CN116143116A - Method for preparing antibacterial active carbon by using distilled grains - Google Patents

Method for preparing antibacterial active carbon by using distilled grains Download PDF

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CN116143116A
CN116143116A CN202310183594.3A CN202310183594A CN116143116A CN 116143116 A CN116143116 A CN 116143116A CN 202310183594 A CN202310183594 A CN 202310183594A CN 116143116 A CN116143116 A CN 116143116A
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zinc
active carbon
drying
activated carbon
vinasse
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肖伽励
周龙生
邹伟超
曹贵华
刘东帆
刘慧文
王道亮
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Yangzhou Polytechnic Institute
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    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
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    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
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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
    • C01B32/318—Preparation characterised by the starting materials
    • C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01B32/00—Carbon; Compounds thereof
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    • C01B32/312—Preparation
    • C01B32/342—Preparation characterised by non-gaseous activating agents
    • C—CHEMISTRY; METALLURGY
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Abstract

The invention relates to a method for preparing antibacterial active carbon by using vinasse, which adopts vinasse as a raw material, performs predrying under the low-temperature condition by utilizing microwaves, then performs soaking by utilizing a certain amount of aqueous solution of urea, zinc chloride and water compound activator, performs activation under the specific activation temperature condition, and finally performs washing and drying to prepare the active carbon with antibacterial function, and has the advantages of rich pore structure, large specific surface area, strong iodine adsorption capacity, high yield and the like. The preparation method has the characteristics of low energy consumption and simple operation, the preparation cost of the antibacterial active carbon adsorbent prepared from the vinasse is reduced, the preparation flow in the conventional process is optimized, the prepared adsorbent has a rich pore structure and large specific surface area, the adsorption performance is effectively improved, and meanwhile, the antibacterial active carbon adsorbent also has certain antibacterial property. Therefore, the preparation method is suitable for wide application, can be better used as an adsorbent for wastewater treatment, gas purification technology and energy storage, and realizes treatment of waste by waste and resource utilization.

Description

Method for preparing antibacterial active carbon by using distilled grains
Technical Field
The invention relates to the field of active carbon preparation, in particular to a method for preparing antibacterial active carbon by using distilled grains.
Background
Distiller's grains are the main waste of the white spirit brewing industry. In 2019 only, the yield of Chinese white spirit reaches 785.9 kiloliters, and about 2400 kilotons of vinasse is generated accordingly. The method is used as a feed, which is the most main utilization mode of the prior distiller's grains, but has limited application and limited consumption capability due to high rice hull content, poor feeding performance and low nutritive value in the multi-grain distiller's grains, so that the need for efficient utilization of multi-grain distiller's grains resources is very important.
The distilled grains can be used for preparing the activated carbon with large specific surface area, stable physicochemical property and excellent adsorption capacity simply through the pyrolysis process. Activated carbon is widely used as an adsorption material in the purification of air and water, and is widely used not only in industry but also in civil products. However, due to the good adsorption performance and the capability of capturing water (vapor), the activated carbon is very easy to become a place for mass propagation of bacterial viruses, thereby affecting the normal use of the activated carbon and even generating peculiar smell. Therefore, the preparation of the antibacterial activated carbon is particularly important.
Inorganic antibacterial materials are currently an important point of research in antibacterial materials, wherein zinc ions are inferior to silver ions in antibacterial ability, and are inexpensive and safe, and are widely used as antibacterial agents. Inorganic antibacterial materials are loaded on the activated carbon in a dipping and drying mode, so that an antibacterial effect is achieved, and the method for preparing the antibacterial activated carbon is common. However, the post-impregnation method not only increases the process steps for preparing the antibacterial active carbon, but also has the more important effect that antibacterial materials are distributed in the pore channels of the active carbon in the impregnation process, and micropores and even mesopores of the active carbon are blocked, so that the adsorption quantity and the adsorption rate of the active carbon are reduced.
Disclosure of Invention
Aiming at the defects in the prior art, the invention prepares the high specific area activated carbon with antibacterial effect based on the waste distillers' grains as raw materials and by combining zinc ions, thereby realizing the recycling of resources.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method for preparing antibacterial active carbon by using distilled grains comprises the following steps:
s1, preparing raw materials: drying, crushing and sieving the vinasse to obtain vinasse particles; dissolving a zinc-containing inorganic compound and urea in water to obtain a mixed solution;
s2, zinc carrying treatment: mixing the vinasse particles obtained in the step S1 with the mixed solution according to the mass-volume ratio of 1:2kg/L, uniformly stirring, and carrying out ultrasonic treatment and soaking for a period of time under certain conditions to obtain a zinc-carrying material;
s3, pre-drying: placing the zinc-carrying material into a crawler-type microwave drying oven, and drying for a period of time at 80-150 ℃;
s4, high-temperature activation: putting the product prepared in the step S3 into an atmosphere furnace with a certain temperature, activating in nitrogen atmosphere for a certain time, and cooling to obtain a crude product;
s5, a finished product: and (3) carrying out acid washing, water washing and drying on the crude product obtained in the step S4 to obtain the target activated carbon product.
Further, the concentration of the zinc-containing inorganic compound and the concentration of the urea in the mixed solution are respectively 0.5-5 mol/L and 1-9 mol/L; the zinc-containing inorganic compound is zinc chloride or zinc nitrate.
Further, in the step S2, the ultrasonic power is 1000-13000W, the ultrasonic time is 10-40 min, and the soaking time is 6-24 h.
Further, in the step S3, the pre-dried product is dried until the water content is 5-15%.
Further, in the step S4, the activation temperature is 400-500 ℃ and the activation time is 0.5-4 h.
The invention adopts vinasse as a raw material, performs predrying under the low-temperature condition by utilizing microwaves, then performs soaking by utilizing a certain amount of aqueous solution of urea, zinc chloride and water compound activator, performs activation under the specific activation temperature condition, and finally performs washing and drying to prepare the active carbon with antibacterial function, and has the advantages of rich pore structure, large specific surface area, strong iodine adsorption capacity, high yield and the like. The invention immerses the lees particles in a certain amount of modified aqueous solution (composed of zinc chloride or zinc nitrate, urea and water) at normal temperature, so that the pore structure and specific surface area of the carbonized activated carbon particles can be well enhanced, ash content can be reduced, and energy consumption is reduced; but also is beneficial to the formation of multiple holes and the generation of volatile tar; uniformly loading ZnO bacteriostat with nanometer size.
And secondly, in the carbonization process, volatile substances and extractable organic compounds can be removed by adopting microwave low-temperature treatment, the aromaticity and condensed carbon of the material can be improved, the microstructure of a carbon matrix is optimized, and a foundation is laid for the porous structure of the activated carbon in the chemical activation step. With a specific activation temperature and activation time, basic zinc carbonate generates CO at the activation temperature 2 And H 2 O and NH 3 The former two develop microporous and mesoporous structures, while NH 3 The generation of alkaline functional groups on the surface of the activated carbon is facilitated; further controlling the micropore and mesopore structure of the active carbon and the size of ZnO.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method has the characteristics of low energy consumption and simple operation, the preparation cost of the antibacterial active carbon adsorbent prepared from the vinasse is reduced, the preparation flow in the conventional process is optimized, the prepared adsorbent has a rich pore structure and large specific surface area, the adsorption performance is effectively improved, and meanwhile, the antibacterial active carbon adsorbent also has certain antibacterial property. Therefore, the preparation method is suitable for wide application, can be better used as an adsorbent for wastewater treatment, gas purification technology and energy storage, and realizes treatment of waste by waste and resource utilization.
Drawings
Fig. 1 is an SEM image of the activated carbon product prepared in example 1.
FIG. 2 is an EDS diagram of the activated carbon product made in example 1.
FIG. 3 is N of the activated carbon product obtained in example 1 2 -adsorption-desorption isotherm plot (a) and pore size profile (b).
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In addition, the technical features of the different embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
The experimental methods used in the embodiment of the invention are conventional methods unless otherwise specified.
Materials, reagents, and the like used in the examples of the present invention are commercially available unless otherwise specified.
Example 1
S1, preparing raw materials: firstly, washing and cleaning distilled grains with water, and drying the distilled grains until the water content is 10% -20% and the drying temperature is 105+/-5 ℃; grinding the dried product, and sieving with 100-200 mesh sieve to obtain distiller grains;
dissolving urea and zinc chloride in water to obtain a mixed solution, wherein the concentration of the zinc chloride is 3.0mol/L and the concentration of the urea is 9.0mol/L;
s2, zinc carrying treatment: mixing the particles obtained in the step S1 with a mixed solution, wherein the mass volume ratio kg/L of the aqueous solution to the distillers grains is 1:2.0, uniformly mixing and stirring, performing ultrasonic treatment at 1000W for 10min, and soaking for 24h to obtain a mixed product;
s3, pre-drying: placing the zinc-loaded raw materials into a crawler-type microwave drying oven at the thickness of 1cm, and drying at the temperature of 80 ℃ for 30min to ensure that the water content of the pre-dried product is within 10% -15%;
s4, high-temperature activation: putting the product prepared in the step S3 into an atmosphere furnace at 400 ℃, activating in nitrogen atmosphere for 4 hours, and cooling to obtain a crude product;
s5, a finished product: and (3) carrying out acid washing, water washing and drying on the crude product obtained in the step S4 to obtain the target activated carbon product.
The results showed that the activated carbon product of example 1 was 41.30% in yield. The iodine value of the product is tested according to the national standard GB/T12496.8-2015, and the iodine value is 1380mg/g.
As shown in fig. 1 and 2, the activated carbon product prepared in example 1 has a rich pore structure containing zinc atoms.
Example 2
S1, preparing raw materials: firstly, washing and cleaning distilled grains with water, and drying the distilled grains until the water content is 15% -20% and the drying temperature is 105+/-5 ℃; grinding the dried product, and sieving with 100-200 mesh sieve to obtain distiller grains;
dissolving urea and zinc chloride in water to obtain a mixed solution, wherein the concentration of the zinc chloride is 3.0mol/L and the concentration of the urea is 9.0mol/L;
s2, zinc carrying treatment: mixing the particles obtained in the step S1 with a mixed solution, wherein the mass volume ratio kg/L of the aqueous solution to the distillers grains is 1:2.0, uniformly mixing and stirring, performing ultrasonic treatment at 1500W for 10min, and soaking for 24h to obtain a mixed product;
s3, pre-drying: placing the zinc-loaded raw materials into a crawler-type microwave drying oven at the thickness of 2cm, and drying for 10min at the temperature of 150 ℃ respectively, so that the water content of the pre-dried product is within 5% -10%;
s4, high-temperature activation: putting the product prepared in the step S3 into an atmosphere furnace at 500 ℃, activating in nitrogen atmosphere for 4 hours, and cooling to obtain a crude product;
s5, a finished product: and (3) carrying out acid washing, water washing and drying on the crude product obtained in the step S4 to obtain the target activated carbon product.
The results showed that the activated carbon product of example 2 was 40.10% in yield. The iodine value of the product is measured according to the national standard GB/T12496.8-2015, and the iodine value is 1275mg/g.
Comparative example 1
The main difference between this comparative example 1 and example 1 is that no zinc chloride was added in step S2.
Comparative example 2
The main difference between this comparative example 1 and example 1 is that no pre-drying with microwaves was performed in step S3.
TABLE 1 bacteriostatic Effect of example 1 and comparative example 1
Figure BDA0004103017050000051
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Figure BDA0004103017050000061
TABLE 2 adsorption Effect of example 1 and comparative example 2
Sample of Iodine adsorption value (mg/g)
Example 1 1380
Comparative example 2 851
Although embodiments of the present invention have been disclosed above, it is not limited to the use of the description and embodiments, it is well suited to various fields of use for the invention, and further modifications may be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the particular details without departing from the general concepts defined in the claims and the equivalents thereof.

Claims (5)

1. A method for preparing antibacterial active carbon by using distilled grains is characterized by comprising the following steps:
s1, preparing raw materials: drying, crushing and sieving the vinasse to obtain vinasse particles; dissolving a zinc-containing inorganic compound and urea in water to obtain a mixed solution;
s2, zinc carrying treatment: mixing the vinasse particles obtained in the step S1 with the mixed solution according to the mass-volume ratio of 1:2kg/L, uniformly stirring, and carrying out ultrasonic treatment and soaking for a period of time under certain conditions to obtain a zinc-carrying material;
s3, pre-drying: placing the zinc-carrying material into a crawler-type microwave drying oven, and drying for a period of time at 80-150 ℃;
s4, high-temperature activation: putting the product prepared in the step S3 into an atmosphere furnace with a certain temperature, activating in nitrogen atmosphere for a certain time, and cooling to obtain a crude product;
s5, a finished product: and (3) carrying out acid washing, water washing and drying on the crude product obtained in the step S4 to obtain the target activated carbon product.
2. The method for preparing bacteriostatic activated carbon by using distillers' grains according to claim 1, wherein the concentration of the zinc-containing inorganic compound and urea in the mixed solution is 0.5-5 mol/L and 1-9 mol/L, respectively; the zinc-containing inorganic compound is zinc chloride or zinc nitrate.
3. The method for preparing antibacterial activated carbon by using distiller' S grains according to claim 1, wherein in the step S2, the ultrasonic power is 1000-13000W, the ultrasonic time is 10-40 min, and the soaking time is 6-24 h.
4. The method for preparing antibacterial activated carbon by using distiller' S grains according to claim 1, wherein in step S3, the pre-dried product is dried to have a water content of 5-15%.
5. The method for preparing antibacterial activated carbon by using distiller' S grains according to claim 1, wherein in the step S4, the activation temperature is 400-500 ℃ and the activation time is 0.5-4 h.
CN202310183594.3A 2023-03-01 2023-03-01 Method for preparing antibacterial active carbon by using distilled grains Pending CN116143116A (en)

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