CN112691643A - Preparation method of micron spherical activated carbon - Google Patents
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- CN112691643A CN112691643A CN202011533044.2A CN202011533044A CN112691643A CN 112691643 A CN112691643 A CN 112691643A CN 202011533044 A CN202011533044 A CN 202011533044A CN 112691643 A CN112691643 A CN 112691643A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 140
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 19
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 33
- 229910021645 metal ion Inorganic materials 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 8
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- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 5
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- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
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- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- WXBLLCUINBKULX-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1.OC(=O)C1=CC=CC=C1 WXBLLCUINBKULX-UHFFFAOYSA-N 0.000 claims description 2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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Abstract
The invention discloses a preparation method of micron spherical activated carbon, belongs to the technical field of activated carbon, and relates to spherical activated carbon. A process for preparing micron-class spherical activated carbon includes mixing activated carbon with sensitizer under microwave condition, and controlling the microwave action on the surface of activated carbon by sensitizer to obtain micron-class spherical activated carbon. The invention has the advantages of easily obtained raw material cost, low energy consumption, simple process flow and high yield, and can realize large-scale production.
Description
Technical Field
The invention belongs to the technical field of activated carbon, relates to spherical activated carbon, and particularly relates to a preparation method of micron spherical activated carbon.
Background
The activated carbon is a porous adsorption material with large specific surface area, developed pore structure and rich surface functional groups, belongs to amorphous carbon, has the characteristics of stable physicochemical property, acid resistance, alkali resistance, heat resistance, insolubility in water and organic solvents, high mechanical strength and recyclability, can be widely applied to gas phase adsorption, adsorption of organic or inorganic substances in liquid phase, colloid particle adsorption, harmful metal ion adsorption and the like, and is an adsorbent with excellent performance.
The spherical activated carbon is a novel activated carbon, can be applied to the fields of preparation of catalyst carriers, electrode materials, template agents, composite materials and the like due to the characteristics of regular spherical structure, good stacking density, high specific surface area, excellent electric and heat conducting properties and the like, becomes an important direction for research and development of material fields, and has good application prospects in the fields of sugar manufacturing, medicines, foods, chemical industry, national defense, environmental protection, agriculture and the like.
The spherical activated carbon can be divided into 3 types according to different raw materials: asphalt-based, polymer-based, and coal-based spherical activated carbons. The coal-based spherical activated carbon has the advantages of wide raw materials, low cost and the like, is used as a diarrhea treatment agent and an oral antidote, has a relatively simple preparation process, and is mainly prepared by a disc rolling spheronization method, but the prepared spherical activated carbon has the defects of low mechanical strength, high ash content and the like, so the application field of the spherical activated carbon is limited; the asphalt-based spherical activated carbon has the advantages of wide raw materials and low price, but has the disadvantages of complex production process flow, many process parameters and variables, high energy consumption and long process flow, low production efficiency, high production cost and poor environmental protection; the cost of the polymer-based raw materials is high, and the large-scale production has certain difficulty. The preparation process comprises a spraying method, an emulsion phase separation method, a precipitation polymerization method, a layering balling method, a hydrothermal method and the like, wherein the spraying method is that the raw materials form liquid drops through spraying, carbonization is carried out under inert gas and high temperature, and finally, spherical active carbon is obtained through activation; the emulsion phase separation method is to disperse one phase in the other phase and polymerize the same into spheres; the precipitation polymerization method is to dissolve a monomer and an initiator in a medium, and after the reaction occurs, as the polymerization degree deepens, the polymer is incompatible with the solvent, so that a precipitate is separated out, and a solid spherical polymer is formed; the material and viscosity reducing agent are mixed and scrupulously and respectfully is melted by a layering and balling method, extruded into strips, cut to a proper size, then the viscosity reducing agent is reduced, cultivated, carbonized and activated to obtain the active carbon; the hydrothermal method is a chemical reaction in a closed pressure vessel with water as a solvent at high temperature and high pressure.
However, the production cost of the prior spherical activated carbon is high, the products need to be imported from foreign countries at high price by domestic random modeling production process and production line, the application of the spherical activated carbon is limited, and the products especially used for national defense and military industry are strictly limited.
In order to solve the problems in the technical field of the existing spherical activated carbon, the invention researches and develops a preparation process of micron-sized activated carbon which is low in cost, easy to operate and capable of being produced in a large scale.
Disclosure of Invention
The invention aims to provide a preparation method of micron spherical activated carbon, so as to achieve the purposes of reducing cost, simplifying process and realizing large-scale production.
The invention is realized by the following technical scheme:
a process for preparing micron-class spherical activated carbon includes mixing activated carbon with sensitizer under microwave condition, and controlling the microwave action on the surface of activated carbon by sensitizer to obtain micron-class spherical activated carbon.
Further, the soluble organic matter is any one or more of polyethylene glycol, sodium polyacrylate, ethanol or benzoic acid.
The metal ion salt is any one of magnesium nitrate, ferric nitrate or aluminum nitrate.
The preparation method of the sensitizer comprises the steps of dissolving organic matters and metal ion salts in a mass ratio of 4-18:10-50 in distilled water, dropwise adding acetic acid and tetrabutyl titanate solution, and uniformly mixing.
The preparation method of the sensitizer comprises the steps of adding 4-18g of organic matters and 10-50g of metal ion salts into 10L of distilled water, then dropwise adding 10mL of tetrabutyl titanate solution and 5-8mL of acetic acid, and uniformly mixing.
The microwave power is 700-750w, and the preferred microwave fire power is 70-50%, for example, a commercial household microwave oven can be used, and the fire power can be medium fire or medium-low fire.
The mixing reaction time of the activated carbon and the sensitizer under the microwave condition is 1-2.5 min.
Every 100g of the activated carbon is mixed with 100 and 200mL of the sensitizer.
The microwave energy can generate an electric field and a magnetic field in the dielectric material, the polar material and the magnetic material, and the point positions have strong action with the microwave energy, so that the microwave energy can be changed into heat energy at the point positions, the point positions are selectively heated to a high temperature in a short time, and the activated carbon has strong microwave absorption property. Because of the non-uniformity of the structure of the activated carbon, a plurality of hot spots are generated on the surface of the activated carbon in the microwave heating process, the hot spot formation has three conditions that materials with different dielectric losses are non-uniformly distributed, a microwave field with non-uniform distribution exists, and reactants have different heat conduction speeds, so that the common active carbon and the sensitizing agent are placed in a microwave environment to enable the surface of the common active carbon to generate a plurality of 'hot spots', the temperature of the 'hot spots' is much higher than that of other parts, the surface of the activated carbon is easily sintered to generate thermal runaway when the temperature exceeds 1000 ℃, tetrabutyl titanate in the sensitizing agent gradually generates gel-like substances through hydrolysis reaction, proper amount of acetic acid is added to prevent the generation of precipitates, soluble organic matters and metal ions are adsorbed on the surface of common active carbon and mainly act on the tip and the convex part to enable the active carbon to be spherical.
The analysis of test data shows that the relative pressure of capillary condensation of microwave pretreated activated carbon is higher than that of the conventional method and water as a treating agent, the mesoporous hysteresis loop formed by the capillary condensation is not changed, and the shapes of the mesoporous hysteresis loop are the same, which shows that the types of pores of the microwave activated carbon are not changed, but are increased in number, so that the pressure of the capillary condensation is increased, and the infrared spectrograms under several pretreatment conditions are compared.
The invention has the advantages of easily obtained raw material cost, low energy consumption, simple process flow and high yield, and can realize large-scale production.
Drawings
FIG. 1 is an electron micrograph of a common commercially available activated carbon of example 1;
FIG. 2 is an IR spectrum of a common commercially available activated carbon of example 1;
FIG. 3 is a drawing showing a common commercially available activated carbon of example 1;
FIG. 4 is an electron microscope image of the spherical activated carbon of example 2 micron;
FIG. 5 is an electron micrograph of the spherical activated carbon of example 3 μm;
FIG. 6 is an infrared spectrum of example 3 micron spherical activated carbon;
FIG. 7 is a drawing of example 3 micron spherical activated carbon;
FIG. 8 is an electron micrograph of the spherical activated carbon of example 4 μm;
FIG. 9 is an infrared spectrum of example 4 micron spherical activated carbon;
FIG. 10 is an electron micrograph of spherical activated carbon of example 5 μm;
FIG. 11 is an IR spectrum of example 5 micron spherical activated carbon;
FIG. 12 is a drawing of example 5 micron spherical activated carbon.
Detailed Description
The invention is further illustrated by the following figures and examples.
Example 1
100g of common commercial activated carbon was mixed with 150mL of water, activated according to a conventional method, and subjected to electron microscope, infrared and adsorption tests respectively, as shown in FIGS. 1, 2 and 3, respectively, having a BET specific surface area of 875.49 m/g and a pore volume of 0.1002 cm/g.
Example 2
(1) Preparing a sensitization control reagent: adding 10L of distilled water, 4g of soluble organic matter sodium polyacrylate and 20 g of metal ion salt magnesium nitrate, dropwise adding 10mL of tetrabutyl titanate solution and 5mL of acetic acid while stirring, and uniformly mixing to obtain a sensitizer;
(2) mixing 100g of activated carbon with 100mL of sensitizer, performing electron microscope test under the condition of household microwave oven fire for 2min, and obtaining the result as shown in FIG. 4, the BET specific surface area is 880.73 m/g, and the pore volume is 0.1019 cm/g.
Example 3
(1) Preparing a sensitization control reagent: adding 10L of distilled water, 15g of soluble organic ethanol and 50g of metal ion salt aluminum nitrate, dropwise adding 10mL of tetrabutyl titanate solution and 6mL of acetic acid under stirring, and uniformly mixing to obtain a sensitizer;
(2) mixing 100g of activated carbon with 120mL of sensitizer, performing electron microscope test under the microwave condition of medium fire and high fire for 1min, performing electron microscope, infrared and adsorption test respectively, wherein the test results are respectively shown in figures 5, 6 and 7, as can be seen from the electron microscope, most of the activated carbon added with the sensitization control reagent is spherical, the surface area and the pore volume are obviously increased,
BET specific surface area 1,759.1108 m/g, pore volume 0.1131 cm were subjected to thin film chromatography.
Example 4
(1) Preparing a sensitization control reagent: adding 10L of distilled water, adding 18g of soluble organic acetic acid and 30 g of metal ion salt aluminum nitrate, stirring, dripping 10mL of tetrabutyl titanate solution and 7mL of acetic acid, and uniformly mixing to obtain a sensitizer;
(2) 100g of activated carbon and 180mL of sensitizer are mixed, and then the mixture is subjected to microwave heating for 3min under microwave high-fire conditions and subjected to electron microscope and infrared test respectively, and the results are shown in FIGS. 8 and 9 respectively, and as can be seen from the electron microscope images, most of the activated carbon added with the sensitization control reagent is spheroidized, but the spheroidization effect is deteriorated due to too long microwave time, so that the microwave time is preferably 1-2.5min, the BET specific surface area is 1,174.1179 m/g, and the pore volume is 0.1425 cm/g.
Example 5
(1) Preparing a sensitization control reagent: adding 10L of distilled water, 12g of soluble organic benzoic acid and 40 g of metal ion salt aluminum nitrate, dropwise adding 10mL of tetrabutyl titanate solution and 8mL of acetic acid under stirring, and uniformly mixing to obtain a sensitizer;
(2) 100g of activated carbon and 200mL of sensitizer are mixed, a household microwave oven is used for medium fire, the microwave time is 2.5min, electron microscopy, infrared and adsorption tests are respectively carried out, and the results are respectively shown in FIGS. 10, 11 and 12.
Claims (8)
1. A preparation method of micron spherical activated carbon is characterized in that the activated carbon is mixed with a sensitizing agent to react under the microwave condition, the sensitizing agent is used for controlling the microwave to act on the surface action site of the activated carbon, and the micron spherical activated carbon is prepared, wherein the sensitizing agent comprises acetic acid, tetrabutyl titanate solution, soluble organic matters and metal ion salts.
2. The method for preparing micron spherical activated carbon according to claim 1, wherein the soluble organic substance is any one or more of polyethylene glycol, sodium polyacrylate, ethanol, or benzoic acid.
3. The method for preparing micron spherical activated carbon according to claim 1 or 2, wherein the metal ion salt is any one of magnesium nitrate, ferric nitrate, or aluminum nitrate.
4. The method for preparing micron spherical activated carbon according to claim 1 or 2, wherein the sensitizer is prepared by dissolving an organic substance and a metal ion salt in a mass ratio of 4-18:10-50 in distilled water, dropwise adding a solution of acetic acid and tetrabutyl titanate, and uniformly mixing.
5. The method for preparing micron spherical activated carbon according to claim 1 or 2, wherein the sensitizer is prepared by adding 4-18g of organic matter and 10-50g of metal ion salt into 10L of distilled water, then adding 10mL of tetrabutyl titanate solution and 5-8mL of acetic acid dropwise, and mixing uniformly.
6. The method as claimed in claim 1 or 2, wherein the microwave power is 700-750 w.
7. The method for preparing micron spherical activated carbon according to claim 1 or 2, wherein the activated carbon and the sensitizer are mixed under microwave condition for reaction time of 1-2.5 min.
8. The method as claimed in claim 1 or 2, wherein the sensitizer is mixed with 200mL of 100-200 g of activated carbon.
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| CN114345318A (en) * | 2021-12-03 | 2022-04-15 | 中北大学 | graphene-SrTiO3Material and method for the production thereof |
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