CN115626644B - Briquetting activated carbon containing nano iron and preparation method and application thereof - Google Patents

Briquetting activated carbon containing nano iron and preparation method and application thereof Download PDF

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CN115626644B
CN115626644B CN202211377418.5A CN202211377418A CN115626644B CN 115626644 B CN115626644 B CN 115626644B CN 202211377418 A CN202211377418 A CN 202211377418A CN 115626644 B CN115626644 B CN 115626644B
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activated carbon
iron
briquetted
coal
solvent
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CN115626644A (en
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姚鑫
庄林生
刘娟
李鑫
谭竣元
王子义
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Ningxia Xiangtai New Material Technology Co ltd
Hefei University of Technology
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Ningxia Xiangtai New Material Technology Co ltd
Hefei University of Technology
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Abstract

The invention relates to the technical field of activated carbon preparation, and particularly discloses a briquetting activated carbon containing nano iron, a preparation method and application thereof, wherein nano particles containing iron elements are dispersed on the surface of the briquetting activated carbon, the nano particles comprise ferroferric oxide, and the particle size of the nano particles is 15-100nm; preferably, the briquetted activated carbon is prepared from raw materials comprising the following components: pulverized coal, an iron source, a surfactant and a solvent; wherein the iron source is selected from ferric salt and/or elemental iron, the ferric salt is selected from ferrous salt or ferric salt, the organic surfactant is selected from one or more than two of dodecyl amine, oleic acid or sodium oleate, and the solvent is selected from one or more than two of water, absolute ethyl alcohol or n-hexane. The invention can effectively promote the mesoporous development of the pressed activated carbon, improve the caramel decoloration rate of the pressed activated carbon, and has wide application prospect in the field of water treatment.

Description

Briquetting activated carbon containing nano iron and preparation method and application thereof
Technical Field
The invention relates to the technical field of activated carbon preparation, in particular to a pressed activated carbon containing nano iron, and a preparation method and application thereof.
Background
The production and application of the pressed and crushed granular activated carbon originate from Europe and America. Compared with powdered activated carbon, the yield of the pressed crushed granular activated carbon is relatively high, and the defects of light stacking weight, high floating rate, low strength and the like of raw coal crushed carbon in water treatment are overcome. Compared with columnar carbon, the briquetted carbon has the advantages of less raw material consumption, no use of coal tar and the like, and has a rough surface, developed mesopores and proper macroporous structures. Therefore, the briquetted and crushed granular activated carbon is a mainstream product of the activated carbon market for water treatment.
In water treatment applications, the mesoporous and macroporous structure of activated carbon has the effect of increasing the adsorption rate and enhancing the adsorption capacity of specific macromolecular adsorbents. At present, research shows that: the caramel color reduction rate of activated carbon can represent to some extent its adsorption capacity in the water treatment field. At present, the pore structure regulation and control means (improving the development of mesopores and improving the decolourization rate of caramel) aiming at the pressed broken particle active carbon mainly comprise coal blending, additives, optimizing carbonization, optimizing activation process parameters and the like. The invention patent with the application number 201610378023.5 provides coal-based briquetting activated carbon with high adsorptivity and high bulk specific gravity, which is prepared by using non-caking coal and strong caking coal as raw materials to mix coal, mixing and crushing the raw materials with asphalt and a strong alkaline compound to obtain raw material coal, and carrying out oxidation treatment, carbonization treatment and activation treatment to obtain the activated carbon. The invention patent with the application number 201610377911.5 provides coal-based briquetting activated carbon suitable for water treatment, which is prepared by blending weakly caking coal and gas coal as raw materials, mixing and crushing the raw materials with hydrogen phosphate to obtain raw material coal, and carrying out forming, granulating, oxidizing treatment, carbonizing treatment and activating treatment on the raw material coal to obtain the activated carbon.
Disclosure of Invention
The present inventors have recognized that the above-described treatment method has the following problems:
(1) In the process of preparing the pressed crushed granular active carbon by the coal blending method, the effect of improving the pore structure is greatly limited by the raw material coal;
(2) The method for regulating the pore structure by the additive has strong adaptability and high catalytic efficiency, but the key is how to realize the effective dispersion of the additive particles in the coal dust, and the traditional dispersion method comprises a mixing method, an impregnation method and an ion exchange method, but the dispersion effect still needs to be improved;
(3) Means for optimizing carbonization or activation process parameters, and regulation and control of pore structures, especially improvement of mesoporous development capability and limited effect of improving caramel decoloration rate, so that the method is limited in application in the field of water treatment;
(4) It is also a technical difficulty how to improve the development of the pore structure of the activated carbon, maintain the strength of the activated carbon, and promote the application and recovery of the activated carbon in the field of water treatment.
Namely, the technical problems solved by the invention are as follows: at present, the adsorption capacity of the coal briquetting activated carbon in the field of water treatment needs to be improved, and the mesopore development, caramel decolorization rate and strength of the coal briquetting activated carbon need to be improved.
The purpose of the invention is that: through the selection of raw material coal, additive preparation and dispersion technology, the mesopore development capability and caramel decoloration rate of the pressed broken particle active carbon are improved, and the application of the pressed broken particle active carbon in the field of water treatment is expanded.
Specifically, aiming at the defects in the prior art, the invention provides the following technical scheme:
The briquetting active carbon containing nano iron is characterized in that nano particles containing iron elements are dispersed on the surface of the briquetting active carbon, the nano particles comprise ferroferric oxide, and the particle size of the ferroferric oxide nano particles is 15-100nm, preferably 15-60nm.
Preferably, in the above briquetted activated carbon, the proportion of the iron element in the ferroferric oxide nano particles to the briquetted activated carbon is 0.1-0.5mmol/g.
Preferably, in the above briquetted activated carbon, the micropore volume of the activated carbon is 0.10-0.32cm 3/g, preferably 0.22-0.27cm 3/g, more preferably 0.25-0.27cm 3/g, and the mesopore volume of the activated carbon is 0.22-0.55cm 3/g, preferably 0.35-0.53cm 3/g, more preferably 0.50-0.53cm 3/g.
Preferably, in the above briquetted activated carbon, the mesoporosity of the activated carbon is 55 to 75%, preferably 60 to 72%, more preferably 65 to 67%.
Preferably, in the above briquetted activated carbon, the microporosity of the activated carbon is 25% to 50%, preferably 28% to 40%, more preferably 33% to 35%.
Preferably, in the above briquetted activated carbon, the specific surface area of the activated carbon is 700-1100m 2/g, preferably 880-1100m 2/g, more preferably 1000-1100m 2/g.
Preferably, in the above briquetted activated carbon, the average pore diameter of the activated carbon is 2.60 to 3.80nm, preferably 2.70 to 3.40nm, more preferably 2.8 to 3.2nm.
Preferably, in the above briquetted activated carbon, the total pore volume of the activated carbon is 0.40-0.80cm 3/g, preferably 0.60-0.80cm 3/g, more preferably 0.75-0.80.
Preferably, in the above briquetted activated carbon, the methylene blue adsorption amount of the activated carbon is 150 to 290mg/g, preferably 180 to 280mg/g, preferably 265 to 275mg/g.
Preferably, in the above briquetted activated carbon, the caramel discoloration rate of the activated carbon is 75% to 98%, preferably 94% to 98%, more preferably 96% to 98%, and still more preferably 97.5% to 98%.
Preferably, the briquetted activated carbon is prepared from the following raw materials:
Pulverized coal, an iron source, a surfactant and a solvent; wherein the iron source is selected from ferric salt and/or elemental iron, the ferric salt is selected from ferrous salt or ferric salt, the organic surfactant is selected from one or more than two of dodecyl amine, oleic acid or sodium oleate, and the solvent is selected from one or more than two of water, absolute ethyl alcohol or n-hexane.
Preferably, in the above briquetted activated carbon, the dry ash-free volatile matter of the pulverized coal is 35 to 45%, preferably 40 to 45%.
Preferably, the caking index of the pulverized coal is 10-30.
Preferably, in the above briquetted activated carbon, the fixed carbon content of the pulverized coal is 55 to 65%, preferably 55 to 60%.
Preferably, in the above briquetted activated carbon, the dry basis moisture of the pulverized coal is 8-18%, preferably 8-12%, more preferably 8-10%; the ash content of the pulverized coal is 1.5-3.5%, preferably 1.5-2.5%, more preferably 1.5-2.0%.
Preferably, in the above briquetted activated carbon, the organic surfactant is oleic acid and dodecylamine, and the solvent is n-hexane. Preferably, the molar ratio of oleic acid to dodecylamine is (0.2-0.5): 1.
Preferably, in the above briquetted activated carbon, the organic surfactant is oleic acid and sodium oleate, and the solvent is water and ethanol. Preferably, the molar ratio of oleic acid to sodium oleate is (4.5-5.0): 1, the volume ratio of water to ethanol is (1-3): 1.
Preferably, in the above briquetted activated carbon, the activated carbon is prepared by a method comprising the steps of:
Mixing raw materials comprising coal dust, an iron source, an organic surfactant and a solvent, and reacting at 160-180 ℃ to obtain a carbonized precursor; or mixing raw materials containing an iron source, a surfactant and a solvent, reacting at 160-180 ℃ to obtain iron-containing nano particles, adding pulverized coal, and mixing to obtain a carbonized precursor;
And (3) carrying out briquetting, carbonization and activation on the obtained carbonized precursor to obtain the briquetted activated carbon containing nano iron.
Preferably, in the above briquetted activated carbon, the reaction temperature is 170 to 180 ℃.
Preferably, in the above briquetted activated carbon, the reaction time is 2 to 24 hours, preferably 12 to 24 hours, more preferably 20 to 24 hours.
Preferably, in the above briquetted activated carbon, the temperature of the carbonization process is 600-900 ℃, preferably 800-900 ℃; the activation temperature of the activation process is 900-960 ℃, preferably 940-960 ℃.
Preferably, in the above briquetted activated carbon, the activating agent in the activation process is CO 2.
Preferably, in the above briquetted activated carbon, the carbonization time is 2-4 hours, and the activation time is 2-4 hours, preferably 2.5-3.5 hours.
Preferably, in the above briquetted activated carbon, the carbonization heating rate is 5-15 ℃/min, the activator flow rate in the activation process is 150-250mL/min, and the heating rate is 5-15 ℃/min.
The invention also provides a preparation method of the pressed activated carbon, which is characterized by comprising the following steps:
Mixing raw materials comprising coal dust, an iron source, an organic surfactant and a solvent, and reacting at 160-180 ℃ to obtain a carbonized precursor; or mixing raw materials containing an iron source, a surfactant and a solvent, reacting at 160-180 ℃ to obtain iron-containing nano particles, adding pulverized coal, and mixing to obtain a carbonized precursor;
And (3) carrying out briquetting, carbonization and activation on the obtained carbonized precursor to obtain the briquetted activated carbon containing nano iron.
Preferably, in the preparation method, the carbonized precursor is subjected to briquetting and carbonization to obtain carbonized material, and the carbonized material is crushed and then subjected to activation to obtain the briquetted activated carbon. Preferably, the carbonized material is crushed to a 8-30 mesh sieve.
Preferably, in the above preparation method, the carbonized material contains nano elemental iron.
Preferably, in the preparation method, the proportion of iron element in the iron source to the pulverized coal is 0.01-0.05mmol/g, preferably 0.03-0.05mmol/g, the proportion of the organic surfactant to the pulverized coal is 0.1-1.0mmol/g, preferably 0.3-0.6mmol/g, and the mass-volume ratio of the pulverized coal to the solvent is (0.1-1.0) g:1ml, preferably (0.3-0.6) g:1ml.
Preferably, in the above preparation method, the iron source includes a trivalent iron salt and elemental iron, and a molar ratio of iron element in the trivalent iron salt to iron element in the elemental iron is (2-4): 1.
Preferably, in the above preparation method, the molding process includes the steps of:
Pressing the raw materials containing the carbonization precursor into cake-shaped coal blocks.
Preferably, the carbonized precursor is extruded for 5-15min under the pressure of 30-50MPa to form cake-shaped coal blocks. Preferably, the diameter of the coal briquette is 20-25mm, and the thickness is 10-15mm.
Preferably, in the above preparation method, the carbonization yield in the carbonization process is 55% -65%, preferably 57% -62%, more preferably 58% -60%; the activation yield of the activation process is 25% -55%, preferably 25% -45%, more preferably 35% -45%.
The invention also provides application of the briquetting activated carbon in the fields of gas separation, water pollution treatment or chemical catalysis.
The invention has the advantages that: in the pressed activated carbon obtained by the invention, nano ferroferric oxide particles are uniformly dispersed, and the granularity is smaller; the invention does not use a binder, and the pressed activated carbon still has higher strength; the invention effectively promotes the development of the mesopores of the pressed activated carbon, and improves the caramel decoloration rate of the pressed activated carbon to 98 percent at most.
Drawings
FIG. 1 shows XRD patterns of the carbonized material and activated carbon obtained in example 1.
FIG. 2 is a transmission electron microscopic image of the pressed activated carbon obtained in example 1, with a scale of 100nm.
FIG. 3 is an enlarged view of the surface ferroferric oxide particles of the briquetted activated carbon obtained in example 1, with a scale of 5nm.
Detailed Description
In view of the fact that the adsorption capacity of the existing coal briquetting activated carbon in water treatment application is still to be improved, the invention provides the activated carbon containing the nano iron and the preparation method thereof.
The nano-iron in the present invention refers to nano-particles containing iron elements, such as elemental iron, iron oxides, such as ferric oxide, ferric oxide nano-particles, and the like.
The briquetted activated carbon containing nano iron according to the present invention, its preparation method and application are further described below by means of specific examples.
In the following examples, shanxi Shenmu long flame coal and Xinjiang Hami weak caking coal (caking index is 16) with large deterioration degree are selected and numbered SM and XJ respectively. The results of the industrial analysis of the coal samples are shown in the following table, wherein ad represents an air-dried basis, d represents a dried basis, and daf represents an air-dried ashless basis:
Table 1 industrial analysis of two coal samples
Sample numbering Mad/％ Ad/％ Vdaf/％ FCdaf/％
XJ 9.4 1.90 42.06 57.94
SM 16.6 3.12 37.14 62.86
TABLE 2 elemental analysis for two coal samples
In this example, other reagents were purchased from the national drug, except for coal dust. The information for each instrument used is shown in the following table:
table 3 instrument information table in example
Reagents/apparatus Specification/model Manufacturer/source
Planetary ball mill QM-3SP2 Nanjing Nanjan instruments Inc
Miniature booster tube furnace KMTF-1100-S-50-220 Hefei Kogyo He power instruments Co Ltd
Fixed target X-ray diffractometer X-PertPROMPD PANalytical
Aperture and specific surface area analyzer Autosorb-iQ QuantachromeInstruments
Transmission electron microscope JEM-2100F JEOL
Visible light spectrophotometer 722G Shanghai Instrument electric analysis instruments Co., ltd
Elemental analyzer varioELcube Elementar
Example 1
The pulverized coal is ground to pass through a 200-mesh sieve and is used for preparing the activated carbon, and the specific preparation process is as follows:
(1) Preparing a carbonization precursor: 12g of dried Xinjiang coal dust, 0.108g (0.4 mmol) FeCl 3·6H2 O, 0.0112g (0.2 mmol) iron powder, 0.35mL (1.2 mmol) oleic acid, 0.8mL (4 mmol) dodecylamine and 40mL of normal hexane are added into a liner of a hydrothermal reaction kettle, and reacted at 180 ℃ for 24 hours to obtain a carbonization precursor.
(2) And (3) forming: and (3) centrifugally drying the obtained carbonized precursor, and extruding for 10min under the pressure of 30MPa to form cake-shaped coal blocks with the diameter of 25mm and the thickness of 10 mm.
(3) Carbonizing: and (3) putting the prepared coal blocks into a tube furnace, introducing nitrogen with the flow of 200mL/min, heating the tube furnace to 600 ℃ at the speed of 10 ℃/min, carbonizing for 2 hours, and naturally cooling to room temperature to obtain the carbonized material.
(4) Activating: crushing the obtained carbonized material to 8-30 meshes, putting the carbonized material into a tube furnace, introducing CO 2 with the flow rate of 200mL/min, heating the tube furnace to 950 ℃ at the speed of 10 ℃/min, activating for 3 hours, immediately removing CO 2, introducing nitrogen, and naturally cooling to room temperature to obtain the pressed activated carbon.
The carbonization yield and activation yield in the preparation process of the embodiment are calculated, and the calculation formula is as follows:
carbonization yield = carbonized material mass 100%/coal mass
Activation yield = activated carbon mass 100%/carbonized mass
Each product of the preparation process was characterized as follows:
(1) XRD. XRD detection is carried out on the obtained carbonized material and activated carbon, and the test conditions are as follows: the Cu target has K alpha radiation lambda= 0.15406nm, power supply voltage 40KV, current 40mA, scanning speed 5 DEG/min, step length 0.02 DEG and scanning range 5-85 deg. As shown in fig. 1, it is clear from the graph that the carbonized material and the activated carbon have peaks at 26.6 degrees and 44.7 degrees, which are considered to be isotropic graphite structures (PDF 25-1077) compared with standard cards of PDF, and are considered to be isotropic graphite structures (PDF 25-1077) compared with standard cards of elemental iron (PDF 06-0696), and that the carbonized material has elemental iron, the peak of elemental iron in the activated carbon has disappeared, and the activated carbon has a Fe 3O4 crystal structure compared with standard cards of Fe 3O4 (PDF 19-0629).
(2) HRTEM. The appearance of the activated carbon is characterized by a high-resolution transmission electron microscope, the result is shown in figure 2, figure 3 is a partial enlarged view of ferroferric oxide particles, and the surface of the activated carbon is dispersed with Fe 3O4 nano particles, and the granularity is 15-40nm.
(3) Caramel decolorization rate is detected according to GB/T7702.18-2008, methylene blue adsorption value is detected according to GB/T7702.6-2008, and strength is measured according to GB/T7702.3-2008.
(4) The nitrogen adsorption/desorption isotherm of the obtained activated carbon sample was measured by using a pore diameter and specific surface area analyzer, the specific surface area of the activated carbon was calculated by using a BET equation, and the pore structure parameters and pore diameter distribution of the activated carbon were analyzed by using a BJH equation, and the results are shown in table 4.
The results show that the carbonization yield of the pressed activated carbon of the embodiment is 59.63%, the activation yield is 40.82%, the methylene blue adsorption value is 272.83mg/g, and the caramel decoloration rate is 97.97%.
Example 2
The preparation process of the activated carbon comprises the following steps:
(1) Preparing a carbonization precursor: 12g of dried Xinjiang coal dust, 0.108g (0.4 mmol) FeCl 3·6H2 O, 0.0112g (0.2 mmol) iron powder, 0.35mL (1.2 mmol) oleic acid, 0.8mL (4 mmol) dodecylamine and 40mL of normal hexane are added into a lining of a hydrothermal reaction kettle, and reacted for 3 hours at 180 ℃ to obtain a carbonization precursor.
(2) And (3) forming: and (3) centrifugally drying the obtained carbonized precursor, and extruding for 10min under the pressure of 30MPa to form cake-shaped coal blocks with the diameter of 25mm and the thickness of 10 mm.
(3) Carbonizing: and (3) putting the prepared coal blocks into a tube furnace, introducing nitrogen with the flow of 200mL/min, heating the tube furnace to 600 ℃ at the speed of 10 ℃/min, carbonizing for 2 hours, and naturally cooling to room temperature to obtain the carbonized material.
(4) Activating: crushing the obtained carbonized material to 8-30 meshes, putting the carbonized material into a tube furnace, introducing CO 2 with the flow rate of 200mL/min, heating the tube furnace to 950 ℃ at the speed of 10 ℃/min, activating for 3 hours, immediately removing CO 2, introducing nitrogen, and naturally cooling to room temperature to obtain the pressed activated carbon.
The results show that the activated carbon obtained in the embodiment has ferric oxide nano particles dispersed on the surface, the particle size is 15-50nm, the carbonization yield of the pressed activated carbon obtained in the embodiment is 61.06%, the activation yield is 42.51%, the methylene blue adsorption value of the activated carbon is 220.12mg/g, and the caramel decoloration rate is 96.79%.
Example 3
Example 3 is similar to example 2, except that in the preparation of the carbonized precursor in step (1), the reaction time of this example is 12 hours, and the briquetted activated carbon is obtained.
The results show that the surface of the active carbon obtained in the embodiment is dispersed with nano ferroferric oxide, and the particle size of the nano particles is 15-40nm. The carbonization yield of the pressed activated carbon obtained in the example is 59.08%, the activation yield is 38.92%, the methylene blue adsorption value is 272.01mg/g, and the caramel decoloration rate is 97.98%.
Example 4
Example 4 was similar to example 2, except that in the activation process of step (3), the activation time of this example was 2 hours, and briquetted activated carbon was prepared.
The results show that the activated carbon obtained in the embodiment has nano ferroferric oxide dispersed on the surface, the particle size of the nano particles is 15-80nm, the carbonization yield of the pressed activated carbon obtained in the embodiment is 59.55%, the activation yield is 54.27%, the methylene blue adsorption value is 165.86mg/g, and the caramel decoloration rate is 81.07%.
Example 5
The preparation method of the pressed activated carbon comprises the following steps:
(1) Preparing a carbonization precursor: 12g of dried Xinjiang coal dust, 0.108g (0.4 mmol) FeCl 3·6H2 O, 0.0112g (0.2 mmol) iron powder, 0.23mL (0.8 mmol) oleic acid, 0.8mL (4 mmol) dodecylamine and 40mL of normal hexane are added into a liner of a hydrothermal reaction kettle, and reacted for 12 hours at 170 ℃ to obtain a carbonization precursor.
(2) And (3) forming: and (3) centrifugally drying the obtained carbonized precursor, and extruding for 10min under the pressure of 30MPa to form cake-shaped coal blocks with the diameter of 25mm and the thickness of 10 mm.
(3) Carbonizing: and (3) putting the prepared coal blocks into a tube furnace, introducing nitrogen with the flow of 200mL/min, heating the tube furnace to 800 ℃ at the speed of 5 ℃/min, carbonizing for 2 hours, and naturally cooling to room temperature to obtain the carbonized material.
(4) Activating: crushing the obtained carbonized material to 8-30 meshes, putting the carbonized material into a tube furnace, introducing CO 2 with the flow rate of 150mL/min, heating the tube furnace to 960 ℃ at the speed of 5 ℃/min, immediately removing CO 2 after activation for 2 hours, introducing nitrogen, and naturally cooling to room temperature to obtain the pressed activated carbon.
The results show that the surface of the activated carbon obtained in the embodiment is dispersed with nano ferroferric oxide, the particle size of the nano particles is 15-60nm, the carbonization yield of the obtained pressed activated carbon is 58.95%, the activation yield is 53.81%, the methylene blue adsorption value is 166.87mg/g, and the caramel decoloration rate is 82.58%.
Example 6
The preparation method of the pressed activated carbon comprises the following steps:
(1) Preparing a carbonization precursor: 12g of dried Xinjiang coal dust, 0.216g (0.8 mmol) FeCl 3·6H2 O, 0.0112g (0.2 mmol) iron powder, 0.58mL (2 mmol) oleic acid, 0.8mL (4 mmol) dodecylamine and 40mL of normal hexane are added into a lining of a hydrothermal reaction kettle, and reacted for 24 hours at 160 ℃ to obtain a carbonization precursor.
(2) And (3) forming: and (3) centrifugally drying the obtained carbonized precursor, and extruding for 10min under the pressure of 30MPa to form cake-shaped coal blocks with the diameter of 20mm and the thickness of 15 mm.
(3) Carbonizing: and (3) putting the prepared coal blocks into a tube furnace, introducing nitrogen with the flow of 200mL/min, heating the tube furnace to 600 ℃ at the speed of 10 ℃/min, carbonizing for 4 hours, and naturally cooling to room temperature to obtain carbonized materials.
(4) Activating: crushing the obtained carbonized material to 8-30 meshes, putting the carbonized material into a tube furnace, introducing CO 2 with the flow rate of 200mL/min, heating the tube furnace to 940 ℃ at the speed of 10 ℃/min, activating for 2 hours, immediately removing CO 2, introducing nitrogen, and naturally cooling to room temperature to obtain the pressed activated carbon.
The results show that the surface of the activated carbon obtained in the embodiment is dispersed with nano ferroferric oxide, the particle size of the nano particles is 15-100nm, the carbonization yield of the obtained pressed activated carbon is 59.59%, the activation yield is 53.59%, the methylene blue adsorption value is 186.37mg/g, and the caramel decoloration rate is 77.64%.
Example 7
The preparation process of the pressed activated carbon comprises the following steps:
(1) Preparing a carbonization precursor: to the inner lining of the hydrothermal reaction kettle, 0.108g (0.4 mmol) FeCl 3·6H2 O, 0.0112g (0.2 mmol) iron powder, 0.35mL (1.2 mmol) oleic acid, 0.8mL (4 mmol) dodecylamine and 20mL n-hexane were added, and reacted at 180℃for 3 hours to obtain a nano Fe 3O4 particle dispersion solution, 12g dry Xinjiang coal dust was added thereto, and after stirring and ultrasonic treatment for 10 minutes, a carbonized precursor was obtained.
(2) And (3) forming: and (3) centrifugally drying the obtained carbonized precursor, and extruding for 10min under the pressure of 30MPa to form cake-shaped coal blocks with the diameter of 25mm and the thickness of 10 mm.
(3) Carbonizing: and (3) putting the prepared coal blocks into a tube furnace, introducing nitrogen with the flow of 200mL/min, heating the tube furnace to 900 ℃ at the speed of 10 ℃/min, carbonizing for 2 hours, and naturally cooling to room temperature to obtain the carbonized material.
(4) Activating: crushing the obtained carbonized material to 8-30 meshes, putting the carbonized material into a tube furnace, introducing CO 2 with the flow rate of 200mL/min, heating the tube furnace to 950 ℃ at the speed of 10 ℃/min, activating for 3 hours, immediately removing CO 2, introducing nitrogen, and naturally cooling to room temperature to obtain the pressed activated carbon.
The results show that the surface of the activated carbon obtained in the embodiment is dispersed with nano ferroferric oxide, the particle size of the nano particles is 15-40nm, the carbonization yield of the obtained pressed activated carbon is 61.24%, the activation yield is 36.06%, the methylene blue adsorption value is 182.07mg/g, and the caramel decoloration rate is 97.21%.
Example 8
(1) Preparing a carbonization precursor: 12g of dried Xinjiang coal dust, 0.108g (0.4 mmol) FeCl 3·6H2 O, 0.35g (1.15 mmol) sodium oleate, 1.6mL (5.5 mmol) oleic acid, 12.8mL absolute ethyl alcohol and 25.6mL deionized water are added into a lining of a hydrothermal reaction kettle, and the mixture is reacted for 3 hours at 180 ℃ to obtain a carbonized precursor containing ferric oxide nano particles.
(2) And (3) forming: and (3) centrifugally drying the obtained carbonized precursor, and extruding for 10min under the pressure of 30MPa to form cake-shaped coal blocks with the diameter of 25mm and the thickness of 10 mm.
(3) Carbonizing: and (3) putting the prepared coal blocks into a tube furnace, introducing nitrogen with the flow of 200mL/min, heating the tube furnace to 600 ℃ at the speed of 10 ℃/min, carbonizing for 2 hours, and naturally cooling to room temperature to obtain the carbonized material.
(4) Activating: crushing the obtained carbonized material to 8-30 meshes, putting the carbonized material into a tube furnace, introducing CO 2 with the flow rate of 200mL/min, heating the tube furnace to 950 ℃ at the speed of 10 ℃/min, activating for 3.5h, immediately removing CO 2, introducing nitrogen, and naturally cooling to room temperature to obtain the pressed activated carbon.
The results show that the surface of the activated carbon obtained in the embodiment is dispersed with nano ferroferric oxide, the particle size of the nano particles is 15-50nm, the carbonization yield of the obtained pressed activated carbon is 58.31%, the activation yield is 27.86%, the methylene blue adsorption value is 217.42mg/g, and the caramel decoloration rate is 94.26%.
Example 9
Example 9 is similar to example 8, except that in the preparation of the carbonized precursor in step (1), the reaction time of this example is 12 hours, and the briquetted activated carbon is prepared.
The results show that the activated carbon obtained in the embodiment has nano ferroferric oxide dispersed on the surface, the particle size of the nano particles is 15-50nm, the carbonization yield of the pressed activated carbon obtained in the embodiment 9 is 57.12%, the activation yield is 31.21%, the methylene blue adsorption value is 216.93mg/g, and the caramel decoloration rate is 94.24%.
Example 10
The preparation process of the pressed activated carbon comprises the following steps:
(1) Preparing a carbonization precursor: 10g of dried Xinjiang coal dust, 0.108g (0.4 mmol) FeCl 3·6H2 O, 0.35g (1.15 mmol) sodium oleate, 1.6mL (5.5 mmol) oleic acid, 12.8mL absolute ethyl alcohol and 25.6mL deionized water are added into a lining of a hydrothermal reaction kettle, and the mixture is reacted for 3 hours at 180 ℃ to obtain a carbonization precursor.
(2) And (3) forming: and (3) centrifugally drying the obtained carbonized precursor, and extruding for 10min under the pressure of 30MPa to form cake-shaped coal blocks with the diameter of 25mm and the thickness of 10 mm.
(3) Carbonizing: and (3) putting the prepared coal blocks into a tube furnace, introducing nitrogen with the flow of 200mL/min, heating the tube furnace to 600 ℃ at the speed of 10 ℃/min, carbonizing for 2 hours, and naturally cooling to room temperature to obtain the carbonized material.
(4) Activating: crushing the obtained carbonized material to 8-30 meshes, putting the carbonized material into a tube furnace, introducing CO 2 with the flow rate of 200mL/min, heating the tube furnace to 950 ℃ at the speed of 10 ℃/min, activating for 2 hours, immediately removing CO 2, introducing nitrogen, and naturally cooling to room temperature to obtain the pressed activated carbon.
The results show that the surface of the activated carbon obtained in the embodiment is dispersed with nano ferroferric oxide, the particle size of the nano particles is 15-100nm, the carbonization yield of the obtained pressed activated carbon is 58.47%, the activation yield is 45.6%, the methylene blue adsorption value is 173.24mg/g, and the caramel decoloration rate is 76.77%.
Example 11
(1) Preparing a carbonization precursor: 16g of dried Xinjiang coal dust, 0.108g (0.4 mmol) FeCl 3·6H2 O, 0.33g (1.1 mmol) sodium oleate, 1.6mL (5.5 mmol) oleic acid, 6mL absolute ethyl alcohol and 14mL deionized water are added into a lining of a hydrothermal reaction kettle, and the mixture is reacted for 12 hours at 160 ℃ to obtain a carbonization precursor.
(2) And (3) forming: and (3) centrifugally drying the obtained carbonized precursor, and extruding for 10min under the pressure of 30MPa to form cake-shaped coal blocks with the diameter of 25mm and the thickness of 10 mm.
(3) Carbonizing: and (3) putting the prepared coal blocks into a tube furnace, introducing nitrogen with the flow of 200mL/min, heating the tube furnace to 600 ℃ at the speed of 10 ℃/min, carbonizing for 2 hours, and naturally cooling to room temperature to obtain the carbonized material.
(4) Activating: crushing the obtained carbonized material to 8-30 meshes, putting the carbonized material into a tube furnace, introducing CO 2 with the flow rate of 200mL/min, heating the tube furnace to 900 ℃ at the speed of 10 ℃/min, activating for 2 hours, immediately removing CO 2, introducing nitrogen, and naturally cooling to room temperature to obtain the pressed activated carbon.
The results show that the surface of the activated carbon obtained in the embodiment is dispersed with nano ferroferric oxide, the particle size of the nano particles is 15-100nm, the carbonization yield of the obtained pressed activated carbon is 56.47%, the activation yield is 42.37%, the methylene blue adsorption value is 166.85mg/g, and the caramel decoloration rate is 75.17%.
Example 12
Example 12 is similar to example 8, except that in the preparation of the carbonized precursor in step (1), the reaction temperature in this example is 170 ℃ and the reaction time is 24 hours; in the activation process of the step (3), the activation time of the embodiment is 2 hours, and the pressed activated carbon is prepared.
The results show that the surface of the activated carbon obtained in the embodiment is dispersed with nano ferroferric oxide, the particle size of the nano particles is 15-80nm, the carbonization yield of the obtained pressed activated carbon is 56.01%, the activation yield is 49.95%, the methylene blue adsorption value is 166.02mg/g, and the caramel decoloration rate is 81.78%.
The strength test results show that the strength of the pressed activated carbon obtained in the examples 1-12 can reach more than 95.
Example 13
Example 13 is similar to example 4 except that the Xinjiang coal dust in step (1) is changed to Shenmu coal dust to prepare briquetted activated carbon.
The results show that the surface of the activated carbon obtained in the embodiment is dispersed with nano ferroferric oxide, the particle size of the nano particles is 15-100nm, the carbonization yield of the obtained pressed activated carbon is 62.45%, the activation yield is 45.84%, the methylene blue adsorption value is 188.90mg/g, and the caramel decoloration rate is 77.51%.
Example 14
Example 14 is similar to example 7 except that Xinjiang coal powder in example 7 is changed to Shenmu coal powder, and in the activation process of step (3), the activation time of this example is 2h, so as to prepare briquetted activated carbon.
The results show that the surface of the activated carbon obtained in the embodiment is dispersed with nano ferroferric oxide, the particle size of the nano particles is 15-100nm, the carbonization yield of the obtained pressed activated carbon is 59.71%, the activation yield is 33.21%, the methylene blue adsorption value is 159.92mg/g, and the caramel decoloration rate is 82.43%.
The strength test results showed that the strength of examples 13 and 14 was between 85-90.
Comparative example 1
6G of Xinjiang coal dust was taken and activated carbon was prepared by the molding, carbonization and activation process described in example 2.
The carbonization yield of the pressed activated carbon obtained in comparative example 1 was 59.31%, the activation yield was 53.15%, and the methylene blue adsorption value was 151.12mg/g.
Comparative example 2
(1) And (3) forming: 6g of dried Shenmu coal powder is taken and extruded for 10min under the pressure of 30MPa to form cake-shaped coal blocks with the diameter of 25mm and the thickness of 10 mm.
(2) Carbonizing: and (3) putting the prepared coal blocks into a tube furnace, introducing nitrogen with the flow of 200mL/min, heating the tube furnace to 950 ℃ at the speed of 10 ℃/min, carbonizing for 2 hours, and naturally cooling to room temperature to obtain the carbonized material.
(3) Activating: crushing the obtained carbonized material to 8-30 meshes, putting the carbonized material into a tube furnace, introducing CO 2 with the flow rate of 200mL/min, heating the tube furnace to 950 ℃ at the speed of 10 ℃/min, activating for 2 hours, immediately removing CO 2, introducing nitrogen, and naturally cooling to room temperature to obtain the pressed activated carbon.
The carbonization yield of the pressed activated carbon obtained in comparative example 2 was 59.75%, the activation yield was 48.86%, and the methylene blue adsorption value was 166.56mg/g.
Comparative example 3
12G of dried Xinjiang coal dust and 40mL of 0.01mol/L FeCl 3 solution are added into a lining of a hydrothermal reaction kettle, the mixture is reacted for 3 hours at 180 ℃, and after centrifugal drying, briquetted activated carbon is prepared by the forming, carbonizing and activating processes described in example 1.
The surface of the pressed activated carbon obtained in the comparative example 3 is dispersed with ferroferric oxide particles, and the particles have larger particle size and uneven distribution. The carbonization yield of the pressed activated carbon obtained in the example is 63.70%, the activation yield is 52.99%, the methylene blue adsorption capacity is 176.41mg/g, and the caramel decoloration rate is 74.37%.
Table 4 pore structure characterization results of the briquetted activated carbons obtained in examples and comparative examples
In conclusion, the invention effectively improves the mesoporous development capability of the pressed activated carbon on the basis of ensuring the strength of the pressed activated carbon by the dispersion technology of the additive through the selection of the raw material coal, greatly improves the caramel decoloration rate of the activated carbon, and has wide application prospect in the field of water treatment.

Claims (8)

1. The coal-based briquetting activated carbon containing nano iron is characterized in that nano particles containing iron elements are dispersed on the surface of the briquetting activated carbon, the nano particles comprise ferroferric oxide, and the particle size of the nano particles is 15-100nm;
wherein the micropore volume of the pressed activated carbon is 0.22-0.27cm 3/g, and the mesopore volume of the pressed activated carbon is 0.35-0.53cm 3/g;
the briquetting activated carbon is prepared by a preparation method comprising the following steps:
Mixing raw materials comprising coal dust, an iron source, an organic surfactant and a solvent, and reacting at 160-180 ℃ to obtain a carbonized precursor; or mixing raw materials containing an iron source, a surfactant and a solvent, reacting at 160-180 ℃ to obtain iron-containing nano particles, adding pulverized coal, and mixing to obtain a carbonized precursor;
The obtained carbonized precursor is subjected to briquetting, carbonization and activation to obtain the briquetted activated carbon containing nano iron;
Wherein, the proportion of iron element in the iron source to coal powder is 0.01-0.05mmol/g, the proportion of organic surfactant to coal powder is 0.1-1.0mmol/g, and the mass volume ratio of coal powder to solvent is (0.1-1.0) g:1ml.
2. The briquetted activated carbon of claim 1, wherein the mesoporosity of the activated carbon is 55-75%.
3. The briquetted activated carbon of claim 1, wherein the activated carbon has an average pore size of 2.60-3.80nm.
4. The briquetted activated carbon of claim 2, wherein the activated carbon has an average pore size of 2.60-3.80nm.
5. The briquetted activated carbon of any one of claims 1 to 4, wherein the iron source is selected from iron salts selected from ferrous or ferric salts, the organic surfactant is selected from one or two or more of dodecanol, oleic acid or sodium oleate, and the solvent is selected from one or two or more of water, absolute ethanol or n-hexane.
6. The briquetted activated carbon of claim 5, wherein the temperature of the carbonization process is 600-900 ℃; the temperature of the activation process is 900-960 ℃.
7. A process for the preparation of briquetted activated carbon according to any one of claims 1 to 6, characterized by comprising the steps of:
Mixing raw materials comprising coal dust, an iron source, an organic surfactant and a solvent, and reacting at 160-180 ℃ to obtain a carbonized precursor; or mixing raw materials containing an iron source, a surfactant and a solvent, reacting at 160-180 ℃ to obtain iron-containing nano particles, adding pulverized coal, and mixing to obtain a carbonized precursor;
The obtained carbonized precursor is subjected to briquetting, carbonization and activation to obtain the briquetted activated carbon containing nano iron;
Wherein, the proportion of iron element in the iron source to coal powder is 0.01-0.05mmol/g, the proportion of organic surfactant to coal powder is 0.1-1.0mmol/g, and the mass volume ratio of coal powder to solvent is (0.1-1.0) g:1ml.
8. Use of the briquetted activated carbon of any one of claims 1-6 in the field of gas separation, water pollution treatment or chemical catalysis.
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