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CN112705166A - Preparation method and application of ammonia water modified eucalyptus activated carbon adsorbent - Google Patents

Preparation method and application of ammonia water modified eucalyptus activated carbon adsorbent Download PDF

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Publication number
CN112705166A
CN112705166A CN202110009900.2A CN202110009900A CN112705166A CN 112705166 A CN112705166 A CN 112705166A CN 202110009900 A CN202110009900 A CN 202110009900A CN 112705166 A CN112705166 A CN 112705166A
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China
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eucalyptus
activated carbon
ammonia water
drying
carbon adsorbent
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Inventor
卢泽
曾惠婷
张康
石清亮
张华�
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Guilin University of Technology
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Guilin University of Technology
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Priority to CN202110009900.2A priority Critical patent/CN112705166A/en
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Priority to GB2314967.7A priority patent/GB2620507A/en
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Abstract

The invention discloses a preparation method and application of an ammonia water modified eucalyptus activated carbon adsorbent. Soaking eucalyptus powder in a phosphoric acid solution, and putting the soaked eucalyptus powder in a muffle furnace for high-temperature pyrolysis, cooling and washing; filtering, drying, grinding and sieving to obtain eucalyptus activated carbon; putting the obtained eucalyptus activated carbon into ethylene glycol, performing ultrasonic treatment, adding ammonia water, performing magnetic stirring, putting the obtained uniform mixed solution into a reaction kettle, drying, cooling and washing; filtering, drying, grinding and sieving to obtain the ammonia water modified eucalyptus activated carbon adsorbent. The invention firstly adopts a phosphoric acid activation method to prepare the active carbon, and then carries out ammonia water modification, the process flow is simple, and the conditions are easy to implement; compared with the original activated carbon, the compound eucalyptus activated carbon loaded with the amino can greatly enhance the capability of removing Cr (VI) in an aqueous solution through electrostatic adsorption, hydrogen bond action and redox action; the prepared adsorbent can be widely applied to the treatment process of wastewater containing Cr (VI) in industrial and mining enterprises.

Description

Preparation method and application of ammonia water modified eucalyptus activated carbon adsorbent
Technical Field
The invention relates to a preparation method and application of an ammonia water modified eucalyptus activated carbon adsorbent. Belonging to the field of material preparation and water treatment.
Background
With the rapid development of industrial activities, industrial waste water containing heavy metals in large quantities is discharged into the environment, causing serious environmental problems due to its non-biodegradable nature and potential carcinogenicity. Among them, chromium contained in industrial wastewater is a major toxic pollutant. Trace amounts of chromium can cause severe physiological or neurological damage. Chromium exists mainly in two valence states of Cr (III) and Cr (VI), and Cr (VI) substances have much more harm than Cr (III) substances due to high toxicity and high mobility. At present, various conventional or modern techniques have been used for treating heavy metal wastewater containing Cr (VI), including reduction, ion exchange, reverse osmosis, membrane separation, electrocoagulation and adsorption. Among these methods, the adsorption method is considered to be a low-cost and high-efficiency method for treating low-concentration heavy metal contaminated water.
The eucalyptus is rich in cellulose, hemicellulose and lignin, can generate a porous structure after pyrolysis, is beneficial to adsorbing and removing Cr (VI) in water, has short growth period and can effectively reduce the production cost when being used as a raw material for preparing the active carbon.
The activated carbon produced by thermo-chemical cracking of eucalyptus under oxygen-free conditions has the characteristics of porous structure, surface area, surface functional groups, mineral components and the like, and is an adsorbent suitable for removing pollutants in aqueous solution. The advantages of environmental protection, economy and high efficiency are receiving more and more attention. However, compared with modified composite activated carbon, the original activated carbon has smaller specific surface area, fewer functional groups and limited pollutant adsorption capacity. In order to improve the adsorption capacity of the activated carbon, a modification method for modifying the activated carbon by ammonia water is selected. In recent years, many researchers have used amino-loaded composites to improve the adsorption of metal ions by adsorbents. Under the acidic condition, the amino is easy to protonate to form a positive charge group, and the zero charge point of the composite material is improved. The removal rate of Cr (VI) in the aqueous solution can be improved through electrostatic adsorption, oxidation reduction and hydrogen bonding of amino groups and Cr (VI) ions. Therefore, how to load amino groups on activated carbon for modification in order to improve the adsorption capacity of activated carbon is a hot problem of current research. Therefore, the ammonia water modified eucalyptus activated carbon adsorbent prepared by taking the eucalyptus as the main raw material and the application thereof have favorable development prospects.
Disclosure of Invention
The invention aims to solve the problem that the original activated carbon has a limited effect of removing Cr (VI) in an aqueous solution, and provides an ammonia water modified eucalyptus activated carbon adsorbent which is prepared by preparing eucalyptus activated carbon by a phosphoric acid activation method, modifying the eucalyptus activated carbon by ammonia water to load amino groups on the surface of the activated carbon, so that the adsorption capacity of Cr (VI) is improved.
Currently, the adsorption materials widely used for adsorbing chromium include natural adsorbents (zeolite, clay, peat, coal ash, etc.), synthetic carbon-based adsorbents (activated carbon, biochar, peat carbon, carbon nanotubes, graphene oxide, etc.), and metal-based adsorbents (nano zero-valent iron, metal oxide nanomaterials, etc.). The main components exerting the adsorption effect in the materials are single. In order to solve the defects of low adsorption capacity and limited adsorption capacity of the current adsorbent and fully utilize rich forestry resources in Guangxi, namely eucalyptus resources, the invention provides a preparation method of an adsorption material with high adsorption capacity on chromium, namely an ammonia water modified eucalyptus activated carbon adsorbent. The ammonia water modified eucalyptus activated carbon adsorbent prepared by the method has the specific surface area of 1654.38m2And/g, adsorbing the Cr (VI) solution with the initial concentration of 300mg/L under the condition of pH 2, wherein the equilibrium adsorption amount is 260mg/g, and the removal rate of the Cr (VI) solution reaches 85.67%.
The method comprises the following specific steps:
(1) sawing the eucalyptus into blocks, cutting into slices, cleaning, drying, placing into a pulverizer, pulverizing, and sieving with a 30-mesh sieve to obtain eucalyptus powder for later use.
(2) Weighing 10g of the eucalyptus powder obtained in the step (1), soaking in 40mL of phosphoric acid solution with the mass percentage concentration of 40%, and soaking for 8-10 h at room temperature.
(3) And (3) placing the soaked eucalyptus powder obtained in the step (2) into a 200mL crucible, placing the crucible into a muffle furnace, and pyrolyzing the eucalyptus powder for 1-2 h at 500-600 ℃, wherein the heating rate is 10 ℃/min.
(4) And (4) cooling the product obtained in the step (3) to room temperature, washing with deionized water, placing in a 100mL centrifuge tube for solid-liquid separation, pouring off the supernatant, repeating the above operations until the pH value of the filtrate is neutral and stable, and filtering.
(5) And (3) placing the product obtained in the step (4) in a culture dish, drying the product in an oven at the temperature of 60-80 ℃ for 18-24 hours, grinding the product and sieving the product with a 200-mesh sieve to obtain the eucalyptus activated carbon.
(6) And (3) adding 0.5g of the eucalyptus activated carbon obtained in the step (5) into a 100mL beaker, adding 60mL of ethylene glycol, placing the mixture into an ultrasonic cleaner for ultrasonic treatment for 20-30 min, adding 20-30 mL of ammonia water, placing the mixture into a magnetic stirrer for stirring (1100rpm) for 30-45 min, placing the obtained uniform mixed solution into a 100mL reaction kettle with a polytetrafluoroethylene lining, and placing the reaction kettle into an air-blowing drying oven for reaction for 10-12 h at 200 ℃.
(7) And (4) naturally cooling the product obtained in the step (6), washing with deionized water, placing into a 100mL centrifuge tube for solid-liquid separation, pouring out the supernatant, repeating the above operations until the pH value of the filtrate is neutral and stable, and filtering.
(8) And (3) placing the product obtained in the step (7) in a culture dish, drying for 18-24 h at the temperature of 60-80 ℃, and sieving with a 200-mesh sieve to obtain the ammonia water modified eucalyptus activated carbon adsorbent.
(9) The prepared ammonia water modified eucalyptus activated carbon adsorbent is applied to adsorption removal of Cr (VI) in an aqueous solution.
The eucalyptus is used as a main raw material, so that the production cost is reduced; the activated carbon is prepared by adopting a phosphoric acid activation method, and then ammonia water is modified, so that the process flow is simple, and the conditions are easy to implement; compared with the original activated carbon, the compound eucalyptus activated carbon loaded with the amino can greatly enhance the adsorption capacity to Cr (VI) in an aqueous solution through electrostatic adsorption, hydrogen bond action and redox action; the prepared adsorbent can be widely applied to the treatment process of wastewater containing Cr (VI) in industrial and mining enterprises.
Description of the drawings:
FIG. 1 is SEM comparison spectra of eucalyptus activated carbon before and after modification at 5000 times prepared by the embodiment of the invention.
FIG. 2 is a FT-IR comparison spectrum of adsorption of Cr (VI) by eucalyptus activated carbon and ammonia water modified eucalyptus activated carbon adsorbent before and after modification according to the embodiment of the present invention.
Fig. 3 is an XPS comparison graph of adsorption of cr (vi) by eucalyptus activated carbon and ammonia water modified eucalyptus activated carbon adsorbent before and after modification according to the embodiment of the present invention.
Fig. 4 is a graph comparing changes of adsorption amounts of cr (vi) in a solution of eucalyptus activated carbon before and after modification according to an embodiment of the present invention under different pH conditions.
Fig. 5 is a graph comparing changes of adsorption amount and removal rate of cr (vi) in a solution of eucalyptus activated carbon before and after modification according to an embodiment of the present invention under different adsorbent amounts.
Fig. 6 is a graph comparing changes of adsorption amount and removal rate of cr (vi) in a solution of eucalyptus activated carbon before and after modification according to an embodiment of the present invention.
Fig. 7 is a comparison graph of changes of adsorption amounts of cr (vi) in solutions of eucalyptus activated carbon before and after modification according to an embodiment of the present invention under different solution concentrations and temperature conditions.
Detailed Description
Example (b):
(1) sawing the eucalyptus into blocks, cutting into slices, cleaning, drying, placing into a pulverizer, pulverizing, and sieving with a 30-mesh sieve to obtain eucalyptus powder for later use.
(2) Weighing 10g of the eucalyptus powder obtained in the step (1), soaking in 40mL of phosphoric acid solution with the mass percentage concentration of 40%, and soaking for 10h at room temperature.
(3) And (3) placing the soaked eucalyptus powder obtained in the step (2) into a 200mL crucible, placing the crucible into a muffle furnace, and pyrolyzing the eucalyptus powder for 1h at 500 ℃ at a heating rate of 10 ℃/min.
(4) And (4) cooling the product obtained in the step (3) to room temperature, washing with deionized water, placing in a 100mL centrifuge tube for solid-liquid separation, pouring off the supernatant, repeating the above operations until the pH value of the filtrate is neutral and stable, and filtering.
(5) And (4) placing the product obtained in the step (4) in a culture dish, drying in an oven at 60 ℃ for 24 hours, grinding and sieving by a 200-mesh sieve to obtain the eucalyptus activated carbon.
(6) And (3) adding 0.5g of the eucalyptus activated carbon obtained in the step (5) into a 100mL beaker, adding 60mL of ethylene glycol, placing the mixture into an ultrasonic cleaner for ultrasonic treatment for 20min, adding 20mL of ammonia water, placing the mixture into a magnetic stirrer for stirring (1100rpm) for 30min, placing the obtained uniform mixed solution into a 100mL reaction kettle with a polytetrafluoroethylene lining, and placing the reaction kettle in an air-blowing drying oven for reaction for 10h at the temperature of 200 ℃.
(7) And (4) naturally cooling the product obtained in the step (6), washing with deionized water, placing into a 100mL centrifuge tube for solid-liquid separation, pouring out the supernatant, repeating the above operations until the pH value of the filtrate is neutral and stable, and filtering.
(8) And (4) placing the product obtained in the step (7) in a culture dish, drying for 24 hours at the temperature of 60 ℃, and sieving with a 200-mesh sieve to obtain the ammonia water modified eucalyptus activated carbon adsorbent.
(9) The ammonia water modified eucalyptus activated carbon adsorbent prepared in the embodiment is applied to adsorption removal of Cr (VI) in an aqueous solution.
(10) Weighing a certain amount of the eucalyptus activated carbon prepared in the embodiment before and after modification into a 100mL centrifuge tube, adding 25mL of Cr (VI) solution with a certain concentration and a certain pH into the centrifuge tube by using a 25mL pipette, placing the centrifuge tube into a gas bath oscillator, oscillating and mixing for a certain time at a certain temperature and at a rotating speed of 200r/min, filtering by using a 0.45-micrometer filter membrane, and measuring the residual concentration of Cr (VI) by using a spectrophotometer to investigate the change of the adsorption capacity of the eucalyptus activated carbon before and after ammonia water modification and the influence of different conditions on the adsorption capacity. The results are shown in FIGS. 4, 5, 6 and 7. It can be seen that when 25mL of 300mg/L Cr (VI) solution is treated with 0.025g of adsorbent under the condition of pH 3, the ammonia water modified eucalyptus activated carbon prepared in this example reaches adsorption equilibrium after about 720min, and the temperature rise promotes the removal of Cr (VI) to some extent. Compared with the original activated carbon, the ammonia water modified eucalyptus activated carbon has obviously improved Cr (VI) removal capability.
Analyzing the surface morphology of the ammonia water modified eucalyptus activated carbon adsorbent by adopting a novel thermal field emission scanning electron microscope (SEM, SU5000, Hitachi, Japan), and obtaining a result shown in figure 1; the phase structure and elemental composition were measured using a FT-IR Fourier Infrared Spectroscopy, model 470FTIR from Thermometer, Inc. and an X-ray diffractometer, model ESCALAB 250Xi, from Thermometer, Inc. and the results are shown in FIGS. 2 and 3.

Claims (2)

1.一种氨水改性桉木活性炭吸附剂的制备方法，其特征在于具体步骤为：1. a preparation method of ammonia water modified eucalyptus activated carbon adsorbent, is characterized in that concrete steps are: (1)将桉木锯成块，切成薄片，清洗并干燥后，置于粉碎机中粉碎并过30目筛，得到桉木粉末备用；(1) sawing eucalyptus into pieces, cut into slices, after cleaning and drying, place pulverizer and pulverize and cross 30 mesh sieves to obtain eucalyptus powder for subsequent use; (2)称取10g步骤(1)所得桉木粉末浸泡于40mL的质量百分比浓度为40％的磷酸溶液中，室温条件下浸泡8～10h；(2) Weigh 10 g of the eucalyptus powder obtained in step (1) and soak it in 40 mL of phosphoric acid solution with a mass percentage concentration of 40%, and soak for 8-10 hours at room temperature; (3)将步骤(2)所得的浸泡后的桉木粉末放置于200mL坩埚中，置于马弗炉内，在500℃～600℃条件下热解1～2h，升温速率为10℃/min；(3) Place the soaked eucalyptus wood powder obtained in step (2) in a 200 mL crucible, put it in a muffle furnace, and pyrolyze it at 500°C to 600°C for 1 to 2 hours, with a heating rate of 10°C/min ; (4)将步骤(3)所得产物冷却至室温，采用去离子水洗涤，并置于100mL的离心管中进行固液分离，倒掉上清液，重复以上操作，直到滤液的pH值在中性稳定，过滤；(4) The product obtained in step (3) was cooled to room temperature, washed with deionized water, and placed in a 100 mL centrifuge tube for solid-liquid separation, poured off the supernatant, and repeated the above operations until the pH value of the filtrate was in the middle Sexual stability, filtration; (5)将步骤(4)所得产物置于培养皿中，放在60℃～80℃的烘箱中烘18～24h，然后研磨并过200目筛，获得桉木活性炭；(5) placing the product obtained in step (4) in a petri dish, drying it in an oven at 60°C to 80°C for 18 to 24 hours, then grinding and passing through a 200-mesh sieve to obtain eucalyptus activated carbon; (6)于100mL烧杯中加入0.5g步骤(5)所得桉木活性炭，再加入60mL乙二醇，置于超声波清洗器中超声20～30min后，再加入20～30mL氨水，置于100rpm磁力搅拌器中搅拌30～45min，所得均一的混合液装入到100mL聚四氟乙烯内衬的反应釜中，置于鼓风干燥箱中200℃条件下反应10～12h；(6) Add 0.5 g of eucalyptus activated carbon obtained in step (5) into a 100 mL beaker, then add 60 mL of ethylene glycol, place it in an ultrasonic cleaner for 20 to 30 minutes, then add 20 to 30 mL of ammonia water, and place it under 100 rpm magnetic stirring Stir in the vessel for 30-45min, the obtained homogeneous mixed solution is charged into a 100mL polytetrafluoroethylene-lined reaction kettle, and placed in a blast drying oven for 10-12h at 200°C; (7)将步骤(6)所得产物自然冷却，采用去离子水洗涤，并置于100mL的离心管中进行固液分离，倒掉上清液，重复以上操作，直到滤液的pH值在中性稳定，过滤；(7) Naturally cooling the product obtained in step (6), washing with deionized water, and placing it in a 100 mL centrifuge tube for solid-liquid separation, pouring off the supernatant, and repeating the above operations until the pH value of the filtrate is neutral stabilize, filter; (8)将步骤(7)所得产物置于培养皿中，在60℃～80℃条件下干燥18～24h，过200目筛，得到氨水改性桉木活性炭吸附剂。(8) The product obtained in step (7) is placed in a petri dish, dried at 60°C to 80°C for 18 to 24 hours, and passed through a 200-mesh sieve to obtain an ammonia-modified eucalyptus activated carbon adsorbent. 2.一种如权利要求1所述的氨水改性桉木活性炭吸附剂的应用，其特征在于，所述氨水改性桉木活性炭吸附剂应用于对水中Cr(VI)的吸附去除。2 . An application of the ammonia-modified eucalyptus activated carbon adsorbent according to claim 1 , wherein the ammonia-modified eucalyptus activated carbon adsorbent is applied to the adsorption and removal of Cr(VI) in water. 3 .
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