CN110734059B - Low specific surface area activated carbon and preparation method and application thereof - Google Patents
Low specific surface area activated carbon and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of activated carbon, and particularly relates to a low-specific-surface-area activated carbon, and a preparation method and application thereof. The specific surface area B of the activated carbon is not more than 900m2(ii) in terms of/g. The preparation method comprises the following steps: 1) carbonizing the spherical polymer; 2) pre-activating the product obtained in the step 1); 3) cooling the product obtained by pre-activation in the step 2), mixing the product with an alkaline compound and an alcohol compound, and activating. The preparation method provided by the invention can prepare the activated carbon with low specific surface area with good yield and low cost, and the obtained product has good granularity.
Description
Technical Field
The invention belongs to the technical field of activated carbon, and particularly relates to a low-specific-surface-area activated carbon, and a preparation method and application thereof.
Background
Activated carbon has a wide range of non-specific adsorption properties and is therefore the most widely used adsorbent. Activated carbon is generally obtained by carbonizing a carbon-containing starting compound, preferably such a compound that yields an economically reasonable yield, followed by activation. This is because the weight loss due to the removal of volatile components during carbonization and subsequent burnout during activation is significant.
The properties of the activated carbon produced (e.g. fine or coarse porosity, firmness or friability, etc.) depend on the starting material. Conventional starting materials are coconut shell, charcoal and wood, peat, stone coal, pitch, etc., because of their wide sources, the application value of activated carbon is more enhanced.
The performance of activated carbon still needs to be further developed to widen its application range.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides the activated carbon with the low specific surface area, wherein the specific surface area B of the activated carbon is not higher than 900m2G, e.g., 600-800m2G, e.g. 400-500m2/g。
According to an embodiment of the present invention, the average pore size of the activated carbon may be 1.0 to 3.0nm, for example, 1.5 to 2.0 nm.
According to an embodiment of the present invention, the average pore volume of the activated carbon may be 0.15 to 0.4cm3A/g, for example, of 0.16 to 0.3cm3/g。
According to the invention, the raw material for preparing the activated carbon is spherical polymer.
The invention also provides a preparation method of the activated carbon with low specific surface area, which comprises the following steps:
1) carbonizing the spherical polymer;
2) pre-activating the product obtained in the step 1);
3) cooling the product obtained by pre-activation in the step 2), mixing the product with an alkaline compound and an alcohol compound, and activating.
According to the present invention, in step 1), the polymer may be prepared by mixing a monomer and an initiator to perform a polymerization reaction.
By way of example, the polymer may be a homopolymer or a copolymer. Wherein, the homopolymer refers to a polymer prepared by polymerizing one monomer, and the copolymer refers to a polymer prepared by polymerizing two or more monomers.
According to the invention, the monomer can be selected from compounds having 2 to 60 carbon atoms and having at least 1 carbon-carbon double bond, for example compounds having 2 to 20 carbon atoms and having at least 1 carbon-carbon double bond. For example, the monomer may be selected from the following: ethylene, propylene, isopropene, butene, isobutylene, pentene, isopentene, neopentene, hexene, isohexene, neohexene, styrene, methylstyrene, acrylic acid, methacrylic acid, methyl acrylate, methyl methacrylate, butadiene, pentadiene, isoprene, pentadiene, isohexadiene, divinylbenzene, diethylene glycol divinyl ether.
Alternatively, the polymer matrix of the copolymer comprises structural units derived from a first monomer having from 2 to 10 carbon atoms and containing at least one carbon-carbon double bond and structural units derived from a second monomer having from 4 to 15 carbon atoms and containing at least two carbon-carbon double bonds.
Preferably, in the polymer matrix of the copolymer, the structural units derived from the first monomer constitute from 75% to 98%, preferably from 80% to 90%, of the total structural units of the polymer network; the structural units derived from the second monomer constitute from 25% to 2%, preferably from 20% to 10%, of the total structural units of the polymer network.
According to the invention, the first monomer is selected from one or more of styrene, methyl styrene, acrylic acid, methacrylic acid, methyl acrylate, methyl methacrylate and mono-olefin with 2-6 carbon atoms, such as ethylene, propylene, isopropene, butene, isobutene, pentene, isopentene, neopentene, hexene, isohexene, neohexene and the like.
According to the invention, the second monomer is selected from one or more of butadiene, pentadiene, isoprene, pentadiene, isohexadiene, divinylbenzene and diethylene glycol divinyl ether.
According to the invention, the polymerization reaction may be a suspension polymerization reaction; preferably, the polymerization is also carried out in the presence of water, dispersants, dispersion aids.
For example, water: dispersing agent: the weight ratio of the auxiliary dispersing agent is 800-1000: 0.5-3.0: 0.05 to 0.2;
when the polymer is a homopolymer, the monomer: the weight ratio of the initiator may be 1: 0.003 to 0.01.
First monomer, if present: a second monomer: the weight ratio of the initiator can be 0.75-0.98: 0.02-0.25: 0.003 to 0.01.
Preferably, the water, the dispersant and the co-dispersant constitute a water phase, and the monomer of the homopolymer, the first monomer of the copolymer, the second monomer and/or the initiator constitute an oil phase; the weight ratio of the oil phase to the water phase can be 1: 4-6.
According to the present invention, the suspension polymerization reaction may comprise:
adding the components into a reaction kettle, introducing compressed air or nitrogen into the reaction kettle, keeping the pressure in the reaction kettle in a positive pressure state with the gauge pressure less than or equal to 0.5MPa, heating to 70-90 ℃, preserving heat for 2-24 hours, heating to 100-150 ℃, preserving heat for 4-36 hours, then washing with water, drying and screening to obtain the spherical polymer.
In a preferred embodiment, the dispersant is an inorganic dispersant such as a silicate, carbonate or phosphate, or a combination thereof, or an organic dispersant such as polyvinyl alcohol, gelatin, carboxymethyl cellulose or polyacrylate, or a combination thereof.
In a preferred embodiment, the co-dispersant is sodium lauryl sulfate, calcium dodecylbenzenesulfonate, sodium dodecylbenzenesulfonate, calcium petroleum sulfonate, sodium petroleum sulfonate or barium stearate, or a combination thereof.
In a preferred embodiment, the initiator is an organic peroxide compound, an inorganic peroxide compound, or an azo compound, or a combination thereof.
In preferred embodiments, the initiator is a diacyl peroxide, a dioxane peroxide, a peroxyester, azobisisobutyronitrile, or a persulfate, or a combination thereof.
Preferably, the polymerization reaction may also be carried out in the presence of a porogen. The porogen may be selected from paraffin, magnesium sulfate, sodium carbonate, gelatin or glycerol, or a combination thereof.
According to the invention, the spherical polymer has a median particle diameter D50It may be 0.1 to 2.0mm, for example, 0.3 to 1.8mm, specifically, 0.8mm, 0.9mm, 1.0mm, 1.1mm, 1.2mm, 1.3mm, 1.4mm, 1.5mm, 1.6mm, 1.7 mm.
According to the invention, the polymer may be a sulfonated polymer or a non-sulfonated polymer. When non-sulfonated polymers are used, sulfonation may be performed prior to the carbonization step and/or sulfonation may be performed in situ during carbonization.
By way of example, the unsulfonated polymers may also be prepared according to known methods or commercially available.
The sulfonation can be carried out using starting materials known in the art, for example, by contacting the unsulfonated polymer with a sulfonating agent. The sulfonating agent may be selected from sulfuric acid (e.g., concentrated sulfuric acid), oleum, SO3A mixture of one or more of them.
According to the invention, the total weight ratio of the non-sulfonated spherical polymer to the sulfonating agent may be 3:1 to 1:3, for example 2:1 to 1:2, such as 1:1 to 1: 1.5.
The temperature of the sulfonation step may vary over a wide range.
For example, when sulfonation is carried out prior to the carbonization step, the temperature of the sulfonation step may be 60 to 200 ℃, such as 70 to 180 ℃, for example 80 to 150 ℃;
preferably, the sulfonation step may be carried out while raising the temperature within the above-mentioned temperature range. The rate of temperature rise may be no more than 10 deg.C/min, for example no more than 5 deg.C/min, such as no more than 3 deg.C/min.
The time of the sulfonation step may be from 0.5 to 12 hours, preferably from 1 to 10 hours, such as from 2 to 10 hours.
Preferably, the sulfonation is carried out under an inert gas atmosphere, which may be selected from a mixture of one or more of nitrogen, helium, and argon.
According to the present invention, the carbonization in step 1) may be performed in an inert atmosphere or in a mixed atmosphere of an inert gas and oxygen.
Typically, the temperature of the carbonization may be 100-950 ℃, such as 150-900 ℃, such as 300-850 ℃.
When sulfonation is performed prior to the carbonization step, the starting temperature of the carbonization step may be equal to or higher than the ending temperature of the sulfonation temperature.
Preferably, the carbonization step may be carried out while raising the temperature within the above-mentioned temperature range. The rate of temperature rise may be no more than 10 deg.C/min, for example no more than 5 deg.C/min, such as no more than 3 deg.C/min.
Preferably, the carbonization may be performed sequentially in 2 or more temperature zones, for example, sequentially in 2 to 10 temperature zones. And preferably, the temperatures of the temperature regions are different from each other. Alternatively, carbonization may be carried out at a gradient of increasing temperature.
Preferably, the carbonization may have the same or different temperature rise rates and the same or different holding times in different temperature regions.
Preferably, when carbonization is sequentially performed in 2 or more temperature zones, carbonization is first performed in a first temperature zone, and then carbonization is sequentially performed in a next temperature zone, for example, a second temperature zone; for example, the temperature of the first temperature region may be 100 to 500 ℃, for example, 150 to 450 ℃; the temperature of the second temperature zone may be higher than the first temperature zone, for example 500 to 950 ℃, such as 650 to 950 ℃.
Preferably, the carbonization time is from 30 minutes to 10 hours, for example from 1 to 8 hours, such as from 2 to 6 hours.
Preferably, the inert gas is selected from at least one of nitrogen, helium, argon;
preferably, when the carbonization is performed under a mixed atmosphere of an inert gas and oxygen, the volume percentage of oxygen in the mixed atmosphere is 1 to 5%.
It will be appreciated that if the spherical polymer is subjected to temperatures that allow sulfonation, the spherical polymer may also be sulfonated in situ during carbonization.
According to the invention, the preactivation of step 2) is carried out in an atmosphere comprising water vapor and/or carbon dioxide.
Preferably, the temperature of the pre-activation treatment is 700-1300 ℃, such as 800-1200 ℃, such as 850-950 ℃; the time for the pre-activation step may be from 1 to 24 hours, for example from 5 to 15 hours, such as from 6 to 12 hours.
Preferably, the atmosphere of the pre-activation step comprises water vapour, in particular water vapour and/or carbon dioxide, and a mixture of inert gases, preferably water vapour and/or carbon dioxide, nitrogen.
Preferably, the volume ratio (flow rate ratio) of the nitrogen gas, the water vapor and the carbon dioxide is 3:1:1 or more, for example, 3 to 10:1:1, preferably 4 to 8:1: 1.
According to the invention, steps3) The basic compound used in (1) can be chosen from organic or inorganic bases chosen from hydroxides, carbonates or bicarbonates of alkali or alkaline earth metals, for example LiOH, NaOH, KOH, Ca (OH)2、Na2CO3、NaHCO3、K2CO3One, two or more.
Alternatively, the basic compound may also be an oxide of an alkali metal or an oxide of an alkaline earth metal, such as CaO, K2O、Li2O or mixtures thereof.
According to the invention, the mass ratio of the product obtained in the step 2) in the step 3) to the alkaline compound is 1 (1-2.5), such as 1 (1-2.0).
According to the invention, the alcohol compound in step 3) is selected from C1-6The alkyl alcohol(s) of (b) is, for example, one or two or more selected from ethanol, propanol, n-butanol and the like.
According to the invention, the adding amount of the alcohol compound in the step 3) is 0.5-5 mL per 1g of the basic compound.
Preferably, the temperature of the activation step is 700-1300 ℃, preferably 800-1200 ℃, for example 850-950 ℃; the time for the activation step is 1 to 10 hours, for example 3 to 8 hours.
Preferably, the atmosphere of the activation step is selected from an atmosphere containing no oxygen.
For example, the atmosphere of the activation step is selected from CO2Or CO2Mixtures with inert gases, e.g. CO2And nitrogen.
Preferably, when the activating atmosphere comprises nitrogen and CO2In the mixture of (1), nitrogen and CO2The volume ratio (flow rate ratio) of (a) may be 10:1 to 1:10, such as 10:1 to 2:1, for example 8:1 to 4:1, such as 3:1 to 2: 1.
According to the present invention, the temperature rise may use a gradient temperature rise. Alternatively, the temperature may be raised to a certain temperature, and then the temperature may be raised again after the temperature is raised to 1 to 240min, for example, 5 to 150 min.
Preferably, the temperature increase process of the present invention may be continuous or intermittent.
The invention also provides the use of the activated carbon as an adsorbent.
Advantageous effects
The activated carbon and the preparation method thereof provided by the invention have obvious advantages. The applicant has surprisingly found that using the preparation method of the present invention, for example adding an alcohol compound during activation, activated carbon with low specific surface area can be prepared in good yield and at low cost. And the obtained product has better granularity.
In addition, the applicant also found that the use of the process of the present invention can improve the material wall sticking problem generated in the process of preparing activated carbon by using polymer and alkali in the existing method. Moreover, the applicant also finds that by using the method of the present application, for example, at the raw material ratio and temperature of the present application, the generation of high-risk substances, such as elemental metal, especially elemental potassium, can be suppressed, so that the problems of explosion and cracking of the generated elemental potassium or other elemental metals at the activation temperature are avoided, and the potential safety hazard existing in the production is reduced. Furthermore, the method greatly reduces the activation temperature, reduces the production energy consumption, and is suitable for industrial production.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
The specific surface areas in the examples were measured by a nitrogen physisorption instrument model Belsorp mini II from microtrac bel corp.
Preparation example 1 preparation of spherical Polymer matrix
20 liters of water is added into a 50 liter polymerization kettle, heated to 35 ℃, and respectively added with 12g of magnesium carbonate,24g of gelatin and 0.17g of methylene blue, stirring uniformly, adding an oil phase formed by mixing 3.5kg of methyl styrene, 1.2kg of dipentene and 24g of benzoyl peroxide, adding 1.25kg of paraffin, sealing a polymerization kettle, introducing clean compressed air into the polymerization kettle, and keeping the gas phase pressure in the kettle at 0.05 MPa. Then, stirring is started, liquid beads in the kettle are adjusted to be proper in particle size, the temperature is raised to 80 ℃, the temperature is maintained for 10 hours, the temperature is raised to 110 ℃, the temperature is maintained for 24 hours, and the white spherical polymer 2.51kg is obtained through filtration, washing, drying and screening, and the BET of the product is detected to be 10.423m2/g。
Example 1
1.1 carbonization
200g of the above white spherical polymer was charged into a rotary tube furnace, and subjected to the following heat treatment at a heating rate of 4 ℃/min under a nitrogen atmosphere:
heating to 150 ℃, and staying for 120 minutes;
heating to 200 ℃, and staying for 200 minutes;
the following heat treatment was carried out at a heating rate of 5 ℃/min:
heating to 350 ℃, and staying for 120 minutes;
heating to 550 ℃, and staying for 200 minutes;
then heated to 700 ℃ for 120 minutes. The temperature was reduced to obtain 188g of a carbonized product.
1.2 Pre-activation and activation
In a rotary tube furnace, the carbonized product obtained in the step 1.1 is heated to 900 ℃ at the speed of 4 ℃/min under the mixed atmosphere of water vapor, carbon dioxide and nitrogen with the flow rate ratio of 1:1:5(L/min), and is kept for 300min, and then is heated to 950 ℃ at the speed of 3 ℃/min, and is kept for 200 min. After cooling, the mixture is uniformly mixed with 376g of NaOH and 188mL of ethanol, heated to 950 ℃ at the speed of 3 ℃/min, kept for 200min and cooled to obtain 156g of low specific surface area activated carbon. The detection shows that the specific surface area of the product is 673m2Per g, mean pore volume 0.2952cm3In terms of/g, the mean pore diameter is 1.7535 nm. After the reaction is finished, the inner wall of the reaction vessel is smooth, and no white solid is generated.
Example 2
2.1 sulfonation and carbonization
The median particle diameter D obtained in preparation example 1 with a mass ratio of 1:1.5500.8mm of the white ball polymer (200g) and SO3Mixing, then adding the mixture into an acid-resistant rotary tube furnace, and carrying out the following heating treatment at a heating speed of 3 ℃/min under a helium atmosphere:
heating to 100 deg.C, and standing for 100 min;
heating to 300 ℃, and staying for 200 minutes;
the following heat treatment was performed in a mixed atmosphere of 5% by volume of oxygen at a heating rate of 4 ℃/min:
heating to 400 ℃, and staying for 100 minutes;
heating to 500 deg.C, and standing for 100 min;
then heated to 650 ℃ and left for 100 minutes. The temperature was reduced to obtain 143g of a carbonized product.
2.2 Pre-activation and activation
And (3) heating the carbonized product obtained in the step 2.1 to 900 ℃ at the speed of 4 ℃/min in a rotary tube furnace under the mixed atmosphere of water vapor and nitrogen with the volume ratio of 1:4, standing for 200min, heating to 950 ℃ at the speed of 4 ℃/min, and standing for 100 min. After cooling, evenly mixing the cooled activated carbon with 357.5g of KOH and 357.5mL of ethanol, heating to 950 ℃ at the speed of 4 ℃/min, staying for 200min, and cooling to obtain the activated carbon with low specific surface area. The specific surface area of the product is 841m by detection2Per g, mean pore volume 0.3843cm3In terms of/g, the mean pore diameter is 1.8275 nm. The inner wall of the reaction vessel is smooth, and no white solid is generated.
Example 3
The resulting low specific surface area activated carbon products described in examples 1 and 2 were used as adsorbents for gaseous contaminant removal rate testing by:
respectively weighing 100 g of samples to be tested, spreading the samples on a tray, vertically placing a glass rod wound with 5 layers of gauze into a 500mL reagent bottle, filling 200mL of pollutant formaldehyde (0.2%), and attaching a mark A1、A2. Placing the tray without the sample in the blank test chamber A, and placing the tray with the sample in the sample experimentIn compartment B. Releasing source A1、A2And respectively putting the test chamber A and the sample test chamber B into the blank test chamber A and the sample test chamber B, and immediately closing the chamber doors. And turning on fans of the A cabin and the B cabin to stir for 1 minute, and keeping the circulating fan on or off according to the requirement of the test conditions. After 24 hours, respectively carrying out sample collection test analysis on the A cabin and the B cabin, and respectively recording the concentrations as CAAnd CB。
The calculation method of the removal rate y (%) comprises the following steps:
y(％)＝(CA–CB)/CA×100
wherein C isAIs the blank cell concentration, CBIs the test chamber concentration.
The removal rate of formaldehyde was calculated to be 23.8% for the sample of example 1 and 36.5% for the sample of example 2.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (1)
1. A preparation method of activated carbon with low specific surface area is characterized by comprising the following steps:
1) adding 20 liters of water into a 50 liter polymerization kettle, heating to 35 ℃, respectively adding 12g of magnesium carbonate, 24g of gelatin and 0.17g of methylene blue under the stirring state, adding an oil phase formed by mixing 3.5kg of methyl styrene, 1.2kg of dipentene and 24g of benzoyl peroxide after uniformly stirring, adding 1.25kg of paraffin, sealing the polymerization kettle, introducing clean compressed air into the polymerization kettle, and keeping the gas phase pressure in the kettle at 0.05 MPa; then, stirring is started, liquid beads in the kettle are adjusted to be proper in particle size, the temperature is raised to 80 ℃, the temperature is maintained for 10 hours, the temperature is raised to 110 ℃, the temperature is maintained for 24 hours, and the white spherical polymer 2.51kg is obtained through filtration, washing, drying and screening, and the BET of the product is detected to be 10.423m2/g；
2) Sulfonation and carbonization
Mixing the mixture obtained in the step 1) with the mass ratio of 1:1.5Median particle diameter D50200g of the above white spherical Polymer having a particle size of 0.8mm and SO3Mixing, then adding the mixture into an acid-resistant rotary tube furnace, and carrying out the following heating treatment at a heating speed of 3 ℃/min under a helium atmosphere:
heating to 100 deg.C, and standing for 100 min;
heating to 300 ℃, and staying for 200 minutes;
the following heat treatment was performed in a mixed atmosphere of 5% by volume of oxygen at a heating rate of 4 ℃/min:
heating to 400 ℃, and staying for 100 minutes;
heating to 500 deg.C, and standing for 100 min;
then heating to 650 ℃, and staying for 100 minutes; cooling to obtain 143g of carbonized product;
3) preactivation and activation
Heating the carbonized product obtained in the step 2) to 900 ℃ at the speed of 4 ℃/min in a rotary tube furnace under the mixed atmosphere of water vapor and nitrogen with the volume ratio of 1:4, staying for 200min, then heating to 950 ℃ at the speed of 4 ℃/min, and staying for 100 min; after cooling, evenly mixing the cooled activated carbon with 357.5g of KOH and 357.5mL of ethanol, heating the mixture to 950 ℃ at the speed of 4 ℃/min, staying for 200min, and cooling to obtain the activated carbon with low specific surface area; the specific surface area of the product is 841m by detection2Per g, mean pore volume 0.3843cm3In terms of/g, the mean pore diameter is 1.8275 nm.
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| 酚醛树脂基活性炭微球的制备及其电化学性能;白俐等;《中南大学学报(自然科学版)》;20111031;第42卷(第10期);第2952-2958页 * |
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