CN113731361A - Preparation method of magnesium oxide loaded activated carbon - Google Patents
Preparation method of magnesium oxide loaded activated carbon Download PDFInfo
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- CN113731361A CN113731361A CN202111036202.8A CN202111036202A CN113731361A CN 113731361 A CN113731361 A CN 113731361A CN 202111036202 A CN202111036202 A CN 202111036202A CN 113731361 A CN113731361 A CN 113731361A
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- 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
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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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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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
- C01B32/312—Preparation
- C01B32/336—Preparation characterised by gaseous activating agents
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Abstract
The invention relates to the technical field of adsorption materials, and particularly relates to a preparation method of magnesium oxide loaded activated carbon. The preparation method provided by the invention adopts different coal types for mixing, and can improve the pore structure of the finally prepared product by utilizing the pore characteristics of different coal types; meanwhile, before the forming and carbonization processes, the coal and the magnesium oxide are mixed, so that the magnesium oxide is more fully loaded in the pore structure of the activated carbon in the subsequent carbonization and activation (further adjustment of the pore structure) processes of the mixture, and the decoloring effect of the activated carbon is further improved.
Description
Technical Field
The invention relates to the technical field of adsorption materials, and particularly relates to a preparation method of magnesium oxide loaded activated carbon.
Background
The magnesium oxide loaded active carbon is a composite material of magnesium oxide and active carbon, and the composite material has strong hydrophilicity, high specific surface area and strong adsorption force, so that the composite material has good application in the field of decolorization.
The preparation of the magnesium oxide loaded active carbon at present mainly comprises a solid phase method and a liquid phase method; the liquid phase method is obtained by impregnating activated carbon in a magnesium-containing solution and then carrying out anaerobic roasting, but the method has the advantages of load, harsh required conditions and limited improvement of the decolorizing capacity of the prepared final product; the solid phase method mainly comprises the step of directly and mechanically mixing activated carbon and magnesium oxide, but the method is simple, but the method cannot effectively load the magnesium oxide on the activated carbon, cannot control the content of the magnesium oxide in the activated carbon, and needs higher content of the magnesium oxide in order to obtain better decolorizing effect.
Disclosure of Invention
The invention aims to provide a preparation method of magnesium oxide loaded activated carbon, which can ensure that the magnesium oxide has a good decolorization effect when the dosage of the magnesium oxide is less than 2.5 wt% of coal.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of magnesium oxide loaded activated carbon, which comprises the following steps:
mixing coal and magnesium oxide to obtain a mixture; the coal comprises Shaanxi clean coal and Datong coal; the Shaanxi clean coal has the water content of less than 10 wt%, the ash content of less than 3 wt% and the volatile component of less than 35 wt%; the moisture content of the Dagong coal is less than 10 wt%, the ash content is less than 4 wt%, and the volatile component is less than 32 wt%; the magnesium oxide accounts for 2-2.5% of the coal by mass;
and sequentially molding, crushing, carbonizing and activating the mixture to obtain the magnesium oxide loaded active carbon.
Preferably, the mass ratio of the Shaanxi clean coal to the Datong coal is (7.5-8.5): (2.5-1.5).
Preferably, the mixing mode is grinding;
the rotation speed of the grinding is 1000-1500 rpm, and the time is 35-40 min.
Preferably, the molding pressure is 20-50 MPa.
Preferably, the carbonization is performed in a carbonization converter;
the temperature of the furnace end of the carbonization converter is 500-550 ℃, the temperature of the furnace is 400-450 ℃, and the temperature of the furnace tail is 220-280 ℃; the rotating speed of the carbonization converter is 1-3 rpm; the carbonization time is 30-60 min; and the moving speed of the crushed material in the carbonization converter is 0.3-0.6 m/min.
Preferably, the activating agent used for the activation comprises water vapor and/or air.
Preferably, the activation temperature is 830-960 ℃, and the activation time is 200 min.
The invention provides a preparation method of magnesium oxide loaded activated carbon, which comprises the following steps: mixing coal and magnesium oxide to obtain a mixture; the coal comprises Shaanxi clean coal and Datong coal; the Shaanxi clean coal has the water content of less than 10 wt%, the ash content of less than 3 wt% and the volatile component of less than 35 wt%; the moisture content of the Dagong coal is less than 10 wt%, the ash content is less than 4 wt%, and the volatile component is less than 32 wt%; the magnesium oxide accounts for 2-2.5% of the coal by mass; and sequentially molding, crushing, carbonizing and activating the mixture to obtain the magnesium oxide loaded active carbon. The invention adopts different coal types for mixing, and can improve the pore structure of the finally prepared product by utilizing the pore characteristics of different coal types; meanwhile, before the forming and carbonization processes, the coal and the magnesium oxide are mixed, so that the magnesium oxide is more fully loaded in the pore structure of the activated carbon in the subsequent carbonization and activation (further adjustment of the pore structure) processes of the mixture, and the decoloring effect of the activated carbon is further improved.
Detailed Description
The invention provides a preparation method of magnesium oxide loaded activated carbon, which comprises the following steps:
mixing coal and magnesium oxide to obtain a mixture; the coal comprises Shaanxi clean coal and Datong coal; the Shaanxi clean coal has the water content of less than 10 wt%, the ash content of less than 3 wt% and the volatile component of less than 35 wt%; the moisture content of the Dagong coal is less than 10 wt%, the ash content is less than 4 wt%, and the volatile component is less than 32 wt%; the magnesium oxide accounts for 2-2.5% of the coal by mass;
and sequentially molding, crushing, carbonizing and activating the mixture to obtain the magnesium oxide loaded active carbon.
In the present invention, all the starting materials for the preparation are commercially available products known to those skilled in the art unless otherwise specified.
Mixing coal and magnesium oxide to obtain a mixture; the coal comprises Shaanxi clean coal and Datong coal; the Shaanxi clean coal has the water content of less than 10 wt%, the ash content of less than 3 wt% and the volatile component of less than 35 wt%; the moisture content of the Dagong coal is less than 10 wt%, the ash content is less than 4 wt%, and the volatile component is less than 32 wt%; the magnesium oxide accounts for 2-2.5% of the coal by mass.
In the invention, the mass ratio of the Shaanxi clean coal to the Dayung coal is preferably (7.5-8.5) - (2.5-1.5), and more preferably 8: 2.
In the present invention, the purity of the magnesium oxide is preferably > 98%, and the magnesium oxide preferably passes through a 100 mesh sieve with a passing rate of 98%; the loading density of the magnesium oxide is preferably <1200 kg/L.
In the invention, the magnesium oxide accounts for 2-2.5% of the coal by mass, preferably 2.1-2.4% of the coal by mass, and more preferably 2.2-2.3% of the coal by mass.
In the present invention, the mixing is preferably performed by grinding; the rotation speed of the grinding is preferably 1000-1500 rpm, more preferably 1100-1400 rpm, and most preferably 1200-1300 rpm; the grinding time is preferably 35-40 min.
In the invention, the volatile content of the mixture is preferably less than 35 wt%, the moisture is preferably 5-7 wt%, and the fineness is preferably 88-92%.
In the invention, the mixture preferably has a passing rate of more than or equal to 90 percent when passing through a 325-mesh sieve.
After the mixture is obtained, the mixture is sequentially subjected to forming, crushing, carbonization and activation to obtain the magnesium oxide loaded activated carbon.
Before forming, the invention also preferably comprises degassing the mixture, wherein the degassing preferably comprises stirring degassing and vacuum degassing which are sequentially carried out. The stirring degassing and vacuum degassing processes are not particularly limited in the present invention, and may be performed by processes well known to those skilled in the art. In the present invention, the degassing is preferably performed in a degassing tank.
In the invention, the molding pressure is preferably 20-50 MPa, and more preferably 30-40 MPa; the time is preferably 40-50 min.
The process of the present invention is not particularly limited, and may be carried out by a process known to those skilled in the art. In the invention, the grain diameter of the irregular material obtained after crushing is preferably 2.0-4.75 mm, and the strength is preferably 90-95 MPa, and more preferably 92 MPa.
In the present invention, the carbonization is preferably performed in a carbonization converter; the furnace end temperature of the carbonization converter is preferably 500-550 ℃, more preferably 510-540 ℃, and most preferably 520-530 ℃; the temperature in the furnace is preferably 400-450 ℃, more preferably 410-440 ℃, and most preferably 420-430 ℃; the temperature of the furnace tail is preferably 220-280 ℃, more preferably 230-270 ℃ and most preferably 240-260 ℃; the rotation speed of the carbonization converter is preferably 1-3 rpm, and more preferably 2 rpm; the carbonization time is preferably 30-60 min, and more preferably 40-50 min; the moving speed of the material obtained after crushing in the carbonization converter is preferably 0.3-0.6 m/min, and more preferably 0.4-0.5 m/min.
In the invention, the temperature setting of the furnace head, the furnace and the furnace tail is beneficial to the stable quality of the produced materials.
In the invention, the carbonization process is preferably to convey the mixture obtained after crushing to a distribution section with a spiral plate, the mixture uniformly enters a grid plate section filled with lattices under the guide of the spiral plate, meanwhile, the carbonization converter rotates in an inclined manner at 3 degrees, the mixture continuously moves towards the furnace end under the rotation state by self weight, and uniformly turns over up and down on the lattice grid plate to be fully contacted with the hot flue gas (the temperature is about 550 ℃) which is reversely passed, and the mixture is heated and distilled. The obtained material is moved to the end of the carbonization furnace cylinder and then falls into a discharge port, and then is conveyed to a carbonization material tank through a scraper conveyor, and after being sprayed and cooled, subsequent activation is carried out.
In the present invention, the activating agent used for the activation preferably includes water vapor and/or air. In the invention, the activation temperature is preferably 830-960 ℃, and the activation time is preferably 200 min; in the invention, the activation preferably comprises a preheating section, a supplementary carbonization section, an activation section and a cooling section which are sequentially carried out; the temperature of the preheating section is preferably 900-50 ℃, and the time is preferably 30 min; the temperature of the supplementary carbonization section is preferably 830-840 ℃, and the time is preferably 30 min; the temperature of the activation section is preferably 950-960 ℃, and the time is preferably 120 min; the temperature of the cooling section is preferably 920-930 ℃, and the time is preferably 20 min.
In the present invention, the above-mentioned activation process is advantageous for increasing the specific surface area of the activated carbon.
In the invention, the activation process is preferably to sequentially perform the processes of a preheating section, a supplementary carbonization section, an activation section and a cooling section from top to bottom after a carbonized material obtained by carbonization enters an activation furnace, so that the carbonized material becomes an activated material with a developed pore structure and a large specific surface area, namely activated carbon. After tail gas discharged by the activation furnace enters the flue, the flue ejector brings the tail gas into the activation furnace along with steam, so that the tail gas is recycled; the residual tail gas is only water vapor and carbon dioxide, so that the tail gas is directly discharged, and the environmental pollution is avoided. In the present invention, the activation process index is preferably: the temperature of the regenerative chamber is preferably 1000-1100 ℃; the temperature of the regenerator can ensure that the temperature in the activation process is maintained in the range of 880-950 ℃, and the stability of the activation quality is ensured.
The following examples are provided to illustrate the preparation method of the magnesium oxide supported activated carbon provided by the present invention in detail, but they should not be construed as limiting the scope of the present invention.
Note: the weight parts in example 1 can be understood that the technical scheme described in example 1 is not influenced by the grade of the used amount of the raw materials, i.e. the used amount of each raw material can be 'g', 'kg' or't'.
Example 1
Mixing and grinding 7.5 parts by weight of Shaanxi clean coal (water content is 10 wt%, ash content is less than 3 wt%, and volatile matter is less than 35 wt%), 2.5 parts by weight of Datong coal (water content is less than 10 wt%, ash content is less than 4 wt%, and volatile matter is less than 32 wt%) and 0.025 parts by weight of magnesium oxide (purity is greater than 98%, passing rate of 100-mesh sieve is 98%, and loading density is less than 1200kg/L), wherein the grinding speed is 1200rpm, the grinding time is 40min, and the mixture meets the condition that the passing rate of 325-mesh sieve is greater than or equal to 90%.
And (2) after sequentially stirring, degassing and vacuum degassing the mixture, sequentially molding (the molding pressure is 36MPa and the molding time is 40min), crushing, carbonizing (the furnace head temperature of a carbonization converter is 520 ℃, the furnace temperature is 400 ℃, the furnace tail temperature is 280 ℃, the rotation speed of the carbonization converter is 3rpm, the carbonization time is 60min, the moving speed of the crushed material in the carbonization converter is 0.5m/min), activating (the temperature of a preheating section is 950 ℃, the time is 30min, the temperature of a supplementary carbonization section is 830 ℃, the time is 30min, the temperature of an activation section is 960 ℃, the time is 120min, the temperature of a cooling section is 925 ℃, the time is 20min), and screening to obtain the magnesium oxide loaded active carbon.
Example 2
8 parts by weight of Shaanxi clean coal (moisture 10 wt%, ash content less than 3 wt%, volatile component less than 35 wt%), 2 parts by weight of Daqing coal (moisture less than 10 wt%, ash content less than 4 wt%, volatile component less than 32 wt%) and 0.022 parts by weight of magnesium oxide (purity > 98%, passing rate of 100 mesh sieve 98%, loading density <1200kg/L) are mixed and ground, the grinding rotation speed is 1200rpm, the time is 40min, and a mixture is obtained, wherein the passing rate of 325 mesh sieve is more than or equal to 90%.
And (2) sequentially stirring, degassing and vacuum degassing the mixture, sequentially molding (the molding pressure is 50MPa, the molding time is 40min), crushing, carbonizing (the head temperature of a carbonization converter is 500 ℃, the temperature in the furnace is 420 ℃, the tail temperature of the furnace is 260 ℃, the rotating speed of the carbonization converter is 2rpm, the carbonizing time is 35min, the moving speed of the crushed material in the carbonization converter is 0.5m/min), activating (the temperature of a preheating section is 905 ℃, the time is 30min, the temperature of a supplementary carbonization section is 840 ℃, the time is 30min, the temperature of an activation section is 953 ℃, the time is 120min, the temperature of a cooling section is 920 ℃, the time is 20min), and screening to obtain the magnesium oxide loaded active carbon (marked as MgO8 × 16 sugar carbon).
Comparative example 1
Drying the Daqin coal with ash content of less than 3% and volatile components of 28-32 wt% by using a JLM hot air drying furnace until the water content is 4.5-6.0 wt%, grinding the Daqin coal by using a GRM vertical grinding machine, wherein the passing rate of the obtained material passing through a 325-mesh sieve is more than or equal to 90%, sequentially briquetting the obtained material (the pressing pressure is 30Mpa and the pressing time is 40min), carbonizing the obtained material (the furnace end temperature of a carbonization converter is 550 ℃, the furnace temperature is 450 ℃, the furnace tail temperature is 280 ℃, the rotating speed of the carbonization converter is 3rpm and the carbonizing time is 60min, moving the crushed material in the carbonization converter at the moving speed of 0.6m/min), activating the obtained material (the activating temperature is 920 ℃ and the activating time is 200min) and sieving the obtained activated carbon (marked as 8 × 16 ordinary carbon).
Comparative example 2
Drying the Daqin coal with ash content of less than 3% and volatile components of 28-32 wt% by using a JLM hot air drying furnace until the water content is 4.5-6.0 wt%, and grinding the Daqin coal by using a GRM vertical grinding machine to obtain powder; the material obtained by adding magnesium meets the condition that the passing rate of the material passing through a 325-mesh sieve is more than or equal to 90 percent, the obtained material is sequentially pressed into blocks (the pressing pressure is 40Mpa and the time is 40min), carbonized (the temperature of a furnace head of a carbonization converter is 550 ℃, the temperature of a furnace body is 450 ℃, the temperature of a furnace tail is 280 ℃, the rotating speed of the carbonization converter is 3rpm, the carbonization time is 60min, the moving speed of the crushed material in the carbonization converter is 0.6m/min), activated (the activation temperature is 920 ℃ and the time is 200min) and sieved, and the magnesium oxide loaded activated carbon (marked as MgO8 plus 16 Mg ordinary carbon) is obtained.
Comparative example 3
Drying the Shaanxi coal with ash content of less than 3% and volatile components of 32-35 wt% by using a JLM hot air drying furnace until the water content is 4.5-6.0 wt%, grinding the Shaanxi coal by using a GRM vertical grinding machine, wherein the passing rate of the obtained material passing through a 325-mesh sieve is more than or equal to 90%, sequentially briquetting the obtained material (the pressing pressure is 40Mpa and the pressing time is 45min), carbonizing the obtained material (the furnace end temperature of a carbonization converter is 550 ℃, the furnace temperature is 450 ℃, the furnace tail temperature is 280 ℃, the rotating speed of the carbonization converter is 3rpm and the carbonizing time is 60min, the moving speed of the crushed material in the carbonization converter is 0.6m/min), activating the obtained material (the activating temperature is 920 ℃ and the activating time is 200min) and sieving the obtained activated carbon (8 x 16 sugar carbon).
Test example
Mixing 5g of brown sugar with 100mL of water to obtain sugar liquid; 100mL of the sugar solution (pH 8.21,) was mixed with 0.1g of each of MgO8 × 16 sugar carbon prepared in example 1, 8 × 16 ordinary carbon prepared in comparative example 1, MgO8 × 16 ordinary carbon prepared in comparative example 2, and 8 × 16 sugar carbon prepared in comparative example 3, and adsorbed at a temperature of 70 ℃ for 6 hours, and the data before and after adsorption are shown in table 1:
TABLE 1 Change of sugar solution before and after adsorption
As can be seen from Table 1, the magnesium oxide loaded activated carbon prepared by the method has a good decolorizing effect.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. The preparation method of the magnesium oxide loaded activated carbon is characterized by comprising the following steps:
mixing coal and magnesium oxide to obtain a mixture; the coal comprises Shaanxi clean coal and Datong coal; the Shaanxi clean coal has the water content of less than 10 wt%, the ash content of less than 3 wt% and the volatile component of less than 35 wt%; the moisture content of the Dagong coal is less than 10 wt%, the ash content is less than 4 wt%, and the volatile component is less than 32 wt%; the magnesium oxide accounts for 2-2.5% of the coal by mass;
and sequentially molding, crushing, carbonizing and activating the mixture to obtain the magnesium oxide loaded active carbon.
2. The preparation method of claim 1, wherein the mass ratio of the Shaanxi clean coal to the Dayungke coal is (7.5-8.5): (2.5-1.5).
3. The method of claim 1, wherein the mixing is by milling;
the rotation speed of the grinding is 1000-1500 rpm, and the time is 35-40 min.
4. The method according to claim 1, wherein the molding pressure is 20 to 50 MPa.
5. The production method according to claim 1, wherein the carbonization is performed in a carbonization converter;
the temperature of the furnace end of the carbonization converter is 500-550 ℃, the temperature of the furnace is 400-450 ℃, and the temperature of the furnace tail is 220-280 ℃; the rotating speed of the carbonization converter is 1-3 rpm; the carbonization time is 30-60 min; and the moving speed of the crushed material in the carbonization converter is 0.3-0.6 m/min.
6. The method of claim 1, wherein the activating agent comprises water vapor and/or air.
7. The method of claim 1 or 6, wherein the activation temperature is 830-960 ℃ and the activation time is 200 min.
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| CN107416825A (en) * | 2017-08-31 | 2017-12-01 | 贺守印 | A kind of graininess coal mass active carbon and preparation method thereof |
| CN107416828A (en) * | 2017-08-31 | 2017-12-01 | 贺守印 | A kind of preparation method of magnesium oxide-based activated carbon |
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2021
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| Publication number | Priority date | Publication date | Assignee | Title |
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| BE843021A (en) * | 1975-06-17 | 1976-12-16 | ACTIVATED CARBON GRANULES AND THEIR PREPARATION PROCESS FROM LOWER QUALITY BITUMIOUS COAL ATTACKED BY DILUTED MINERAL ACID | |
| CN101041436A (en) * | 2007-03-09 | 2007-09-26 | 朝阳森塬活性炭有限公司 | Special activated charcoal for gasoline vapor adsorption and preparation method thereof |
| CN101717085A (en) * | 2009-12-07 | 2010-06-02 | 北京化工大学 | Activated carbon microspheres and preparation method thereof |
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