursor（g）With the volume of magnesium precursor solution（L）Than for 0.05-30：1；
（4）Carbonization：By step（3）The coprecipitated thing for obtaining is placed in tube furnace, is warming up to 600-900 DEG C with the heating rate of 5-10 DEG C/min in an inert atmosphere, keeps 0.5-3 hours；
（5）Template is removed and regenerated：Sample dilute acid soln and deionized water after carbonization is washed successively, 120 DEG C of dryings 2 hours, obtains the porous carbon material with excellent properties；
Described diluted acid is dilute sulfuric acid, dilute hydrochloric acid, one kind of dust technology, and and step（3）In magnesium salt used have identical anion.The concentration of diluted acid be 0.25-1.5 mol/L, carbonaceous presoma（g）With the volume of acid solution（L）Than for 3-10:1.
Preferably, step（4）Noble gases used are the one kind in high pure nitrogen, high-purity argon gas and its gaseous mixture.
The present invention is in step（2）In a large amount of hydrophilic functional groups are introduced by concentrated acid oxidation, hydroxyl, carboxyl, sulfonic presence causes the presoma through aoxidizing to may be uniformly dispersed in aqueous slkali, forms stable colloid.Step（3）Described being added to the aqueous solution of magnesium salt in described colloid solution generates cotton-shaped with a template magnesium hydroxide compared with Large ratio surface, and with the reduction of pH value, carbonaceous presoma is gradually deposited with the precipitation of magnesium hydroxide ultrafine particle.This co-precipitation mode realizes mixing for carbonaceous presoma and template.Step（5）Secondary template agent MgO after middle carbonization reacts with dilute acid soln, generates corresponding magnesium salt, as step after being dried（3）Magnesium source.Whole processing route reduces production cost while added value is improved, and realizes the recycling of material in technical process.
The present invention has compared with prior art following features and beneficial effect：
（1）With ethylene bottom oil as raw material, wide material sources are cheap.The deep processing and utilization to waste resource is realized, while solving the environmental pollution for causing of directly burning, there is very high economic worth；
（2）The template of this fabricated in situ is realized and mixed with carbonaceous presoma, solves the problems, such as that conventional chemical activation process prepares the mixing that template is present uneven
（3）This technique has synthesized the activated carbon with narrow pore-size distribution, containing abundant meso-hole structure, overcomes the defect that traditional chemical activates back aperture wider distribution, is conducive to the raising of chemical property；
（4）The template of this technique is renewable, and the recycling of material is capable of achieving in whole synthesis path, and compare has very big economic advantages with other template synthesis methods, and is conducive to industrialized production；
（5）The porous charcoal specific surface of present invention synthesis is up to 1620
m2/ g, specific capacitance can reach 260 F/g.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the porous charcoal prepared in the embodiment of the present invention 1
Fig. 2 is the nitrogen adsorption desorption line and pore size distribution curve of the porous charcoal prepared in the embodiment of the present invention 1
Fig. 3 is the nitrogen adsorption desorption line and pore size distribution curve of the porous charcoal prepared in the embodiment of the present invention 2
Fig. 4 is the nitrogen adsorption desorption line and pore size distribution curve of the porous charcoal prepared in the embodiment of the present invention 3
Fig. 5 is the constant current charge-discharge curve chart of the porous charcoal prepared in the embodiment of the present invention 1
Fig. 6 is the cyclic voltammogram of the porous charcoal prepared in the embodiment of the present invention 1.
Specific embodiment
Embodiment one.
The preparation of carbonaceous presoma：10g ethylene bottom oils are dissolved in 600ml normal heptane, are heated to 120 DEG C, are flowed back 5 hours, are filtered, and are taken worry cake and are placed in drying 2 hours in 80 DEG C of baking oven.Take the above-mentioned solids of 5g to be dissolved in 35 mL mass fractions is in 98% concentrated sulphuric acid, to be slowly added to the concentrated nitric acid that 15mL mass fractions are 37%, is reacted 60 minutes under the conditions of being stirred at room temperature.Liquid after oxidation is transferred in 1L water, is filtered, 70 DEG C of dryings 3 hours, and the oxidation product for obtaining is the presoma of porous carbon material.
The preparation of porous charcoal：Take 1g carbonaceous presomas to be dissolved in the sodium hydroxide solution that 800mL concentration is 0.34mol/L, under conditions of being stirred vigorously, instill Adlerika of the 300mL concentration for 0.3mol/L.Stand overnight, remove supernatant, through centrifugation, be dried, obtain the co-precipitate of carbonaceous presoma and magnesium hydroxide.Above-mentioned co-precipitate is placed in tube furnace, 800 DEG C are warming up to the heating rate of 7 DEG C/min in ar gas environment, be incubated 1 hour, obtain the mixture of porous carbon and magnesium oxide.Said mixture is washed with the sulfuric acid solution that 250mL concentration is 1mol/L, removes template magnesium oxide, and then deionized water is rinsed, and in 120 DEG C of dryings 2 hours, obtains target product.
Scanning electron microscope (SEM) photograph in accompanying drawing 1 is observed that the porous carbon that sheet stacking is presented, and possesses obvious pore structure.Accompanying drawing 2 is its nitrogen adsorption desorption line and pore size distribution curve, and the porous charcoal specific surface for thus obtaining preparing is 1620 m2/ g, and with narrower pore-size distribution.
Electrochemical property test：The porous charcoal of preparation：Acetylene black：The mass ratio of binding agent PTFE is 85:10:5.Add ethanol so as to be tuned into pasty state, apply with foam nickel sheet, working electrode is prepared in 80 DEG C of dryings 12 hours.This survey sets and adopts three-electrode system, uses 6
The potassium hydroxide solution of mol/L is used as electrolyte.As Fig. 5, Fig. 6 are respectively its constant current charge-discharge curve chart and cyclic voltammogram, electric current density is thus obtained for 0.35 A g-1When specific capacitance be 260Fg-1。
Embodiment two.
It is prepared by carbonaceous presoma：Carbonaceous presoma is prepared according to the mode described in embodiment 1.
It is prepared by porous charcoal：Take 1g carbonaceous presomas to be dissolved in the sodium hydroxide solution that 500mL concentration is 0.6mol/L, under conditions of being stirred vigorously, instill magnesium nitrate solution of the 650mL concentration for 0.15mol/L.Stand overnight.Supernatant is removed, through centrifugation, is dried, obtain the co-precipitate of carbonaceous presoma and magnesium hydroxide.Above-mentioned co-precipitate is placed in tube furnace, 700 DEG C are warming up to the heating rate of 7 DEG C/min in ar gas environment, be incubated 1 hour, obtain the mixture of porous carbon and magnesium oxide.Said mixture is washed with the salpeter solution that 350mL concentration is 0.25mol/L, removes template magnesium oxide, and then deionized water is rinsed, and in 120 DEG C of dryings 2 hours, obtains target product.Method of testing is its nitrogen adsorption desorption line and pore size distribution curve, as a result shows with embodiment 1, accompanying drawing 3：Its specific surface is 980 m2/ g, is 0.35 A g in electric current density-1When specific capacitance up to 185Fg-1。
Embodiment three.
It is prepared by carbonaceous presoma：Carbonaceous presoma is prepared according to the mode described in embodiment 1.
It is prepared by porous charcoal：Take 1g carbonaceous presomas to be dissolved in the potassium hydroxide solution that 300mL concentration is 1mol/L, under conditions of being stirred vigorously, instill magnesium chloride solution of the 2L concentration for 0.05mol/L.Stand overnight.Supernatant is removed, through centrifugation, is dried, obtain the co-precipitate of carbonaceous presoma and magnesium hydroxide.Above-mentioned co-precipitate is placed in tube furnace, 800 DEG C are warming up to the heating rate of 7 DEG C/min in ar gas environment, be incubated 2 hours, obtain the mixture of porous carbon and magnesium oxide.Said mixture adopts 250mL concentration and washs for the hydrochloric acid solution of 1mol/L, removes template magnesium oxide, and then deionized water is rinsed, and in 120 DEG C of dryings 2 hours, obtains target product.Method of testing is its nitrogen adsorption desorption line and pore size distribution curve, as a result shows with embodiment 1, accompanying drawing 4：Its specific surface is 1500
m2/ g, is 0.35 A g in electric current density-1When specific capacitance up to 220Fg-1。
Example IV.
It is prepared by carbonaceous presoma：Carbonaceous presoma is prepared according to the mode described in embodiment 1.
It is prepared by porous charcoal：Take 1g carbonaceous presomas to be dissolved in the ammonia spirit that 900mL concentration is 0.5mol/L, under conditions of being stirred vigorously, instill Adlerika of the 750mL concentration for 0.2mol/L.Stand overnight.Supernatant is removed, through centrifugation, is dried, obtain the co-precipitate of carbonaceous presoma and magnesium hydroxide.Above-mentioned co-precipitate is placed in tube furnace, 800 DEG C are warming up to the heating rate of 10 DEG C/min in ar gas environment, be incubated 1 hour, obtain the mixture of porous carbon and magnesium oxide.Said mixture adopts 500mL concentration and washs for the sulfuric acid solution of 0.75mol/L, removes template magnesium oxide, and then deionized water is rinsed, and in 120 DEG C of dryings 2 hours, obtains target product.As a result method of testing shows with embodiment 1：Its specific surface is 1400 m2/ g, is 0.35 in electric current density
A g-1When specific capacitance up to 237Fg-1。
Embodiment five.
It is prepared by carbonaceous presoma：Carbonaceous presoma is prepared according to the mode described in embodiment 1.
It is prepared by porous charcoal：Take 1g carbonaceous presomas to be dissolved in the sodium hydroxide solution that 100mL concentration is 3mol/L, under conditions of being stirred vigorously, instill Adlerika of the 3.2L concentration for 0.03mol/L.Stand overnight.Supernatant is removed, through centrifugation, is dried, obtain the co-precipitate of carbonaceous presoma and magnesium hydroxide.Above-mentioned co-precipitate is placed in tube furnace, 800 DEG C are warming up to the heating rate of 10 DEG C/min in ar gas environment, be incubated 1 hour, obtain the mixture of porous carbon and magnesium oxide.Said mixture adopts 250mL concentration and washs for the sulfuric acid solution of 1mol/L, removes template magnesium oxide, and then deionized water is rinsed, and in 120 DEG C of dryings 2 hours, obtains target product.As a result method of testing shows with embodiment 1：Its specific surface is 1370 m2/ g, is 0.35 in electric current density
A g-1When specific capacitance up to 210Fg-1。
Embodiment six.
It is prepared by carbonaceous presoma：Carbonaceous presoma is prepared according to the mode described in embodiment 1.
It is prepared by porous charcoal：Take 1g carbonaceous presomas to be dissolved in the sodium hydroxide solution that 4.5L concentration is 0.1mol/L, under conditions of being stirred vigorously, instill magnesium nitrate solution of the 60mL concentration for 2.5mol/L.Stand overnight.Supernatant is removed, through centrifugation, is dried, obtain the co-precipitate of carbonaceous presoma and magnesium hydroxide.Above-mentioned co-precipitate is placed in tube furnace, 800 DEG C are warming up to the heating rate of 10 DEG C/min in ar gas environment, be incubated 1 hour, obtain the mixture of porous carbon and magnesium oxide.Said mixture adopts 470mL concentration and washs for the salpeter solution of 0.8mol/L, removes template magnesium oxide, and then deionized water is rinsed, and in 120 DEG C of dryings 2 hours, obtains target product.As a result method of testing shows with embodiment 1：Its specific surface is 1460 m2/ g, is 0.35 in electric current density
A g-1When specific capacitance up to 248Fg-1。
Embodiment seven.
It is prepared by carbonaceous presoma：Carbonaceous presoma is prepared according to the mode described in embodiment 1.
It is prepared by porous charcoal：Take 1g carbonaceous presomas to be dissolved in the potassium hydroxide solution that 1.1L concentration is 0.4mol/L, under conditions of being stirred vigorously, instill Adlerika of the 500mL concentration for 0.3mol/L.Stand overnight.Supernatant is removed, through centrifugation, is dried, obtain the co-precipitate of carbonaceous presoma and magnesium hydroxide.Above-mentioned co-precipitate is placed in tube furnace, 800 DEG C are warming up to the heating rate of 8 DEG C/min in ar gas environment, be incubated 1 hour, obtain the mixture of porous carbon and magnesium oxide.Said mixture adopts 380mL concentration and washs for the sulfuric acid solution of 1mol/L, removes template magnesium oxide, and then deionized water is rinsed, and in 120 DEG C of dryings 2 hours, obtains target product.As a result method of testing shows with embodiment 1：Its specific surface is 1385 m2/ g, is 0.35 in electric current density
A g-1When specific capacitance up to 239Fg-1。
Claims (7)
1. a kind of preparation method of ethylene bottom oil base porous charcoal, it is characterised in that step and condition are as follows：
（1）Pretreatment：A certain amount of ethylene bottom oil is dissolved in normal heptane and being flowed back 5 hours in 120 DEG C, after completion of the reaction, filters, and takes filter cake and is placed in baking oven 80 DEG C of dryings 2 hours；
（2）Pre-oxidation：By step（1）In solid dissolving be in 98% concentrated sulphuric acid to mass fraction, under conditions of being stirred at room temperature, add the concentrated nitric acid that mass fraction is 65%, 60 minutes response time, liquid after oxidation is transferred in a large amount of water, filter, 70 DEG C of dryings 3 hours, the oxidation product for obtaining is the presoma of porous carbon material；
（3）Precursor solution situ synthesizes chemical template：By step（2）In the presoma that obtains be distributed in certain density aqueous slkali and form colloid, 5-8 hours are stirred under room temperature；Under conditions of being stirred vigorously, the precursor water solution for taking magnesium is slowly dropped in above-mentioned colloid solution；Stand overnight, pour out supernatant, then by centrifugation, be dried, obtain carbonaceous presoma and template Mg (OH)2Coprecipitated thing；
（4）Carbonization：By step（3）The coprecipitated thing for obtaining is placed in tube furnace, is warming up to 600-900 DEG C with the heating rate of 5-10 DEG C/min in an inert atmosphere, keeps 0.5-3 hours；
（5）Template is removed and regenerated：Sample dilute acid soln and deionized water after carbonization is washed successively, 120 DEG C of dryings 2 hours, obtains the porous carbon material with excellent properties.
2. a kind of a kind of preparation method of the porous charcoal with ethylene bottom oil as raw material as claimed in claim 1, it is characterised in that step（1）The quality (g) of middle ethylene bottom oil and the volume ratio of normal heptane（ml）For 1:50-1:80.
3. a kind of a kind of preparation method of the porous charcoal with ethylene bottom oil as raw material as claimed in claim 1, it is characterised in that step（2）Middle concentrated sulphuric acid is 3 with the volume ratio of concentrated nitric acid:7, pretreated raw materials quality（g）Volume (ml) ratio with nitration mixture is 1：10.
4. a kind of a kind of preparation method of the porous charcoal with ethylene bottom oil as raw material as claimed in claim 1, it is characterised in that step（3）In aqueous slkali be one kind in potassium hydroxide solution, sodium hydroxide solution and ammonia, the concentration of aqueous slkali is 0.01-5 mol/L, the quality of carbon precursor（g）With the volume of aqueous slkali（L）Than for：0.067-50:1.
5. a kind of a kind of preparation method of the porous charcoal with ethylene bottom oil as raw material as claimed in claim 1, it is characterised in that step（3）The precursor solution of middle magnesium is magnesium sulfate, magnesium nitrate, one kind of magnesium chloride, and the concentration of magnesium presoma is 0.01-3 mol/L, the quality of carbon precursor（g）With the volume of magnesium precursor solution（L）Than for 0.05-30：1.
6. a kind of a kind of preparation method of the porous charcoal with ethylene bottom oil as raw material as claimed in claim 1, it is characterised in that step（4）In inert atmosphere be nitrogen, argon and its blender in one kind.
7. a kind of a kind of preparation method of the porous charcoal with ethylene bottom oil as raw material as claimed in claim 1, it is characterised in that step（5）In diluted acid be dilute sulfuric acid, dilute hydrochloric acid, one kind of dust technology, and and step（3）In magnesium salt used have an identical anion, dilute acid concentration is 0.25-1.5 mol/L, carbonaceous presoma（g）With the volume of acid solution（L）Than for 3-10:1.
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Application publication date: 20170517 |