CN112156754B - Preparation method of waste sponge foam carbon-based composite adsorption material and application of waste sponge foam carbon-based composite adsorption material in adsorption removal of chromium in wastewater - Google Patents
Preparation method of waste sponge foam carbon-based composite adsorption material and application of waste sponge foam carbon-based composite adsorption material in adsorption removal of chromium in wastewater Download PDFInfo
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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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- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
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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
- B01J20/28042—Shaped bodies; Monolithic structures
- B01J20/28045—Honeycomb or cellular structures; Solid foams or sponges
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
Abstract
A preparation method of a waste sponge carbon-based composite adsorption material and application of the waste sponge carbon-based composite adsorption material in adsorption removal of chromium in wastewater relate to the technical field of waste sponge foam treatment and chromium-containing wastewater treatment. The invention takes waste sponge/foam carbon base as a main carrier material and ZnO-MoO with certain content and composition 3 MgO is used as filler to prepare the multielement composite adsorption material with excellent performance. And the adsorption performance is tested, and the modified waste sponge carbon-based adsorption material C-ZnO-MoO with excellent performance is screened out 3 MgO, and experiments prove that the modified waste sponge foam carbon-based adsorption material can be used for treating chromium-containing wastewater.
Description
Technical Field
The invention relates to the technical field of waste sponge foam treatment and chromium-containing wastewater treatment, in particular to a preparation method of a waste sponge foam carbon-based composite adsorption material and application of the adsorption material in adsorption removal of chromium in wastewater.
Background
Chromium pollution mainly comes from industrial waste water, waste gas and waste residues of chromium ore and metal smelting, electroplating, leather making and the like. Chromium is a heavy metal with high toxicity, trivalent chromium is easy to form oxide or hydroxide precipitate, the toxicity is relatively weak, and hexavalent chromium is generally considered to be 100 times more toxic than trivalent chromium. Chromium and its compounds are blacklisted as water environment priority pollutants in china due to its high toxicity. Chromium entering the human body is accumulated in human tissues and is slowly metabolized and removed. After entering blood, chromium is mainly combined with globulin, albumin and r-globulin in blood plasma. Hexavalent chromium can also permeate erythrocyte membranes, and 50% of hexavalent chromium can enter cells within 15 minutes and is combined with hemoglobin after entering the erythrocytes. Chromium metabolites are mainly excreted from the kidneys, and a small amount is excreted via the feces. Hexavalent chromium is mainly chronic toxic to humans, and it can invade the human body through the digestive tract, respiratory tract, skin and mucous membrane, accumulating in the body mainly in the liver, kidney and endocrine glands. The air entering through the respiratory tract is easily accumulated in the lungs. Hexavalent chromium has a strong oxidizing effect, so chronic poisoning gradually progresses to irrecoverable drugs from local lesions. When invading into human body through respiratory tract, it starts to invade upper respiratory tract, causing rhinitis, pharyngitis, laryngitis and bronchitis.
Excessive intake of chromium can cause poisoning. Chromium poisoning is mainly caused by the occasional inhalation of a limited amount of chromic acid or chromate, causing extensive pathologies in the kidneys, liver, nervous system and blood, leading to death. There are also cases of poisoning caused by sodium chromate absorbed by the burned wound. Prolonged occupational exposure, air pollution or exposure to chromium dust can cause skin irritation and ulceration, inflammation, necrosis of the nasal cavity and even lung cancer. When orally taken, it can cause gastrointestinal tract injury, circulatory disturbance and renal failure. The treatment method is characterized in that the turtle mixture is used for treatment after the turtle is separated from contact, and the chromium excretion amount is increased due to high sugar intake. Chromium has three compounds with valences of 2, 3 and 6. The main cause of poisoning is 6-valent chromium which has strong oxidizing property and is easy to penetrate into a biological membrane to play a role; the 2-valent and 3-valent chromium is combined with protein on the surface layer of skin to form stable complex without causing biological effect.
In recent years, with the rapid development of economy and science and technology, a carbon-based material is a non-pollution and environment-friendly adsorbent material. The composite adsorption material loaded with the adsorption modifier has rich porous structure, ultrahigh specific surface area and rich surface functional groups, and is widely applied to the fields of adsorption separation, sewage treatment, gas purification and the like. Because the unique three-dimensional structure is widely concerned at present, the composite material has a unique framework structure, a higher surface area, directional pore channel distribution and higher chemical stability. The synthesis methods of common modified composite adsorbing materials comprise a carbonization method, a physicochemical activation method, a catalytic activation method, an organogel carbonization method, a self-assembly method, a template method and the like, and the composite adsorbing materials prepared by the methods have different adsorption performances and good and uneven product quality.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a waste sponge foam carbon-based composite adsorption material and application of the waste sponge foam carbon-based composite adsorption material in adsorption removal of chromium in wastewater so as to prepare an adsorption material capable of being used for treating chromium-containing wastewater.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of a waste sponge carbon-based composite adsorption material comprises the steps of dissolving zinc salt, magnesium salt and molybdenum salt in water, adding a proper amount of dilute nitric acid, uniformly mixing, adding waste sponge carbon foam, uniformly mixing, and carrying out hydrothermal impregnation reaction in an ultrasonic reactor to prepare the waste sponge carbon-based composite adsorption material C-ZnO-MoO 3 -MgO。
As an optimal technical scheme of the preparation method of the waste sponge foam carbon-based composite adsorption material, the preparation method comprises the following specific steps:
1) Weighing zinc nitrate, magnesium oxide and ammonium molybdate, adding the zinc nitrate, the magnesium oxide and the ammonium molybdate into a beaker, dissolving the zinc nitrate, the magnesium oxide and the ammonium molybdate by using distilled water and dilute nitric acid, then adding the waste sponge carbon foam, adding ammonia water to adjust the pH value of the solution to 6-12, and fully stirring;
2) Placing the mixture into an ultrasonic reactor, placing a beaker into a hydrothermal dipping reactor to react for 30min at 85 ℃, wherein the ultrasonic starting power is 1200W;
3) Drying the obtained product at 120 ℃ after the reaction is finished to obtain the waste sponge foam carbon-based composite adsorption material C-ZnO-MoO 3 -MgO。
As a further preferable technical scheme of the preparation method of the waste sponge carbon-based composite adsorption material, the preparation method of the waste sponge carbon foam comprises the following steps: and (2) placing the waste sponge and the waste foamed plastic in inert gas for high-temperature carbonization, then cleaning and drying, and finally activating and forming pores in the inert atmosphere to obtain the waste sponge foamed carbon material.
Obtaining the waste sponge foam carbon-based composite adsorbing material C-ZnO-MoO 3 C, znO and MoO in-MgO 3 And the doping molar ratio of MgO is 7:1 to 2:1 to 2:1 to 2. Further preferably, the waste sponge foam carbon-based composite adsorbing material C-ZnO-MoO is obtained 3 -C, znO and MoO in MgO 3 And the doping molar ratio of MgO is 7:1:2:2.
the invention also provides application of the waste sponge foam carbon-based composite adsorption material prepared by the method in adsorption removal of chromium in wastewater.
Compared with the prior art, the invention has the beneficial effects that:
the invention takes waste sponge/foam carbon base as a main carrier material and ZnO-MoO with certain content and composition 3 MgO is used as filler of the adsorbing material to prepare the multi-element composite adsorbing material with excellent performance. The structure of the ZnO-MoO is characterized by adopting an instrument characterization means XRD and SEM, the adsorption performance is tested, and ZnO-MoO with excellent performance is screened out 3 MgO modified waste sponge carbon-based adsorption material. Experiments show that the prepared ZnO-MoO 3 The MgO (1. The prepared target product reaches the expected target of experimental design, and the ZnO-MoO is proved 3 The MgO modified waste sponge carbon-based adsorption material can be used for treating chromium-containing wastewater. In addition, the enriched chromium can be used in the fields of electroplating, tanning, printing and dyeing, medicine, fuel, catalysts, oxidants, matches, metal corrosion inhibitors and the like.
Drawings
The following provides further details of the preparation method of the waste sponge foam carbon-based composite adsorption material and the application of the waste sponge foam carbon-based composite adsorption material in adsorption removal of chromium in wastewater, with reference to the examples and the accompanying drawings.
Fig. 1 is an XRD pattern of each series of composite adsorbents prepared in examples 1 to 7.
Fig. 2 is SEM images of low, medium, and high magnification in order of the composite adsorbent prepared in example 1.
FIG. 3 is a graph showing the percentage of adsorbed residual chromium ions in the series of composite adsorbent materials prepared in examples 1 to 9.
FIG. 4 is a graph showing the adsorption amounts of the composite adsorbents of examples 1 to 7.
Detailed Description
Example 1
In the implementation, the prepared waste sponge carbon-based composite adsorbing material C-ZnO-MoO 3 in-MgO, C, znO, moO 3 And the doping molar ratio of MgO is 7:1:2:2. the preparation method comprises the following steps:
1) And placing the waste sponge and the waste foamed plastic in inert gas for high-temperature carbonization, then cleaning and drying, and finally activating and forming pores in inert atmosphere to obtain the waste sponge foamed carbon material.
2) Weighing zinc nitrate, magnesium oxide and ammonium molybdate, adding the zinc nitrate, the magnesium oxide and the ammonium molybdate into a beaker, dissolving the zinc nitrate, the magnesium oxide and the ammonium molybdate by using distilled water and dilute nitric acid, then adding the waste sponge carbon foam, adding ammonia water to adjust the pH value of the solution to 10, and fully stirring.
3) Placing the mixture into an ultrasonic reactor, placing a beaker into a hydrothermal dipping reactor, and reacting for 30min at 85 ℃ with the ultrasonic starting power of 1200W.
4) After the reaction is finished, drying the obtained product at 120 ℃ to obtain the waste sponge carbon-based composite adsorbing material C-ZnO-MoO 3 -MgO(7：1：2：2)。
Example 2
In this example, the prepared waste sponge carbon-based composite adsorbing material C-ZnO-MoO 3 in-MgO, C, znO, moO 3 The doping molar ratio of MgO is 7:1:1:1, the preparation method is the same as that of example 1, and the waste sponge foam carbon-based composite adsorbing material C-ZnO-MoO is obtained 3 -MgO(7：1：1：1)。
Example 3
In this example, the waste sponge producedCarbon foam-based composite adsorption material C-ZnO-MoO 3 in-MgO, C, znO, moO 3 The doping molar ratio of MgO is 7:1:1:2, the preparation method is the same as that of the example 1, and the waste sponge foam carbon-based composite adsorbing material C-ZnO-MoO is obtained 3 -MgO(7：1：1：2)。
Example 4
In the embodiment, the prepared waste sponge foam carbon-based composite adsorbing material C-ZnO-MoO 3 in-MgO, C, znO, moO 3 And the doping molar ratio of MgO is 7:1:2:1, the preparation method is the same as that of example 1, and the waste sponge foam carbon-based composite adsorbing material C-ZnO-MoO is obtained 3 -MgO(7：1：2：1)。
Example 5
In this example, the prepared waste sponge carbon-based composite adsorbing material C-ZnO-MoO 3 of-MgO, C, znO, moO 3 And the doping molar ratio of MgO is 7:2:1:1, the preparation method is the same as that of example 1, and the waste sponge foam carbon-based composite adsorbing material C-ZnO-MoO is obtained 3 -MgO(7：2：1：1)。
Example 6
In the embodiment, the prepared waste sponge foam carbon-based composite adsorbing material C-ZnO-MoO 3 in-MgO, C, znO, moO 3 And the doping molar ratio of MgO is 7:2:1:2, the preparation method is the same as that of the example 1, and the waste sponge foam carbon-based composite adsorbing material C-ZnO-MoO is obtained 3 -MgO(7：2：1：2)。
Example 7
In the embodiment, the prepared waste sponge foam carbon-based composite adsorbing material C-ZnO-MoO 3 in-MgO, C, znO, moO 3 And the doping molar ratio of MgO is 7:2:2:1, the preparation method is the same as that of example 1, and the waste sponge foam carbon-based composite adsorbing material C-ZnO-MoO is obtained 3 -MgO(7：2：2：1)。
Example 8
In this example, zinc nitrate and magnesium oxide were not added, and the prepared waste sponge carbon-based composite adsorption material C-MoO 3 Middle, C, moO 3 Is 7:1, other preparation methods are the same as example 1, and the waste sponge foam carbon-based composite material is obtainedAdsorbing material C-MoO 3 (7：1)。
Example 9
In this example, ammonium molybdate and magnesium oxide were not added, and the doping molar ratio of C, znO in the prepared waste sponge foam carbon-based composite adsorbing material C-ZnO was 7:2, the other preparation methods are the same as the example 1, and the waste sponge foam carbon-based composite adsorbing material C-ZnO (7:2) is obtained.
Fig. 1 is an XRD pattern of each series of composite adsorbents prepared in examples 1 to 7. As can be seen from FIG. 1, the diffraction intensity peak and C-ZnO-MoO of the sample 3 MgO basically corresponds to MgO. The XRD diffraction pattern has obvious MgO, znO and MoO 3 The diffraction peaks are relatively sharp, which shows that the synthesized composite adsorbent is in phase with the experimental design target waste sponge carbon-based composite adsorption material C-ZnO-MoO 3 MgO fit.
Fig. 2 is SEM images of low, medium, and high magnifications of the composite adsorbent prepared in example 1 in this order. As can be seen from FIG. 2, example 1 obtained a spent sponge carbon-based composite adsorbent C-ZnO-MoO having a mixed structure of a spherical shape and a rod shape 3 MgO, the channel structure is obvious, the microstructure of the composite material presents multi-level and multi-scale, and the size range is 400nm-3 um.
FIG. 3 shows the influence of a series of waste sponge carbon-based composite adsorbent materials composed of different composite proportions on the removal rate of chromium-containing sewage solution under the condition of sunlight. Wherein the dosage of sample materials is 30mg, the adsorption time is 70min, the volume of the chromium-containing sewage solution is 100mL, and the initial concentration is 80mg/L. As can be seen from FIG. 3, the waste sponge carbon-based composite adsorbing material C-ZnO-MoO prepared in example 1 3 The adsorption effect of MgO (7.
FIG. 4 is a curve of adsorption capacity, removal time and substance composition of a series of waste sponge carbon-based composite materials with different compositions on a chromium (3-valent chromium and 6-valent chromium) containing solution under a sunlight condition. Wherein the dosage of the sample material is 60mg, the adsorption time is 140min, and the volume of the chromium-containing (3-valent chromium and 6-valent chromium) solution is 500mL. As is clear from FIG. 4, the product of example 1Prepared waste sponge foam carbon-based composite adsorption material C-ZnO-MoO 3 The adsorption effect of MgO (7.
Experiments show that the prepared target product achieves the expected target of experimental design, and the prepared waste sponge foam carbon-based composite adsorption material C-ZnO-MoO is proved 3 the-MgO can be used for the environmental treatment of industrial sewage and wastewater containing chromium heavy metal solution.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (2)
1. A preparation method of a waste sponge foam carbon-based composite adsorption material is characterized by comprising the following specific steps:
1) Weighing zinc nitrate, magnesium oxide and ammonium molybdate, adding the zinc nitrate, the magnesium oxide and the ammonium molybdate into a beaker, dissolving the zinc nitrate, the magnesium oxide and the ammonium molybdate by using distilled water and dilute nitric acid, then adding the waste sponge carbon foam, adding ammonia water to adjust the pH value of the solution to 10, and fully stirring the mixture;
the preparation method of the waste sponge carbon foam comprises the following steps: placing the waste sponge and the waste foamed plastic in inert gas for high-temperature carbonization, then cleaning and drying, and finally activating and forming pores in inert atmosphere to obtain a waste sponge foamed carbon material;
2) Placing the mixture into an ultrasonic reactor, placing a beaker into hydrothermal impregnation, and reacting for 30min at 85 ℃, wherein the ultrasonic starting power is 1200W;
3) After the reaction is finished, drying the obtained product at 120 ℃ to obtain the waste sponge carbon-based composite adsorbing material C-ZnO-MoO 3 MgO, obtaining wasteCarbon-based composite adsorption material C-ZnO-MoO prepared by abandoned sponge foam 3 -C, znO and MoO in MgO 3 And the doping molar ratio of MgO is 7:1:2:2.
2. the application of the waste sponge foam carbon-based composite adsorption material prepared by the method of claim 1 in adsorption removal of chromium in wastewater.
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2020
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| EP0037537A1 (en) * | 1980-04-03 | 1981-10-14 | Fraunhofer-Gesellschaft Zur Förderung Der Angewandten Forschung E.V. | Process for the manufacture of highly specific active char |
| US5000858A (en) * | 1989-07-17 | 1991-03-19 | Coltec Industries Inc. | Method for removing hexavalent chromium from water |
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