CN113398890A - Method for preparing heavy metal composite adsorbent from coal-based sodium humate/zeolite - Google Patents
Method for preparing heavy metal composite adsorbent from coal-based sodium humate/zeolite Download PDFInfo
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- CN113398890A CN113398890A CN202110683629.0A CN202110683629A CN113398890A CN 113398890 A CN113398890 A CN 113398890A CN 202110683629 A CN202110683629 A CN 202110683629A CN 113398890 A CN113398890 A CN 113398890A
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
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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
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Abstract
The invention belongs to the technical field of adsorption separation, and relates to a preparation method of an adsorbent for removing heavy metals such as lead, cadmium, chromium and the like. The invention carries out composite regulation and control on two materials based on the structural characteristics of the coal-based sodium humate and the artificial zeolite, optimizes the performance of the adsorbent and has stable adsorption and removal effects on heavy metal ions. The composite adsorbent provided by the invention is used for adsorbing Pb2+The adsorption capacity of the composite can reach 531mg/g, which is far higher than that of the active carbon, the modified fly ash and the sodiumCommon adsorbents such as rice clay; compared with other adsorbing materials, the composite adsorbent has excellent environmental adaptability, and particularly in an acidic environment (pH is 3-6), the removal rate can still be kept above 90%.
Description
Technical Field
The invention belongs to the technical field of adsorption separation, and relates to a preparation method of a composite adsorbent for removing heavy metals such as lead, cadmium, chromium and the like in acidic wastewater.
Background
With the rapid development of industry, the heavy metal pollution events of related water areas caused by industrial and mining wastewater are frequent, and lead, cadmium, chromium and the like belong to high-risk heavy metals, thereby greatly threatening the health of the public. The removal and purification of heavy metals in water bodies become one of the key and difficult points of industrial and mining wastewater treatment.
At present, an adsorption method is widely adopted for treating heavy metal pollution of wastewater. Previous studies have used clay substances such as rectorite and bentonite, and organic substances such as humic acid and sodium alginate, but all have the problems of high adsorption amount, poor stability and extremely low adsorption capacity in an acidic environment. From the structural characteristic analysis of zeolite and humic acid, the adsorption performance is hopefully improved by compounding the zeolite and the humic acid, and the adaptability of the zeolite to an acidic environment is enhanced. No research report in this aspect is found at present.
The inventor thinks that the weathered coal resources in China are extremely rich, the weathered coal humic acid (salt) contains a large amount of carboxyl and phenolic hydroxyl functional groups, has good adsorption and complexation effects on heavy metal ions, and the formed complex has good tolerance to an acid environment, and when the pH value is reduced, the macromolecular network structure of the humic acid can buffer the water solubility of the heavy metal complex. The zeolite has rich pore passage gaps and strong cation exchange capacity, heavy metal ions have chemical and electrostatic bonding effects on the surface of the zeolite, the chemical bonding adsorption has strong selectivity and irreversibility, the electrostatic bonding adsorption has no selectivity and has strong reversibility, so the adsorption effect of the conventional zeolite on the heavy metal in the water body is conditional: under acidic conditions, some heavy metal ions can be released, migrated and restored to toxicity. Therefore, based on different structural characteristics of the humic acid substances and the zeolite-type adsorbent, a synergistic effect can be formed, and the removal capacity of the composite adsorbent for heavy metals is enhanced. Particularly, the waste water with high content of general heavy metals is mostly acidic, the composite adsorbent can greatly enhance the adaptability to the acidic water environment, and can keep higher and more stable adsorption capacity within the range of pH 3-6.
Disclosure of Invention
The invention aims to provide a method for preparing heavy metal adsorbents such as lead, cadmium, chromium and the like by using coal-based sodium humate and artificial zeolite, wherein the composite adsorbent has a strong adsorption and fixation effect on heavy metal ions, and is simple in preparation method, low in price, easy to obtain, wide in application range and strong in environmental adaptability.
The technical scheme adopted by the invention is as follows:
a preparation method of a composite adsorbent for removing heavy metals such as lead, cadmium, chromium and the like is obtained by the following steps: compounding coal-based sodium humate and artificial zeolite according to a certain mass ratio, and carrying out wet grinding and drying at a specific temperature to obtain the composite adsorbent.
The artificial zeolite (provided by Shanghai Michelin Biochemical technology Co., Ltd.) has a primary particle size of 5 mm; sodium humate (extracted from weathered coal, E4/E6 is 2.63), does not need to be converted into humic acid, simplifies the process and greatly reduces the production cost.
Further, the mass ratio of the coal-based sodium humate to the artificial zeolite is 1: 3-4: 1.
preferably, the artificial zeolite is ground and sieved, and the particle size is 120-200 meshes.
Weighing coal-based sodium humate and ground and sieved artificial zeolite according to a certain solid-liquid ratio, adding a proper amount of deionized water for grinding for three times, and uniformly mixing the two.
Specifically, the ratio of 1: 2-1: 5, adding deionized water into the solid-liquid ratio, and grinding the mixture to be pasty.
And (3) drying the uniformly mixed paste slurry in a 60 ℃ oven for 60-120 min to form a composite adsorbent after complete drying, grinding the composite adsorbent into a powdery product, and sealing and storing the powdery product.
The composite adsorbent for removing heavy metals such as lead, cadmium, chromium and the like, which is obtained by the method, fully exerts the good adsorption, ion exchange and surface complexation characteristics of the artificial zeolite and the coal-based sodium humate on the heavy metal ions, and forms a synergistic effect. Can still maintain excellent adsorption capacity and adsorption stability for stronger acidic wastewater (especially under the condition that the pH value is approximately equal to 3). Compared with the traditional adsorbing material, the composite adsorbent obtained by the invention has wider application range, higher adsorption capacity and adsorption efficiency, and shows excellent performance in adsorption and desorption experiments of heavy metal lead and cadmium ions.
The adsorption performance in the actual adsorption and desorption experiment is explained as follows:
the adsorption performance of the composite adsorbent is as follows: the maximum adsorption capacity of the adsorbent in a lead ion solution of 100mg/L is 410-470 mg/g; the maximum adsorption capacity of the adsorbent in 350mg/L lead ion solution is 525-540 mg/g.
Adsorption rate of the composite adsorbent: in an adsorption experiment, the removal rate is 84.2% in 60min, the removal rate can reach 98.1% in adsorption equilibrium, the adsorption rate is not greatly influenced by temperature, and the adsorption is facilitated by properly increasing the temperature.
Adsorption stability of the composite adsorbent: in a pure water desorption experiment, the desorption rate of lead ions is not more than 5 percent.
Applicability of the composite adsorbent: the adsorbent has high adsorption capacity and adsorption efficiency in weak acid solution, taking 100mg/L lead ion solution as an example, when the pH value is 3, the adsorption capacity is 210-230 mg/g; when the pH value is 4-6, the adsorption capacity is 410-470 mg/g, which is higher than other adsorbents of the same type.
Data fitting of composite adsorbent: and fitting an adsorption kinetic model and an isothermal adsorption model through adsorption experimental data. The fitted curve proves that the adsorption process of the material conforms to a quasi-second-order adsorption kinetic model and a Langmuir isothermal adsorption model, and the adsorption process of the material is controlled by chemical adsorption, namely the chemical adsorption is taken as the main factor.
The processes of electrostatic attraction, surface complexation, ion exchange and the like can be speculated by combining experimental data, a fitted adsorption kinetics model and an isothermal adsorption model, wherein the adsorption of the monolayer is mainly performed on lead ions and the adsorbent.
Compared with the prior art, the invention has the following advantages:
the invention provides a preparation method of a composite adsorbent for removing heavy metals such as lead, cadmium, chromium and the like, and the composite adsorbent has strong adsorption capacity for heavy metal ions, stable combination, large adsorption capacity, high adsorption efficiency, low desorption rate, simple operation method, low price, easy obtainment and strong environmental adaptability, and is particularly suitable for treating heavy metals in acidic wastewater.
Description of the drawings: FIG. 1 is a process flow diagram of the present invention; FIG. 2 is a schematic view of an adsorption experiment according to the present invention; FIG. 3 is a schematic diagram of a desorption experiment (stability test) according to the present invention; FIG. 4 shows different Pb2+The form of the adsorbent after adsorption under the condition of initial concentration.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples, comparative examples and drawings, but these examples are not intended to limit the scope of the present invention. The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and conventional commercial products are available from regular distributors.
Examples 1 to 7 and comparative examples 1 to 3 were carried out as follows:
adsorption experiment: weighing a certain mass ratio of coal-based sodium humate and artificial zeolite, adding deionized water for three times according to different solid-liquid ratios, grinding, uniformly mixing, placing in a 60 ℃ oven, drying for 90min, forming a composite adsorbent after complete drying, grinding into a powdery product, and sealing for later use; weighing a composite adsorbent with required mass, uniformly mixing the adsorbent with 10mL of deionized water to form a brown colloidal solution, sealing the solution by using a dialysis bag with the molecular weight of 3500D, and putting the solution into a conical flask filled with 50mL of heavy metal waste liquid to perform an adsorption experiment (earlier experiments prove that the dialysis bag has little influence on adsorption performance and can be ignored; in the data processing process, the volume of the solution in the dialysis bag is converted to ensure the validity of experimental data); under the conditions of different initial concentrations of heavy metal ions, the pH value of the solution and the adding amount of the adsorbent, oscillating at a constant temperature of 25 ℃, absorbing at a rotating speed of 150rpm for 24 hours, taking the supernatant of the dialysis bag, detecting the concentration of the heavy metal ions, and calculating the removal rate and the adsorption capacity, wherein the specific experimental operation is shown in figure 2;
desorption experiment (stability test): and (3) changing the lead solution adsorbed in the conical flask into deionized water with the same volume, oscillating and desorbing for 24h under the same condition, detecting the concentration of heavy metal ions in the liquid, and calculating the retention rate, wherein the specific experimental operation is shown in figure 3.
Example 1 (adsorption of Pb2+)：
The compounding ratio of the adsorbent is that coal-based sodium humate/artificial zeolite is 1: 2, the solid-liquid ratio is 1: 3, Pb2+Initial concentration of 100mg/L, solution pH of 3, adsorbent dosage of 0.5g/L, adsorption performance: the adsorption capacity was 197mg/g, the removal rate was 98.5%, and the retention rate was 94.3%.
Example 2 (adsorption of Pb2+)：
The compounding ratio of the adsorbent is that coal-based sodium humate/artificial zeolite is 1: 2, the solid-liquid ratio is 1: 3, Pb2+Initial concentration of 100mg/L, solution pH 4, adsorbent dosage of 0.4g/L, adsorption performance: the adsorption capacity is 248mg/g, the removal rate is 99.4 percent, and the retention rate is 95.7 percent.
Example 3 (adsorption of Pb2+)：
The compounding ratio of the adsorbent is that coal-based sodium humate/artificial zeolite is 1: 3, the solid-liquid ratio is 1: 2, Pb2+Initial concentration of 100mg/L, solution pH 5, adsorbent dosage of 0.4g/L, adsorption performance: the adsorption capacity was 246mg/g, the removal rate was 98.5%, and the retention rate was 94.7%.
Example 4 (adsorption of Pb2+)：
The compounding ratio of the adsorbent is that coal-based sodium humate/artificial zeolite is 1: 1, the solid-to-liquid ratio is 1: 4, Pb2+Initial concentration of 100mg/L, solution pH 6, adsorbent dosage of 0.2g/L, adsorption performance: the adsorption capacity was 482mg/g, the removal rate was 96.4%, and the retention rate was 94.0%.
Example 5 (adsorption of Pb2+)：
The compounding ratio of the adsorbent is that coal-based sodium humate/artificial zeolite is 3: 1, the solid-to-liquid ratio is 1: 5, Pb2+Initial concentration of 100mg/, solution pH 6, adsorbent dosage of 0.3g/L, adsorption performance: the adsorption capacity was 314mg/g, the removal rate was 94.2%, and the retention rate was 90.0%.
Example 6 (adsorption of Pb2+)：
The compounding ratio of the adsorbent is that coal-based sodium humate/artificial zeolite is 1: 1, the solid-to-liquid ratio is 1: 4, Pb2+The initial concentration was 350mg/L, the pH of the solution was 5 and the amount of adsorbent added was 0.4 g/L. Adsorption performance: the adsorption capacity was 527mg/G, the removal rate was 66.8%, the retention rate was 64.9%, and the state after adsorption of the adsorbent is shown as G in FIG. 4.
Example 7 (adsorption of Cd for immobilization2+)：
The compounding ratio of the adsorbent is that coal-based sodium humate/artificial zeolite is 1: 1, the solid-to-liquid ratio is 1: 4, Cd2+Initial concentration of 100mg/L, solution pH 5, adsorbent dosage of 0.4g/L, adsorption performance: the adsorption capacity is 238mg/g, the removal rate is 95.3 percent, the retention rate is 92.4 percent,
comparative example 1 (adsorption of Pb2+)：
The adsorbent is coal-based sodium humate before compounding; adsorption performance under the same conditions as the operating and experimental conditions of example 1: the adsorption capacity was 169mg/g, the removal rate was 84.4%, and the retention rate was 82.9%.
Comparative example 2 (adsorption of Pb2+)：
The adsorbent is coal-based sodium humate before compounding; adsorption performance under the same conditions as the operating and experimental conditions of example 2: the adsorption capacity is 239mg/g, the removal rate is 95.5 percent, and the retention rate is 86.8 percent.
Comparative example 3 (adsorption of Pb2+)：
The adsorbent is artificial zeolite before compounding; adsorption performance under the same conditions as the operating and experimental conditions of example 1: the adsorption capacity was 133mg/g, the removal rate was 66.6%, and the retention rate was 64.6%.
As described above, although the embodiments of the present invention have been described in detail, it will be apparent to those skilled in the art that many modifications are possible without substantially departing from the spirit and scope of the present invention. Therefore, such modifications are also all included in the scope of protection of the present invention.
Claims (6)
1. A preparation method of a composite adsorbent for removing heavy metals such as lead, cadmium, chromium and the like is characterized in that coal-based sodium humate and artificial zeolite are compounded according to a certain proportion, and the composite adsorbent is obtained after wet grinding and drying.
2. The preparation method of the composite adsorbent for removing heavy metals such as lead, cadmium and chromium according to claim 1, wherein the artificial zeolite is crushed and sieved to 80-200 meshes.
3. The preparation method of the composite adsorbent for removing heavy metals such as lead, cadmium, chromium and the like as claimed in claim 2, wherein the mass ratio of the coal-based sodium humate to the artificial zeolite is 1: 3-4: 1.
4. the method for preparing the composite adsorbent for removing heavy metals such as lead, cadmium, chromium and the like according to claim 3, wherein the coal-based sodium humate and the artificial zeolite which is ground and sieved are weighed according to the proportion, and the ratio of the coal-based sodium humate to the artificial zeolite is 1: 2-1: 5, grinding by adding water in a solid-liquid ratio, and uniformly adding deionized water for three times in the grinding period to fully mix the two.
5. The preparation method of the composite adsorbent for removing heavy metals such as lead, cadmium and chromium according to claim 4, wherein the uniformly mixed paste slurry is put into a 60 ℃ oven to be dried for 60-120 min, the composite adsorbent is formed after the drying is completed, and the composite adsorbent is ground into a powdery product to be sealed for later use.
6. The coal-based sodium humate/artificial zeolite composite adsorbent as claimed in claim 1, which is characterized in that: treating acidic wastewater containing heavy metal ions, wherein the pH value is 3-6 and initial Pb is obtained2+The concentration is 100mg/L, the input amount of the adsorbent is 0.2-0.5 g/L, the adsorption amount can reach 410-470 mg/g, and the removal rate is more than 90%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115106052A (en) * | 2022-07-19 | 2022-09-27 | 上海应用技术大学 | Sepiolite/montmorillonite composite material and preparation method and application thereof |
| CN117282400A (en) * | 2023-09-20 | 2023-12-26 | 深圳信息职业技术学院 | Application method of utilizing waste glass to hydrothermally synthesize analcite as heavy metal adsorption material in wastewater |
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| HUT54878A (en) * | 1989-08-18 | 1991-04-29 | Katalizator Kereskedoe Foevall | Method for producing fodder additive fixing radioactive and heavy-metal contaminations in the organism of animals and extracting them from there |
| CN1267641A (en) * | 1999-03-15 | 2000-09-27 | 中国地质大学（北京） | Technology of applying 13x zeolite in treating heavy metal-containing waste water and recovering metal |
| JP2009027957A (en) * | 2007-07-26 | 2009-02-12 | Nanasawa Kenkyusho:Kk | Soft drink for internal purification, and method for producing the same |
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| CN111377496A (en) * | 2019-08-02 | 2020-07-07 | 环亚(天津)环保科技有限公司 | Water environment restoration agent for reducing heavy metal content in water |
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Patent Citations (7)
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| HUT54878A (en) * | 1989-08-18 | 1991-04-29 | Katalizator Kereskedoe Foevall | Method for producing fodder additive fixing radioactive and heavy-metal contaminations in the organism of animals and extracting them from there |
| CN1267641A (en) * | 1999-03-15 | 2000-09-27 | 中国地质大学（北京） | Technology of applying 13x zeolite in treating heavy metal-containing waste water and recovering metal |
| JP2009027957A (en) * | 2007-07-26 | 2009-02-12 | Nanasawa Kenkyusho:Kk | Soft drink for internal purification, and method for producing the same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115106052A (en) * | 2022-07-19 | 2022-09-27 | 上海应用技术大学 | Sepiolite/montmorillonite composite material and preparation method and application thereof |
| CN117282400A (en) * | 2023-09-20 | 2023-12-26 | 深圳信息职业技术学院 | Application method of utilizing waste glass to hydrothermally synthesize analcite as heavy metal adsorption material in wastewater |
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Application publication date: 20210917 |