CN114471475A - Heavy metal adsorbent and preparation method thereof - Google Patents
Heavy metal adsorbent and preparation method thereof Download PDFInfo
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- CN114471475A CN114471475A CN202210198001.6A CN202210198001A CN114471475A CN 114471475 A CN114471475 A CN 114471475A CN 202210198001 A CN202210198001 A CN 202210198001A CN 114471475 A CN114471475 A CN 114471475A
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- heavy metal
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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
- B01J20/14—Diatomaceous earth
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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
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
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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
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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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- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a heavy metal adsorbent and a preparation method thereof, and belongs to the technical field of treatment of heavy metal-containing wastewater. The preparation method of the heavy metal adsorbent comprises the following steps: (1) microwave acid leaching of diatomite; (2) dispersing the diatomite subjected to microwave acid leaching into ammonia water, adding zinc hydroxide, and stirring for dissolving; (3) and (3) adding a 2-methylimidazole methanol solution into the solution obtained in the step (2), filtering after the reaction is finished, and drying filter residues to obtain the heavy metal adsorbent. The preparation method provided by the invention is simple, the used raw materials are conventional, special equipment is not needed, and the prepared heavy metal adsorbent is strong in adsorption capacity, economical, applicable and high in popularization value.
Description
Technical Field
The invention relates to the technical field of heavy metal-containing wastewater treatment, and particularly relates to a heavy metal adsorbent and a preparation method thereof.
Background
Water is a source of life, however, with the development of industrialization, the discharge of industrial wastewater, especially chemical wastewater, seriously threatens the limited fresh water resource. Heavy metal ions are one of important harmful substances in wastewater, if the wastewater containing the heavy metal ions is carelessly introduced in aquatic animal breeding, the heavy metals can be accumulated in animal bodies and cannot be discharged through metabolism, and further, if corresponding animals such as fish, shrimps, crabs, cows, sheep and the like are eaten by human beings, the heavy metals can be enriched in human bodies, so that different serious diseases are caused. For example, arsenic is carcinogenic, cadmium causes osteoporosis and kidney damage, mercury destroys the central nervous system, etc., and only trace amounts of heavy metal ions are sufficient to harm the health of humans and other animals and plants. Therefore, it is necessary to remove heavy metal ions in wastewater treatment.
At present, the treatment technology of heavy metal ions in wastewater comprises the following steps: membrane separation technology, coagulation and flocculation precipitation, filtration technology, adsorption method, chemical method and the like, wherein the adsorption method is always a research hotspot due to simple process, low cost and high efficiency. Common adsorbents such as activated carbon, diatomite, functionalized silica, carbon nanotubes and the like are often small in adsorption capacity, unstable in adsorption and easy to desorb, so that the practical application of the adsorption technology is restricted.
Disclosure of Invention
In order to solve the problems, the invention provides a heavy metal adsorbent and a preparation method thereof. The pore volume of the diatomite is expanded through microwave acid leaching, then zeolite imidazolate framework materials formed by zinc hydroxide and 2-methylimidazole are compounded with the diatomite, and the heavy metal adsorbent with stronger adsorption capacity is prepared through the synergistic adsorption effect of the diatomite and the zeolite imidazolate framework materials.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention adopts one of the technical schemes: the preparation method of the heavy metal adsorbent comprises the following steps:
(1) microwave acid leaching of diatomite;
(2) dispersing the diatomite subjected to microwave acid leaching into ammonia water, adding zinc hydroxide, and stirring for dissolving;
(3) and (3) adding a 2-methylimidazole methanol solution into the solution obtained in the step (2), filtering after the reaction is finished, and drying filter residues to obtain the heavy metal adsorbent.
Preferably, the particle size of the diatomite is less than or equal to 0.075 mm.
Preferably, the acid leaching solution for microwave acid leaching is a sulfuric acid solution with the mass fraction of 35-45%, the microwave power is 300-400W, and the acid leaching time is 25-35 min.
Preferably, the mass ratio of the diatomite subjected to microwave acid leaching to the zinc hydroxide is (20-25): 1.
Preferably, the mass fraction of the ammonia water is 25-30%.
More preferably, the mass volume ratio of the zinc hydroxide to the ammonia water is 1g (2-2.5) L.
Preferably, the molar ratio of the zinc hydroxide to the 2-methylimidazole is 1 (3-4).
Preferably, the reaction time in the step (3) is 15-20 min.
The second technical scheme of the invention is as follows: provides a heavy metal adsorbent prepared by the preparation method of the heavy metal adsorbent.
The zeolite imidazole ester framework material is a novel metal organic framework material which is synthesized in recent years and has a framework structure similar to that of a zeolite porous material. The method has strong heavy metal ion adsorption capacity, and the cost is too high although the heavy metal adsorption capacity is strong, so that the method is not high in practicability because the method is applied to removing the heavy metal ions in the wastewater at too high cost.
According to the invention, the heavy metal ions are loaded on the surface of the diatomite and are firstly adsorbed by the zeolitic imidazolate framework material with stronger adsorption capacity, so that a heavy metal ion high-concentration area is formed on the surface of the diatomite, the heavy metal ions in the high-concentration area are slowly diffused to a diatomite low-concentration area, at the moment, the diatomite adsorbs the heavy metal ions in the diatomite through surface complexation, pore channel adsorption, ion exchange and other modes, when the diatomite is saturated in adsorption, the heavy metal ions are diffused outwards, at the moment, the zeolitic imidazolate framework material blocks the heavy metal ions from being diffused outwards, and the adsorption capacity of the heavy metal adsorbent obtained by compounding the diatomite and the zeolitic imidazolate framework material is greatly improved through the synergistic effect of the zeolitic imidazolate framework material and the ion.
The invention has the following beneficial technical effects:
the invention provides a preparation method of a heavy metal adsorbent. Firstly, expanding the pore volume of diatomite by microwave acid leaching, then, utilizing a zeolite imidazolate framework material formed by zinc hydroxide and 2-methylimidazole to be compounded with the diatomite, loading the zeolite imidazolate framework material on the surface of the diatomite, and preparing the heavy metal adsorbent with stronger adsorption capacity through the synergistic adsorption effect of the diatomite and the zeolite imidazolate framework material.
The preparation method provided by the invention is simple, the used raw materials are conventional, special equipment is not needed, and the prepared heavy metal adsorbent is strong in adsorption capacity, economical, applicable and high in popularization value.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every intervening value, to the extent any stated value or intervening value in a stated range, and any other stated or intervening value in a stated range, is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The diatomite used in the invention is diatomite which is sieved by a 200-mesh sieve (0.075mm), and the pore volume is 0.85cm3/g。
Example 1
Preparation of heavy metal adsorbent:
(1) adding 20g of diatomite into 200mL of 40% sulfuric acid aqueous solution, adding 0.4g of dispersing agent sodium hexametaphosphate, stirring to uniformly disperse the diatomite, placing the diatomite into a microwave heating device, heating the diatomite by microwave at the microwave power of 300W for 35min, filtering the diatomite after microwave heating, washing filter residues to be neutral by water, drying the filter residues at the temperature of 80 ℃ for 10h, crushing the filter residues, sieving the filter residues by a 200-mesh sieve, and measuring the pore volume of the obtained diatomite to be 0.98cm3/g。
(2) 2g of the diatomite treated in the step (1) is added into 200mL of ammonia water with the mass fraction of 25%, then 0.1g (1mmol) of zinc hydroxide is added, and the mixture is stirred at 400rpm for 10 min.
(3) And (3) adding 5.0mL of methanol solution in which 0.328g (4mmol) of 2-methylimidazole is dissolved into the solution obtained in the step (2), stirring at the normal temperature of 400rpm for 15min, filtering, washing filter residues with methanol, and drying at the temperature of 80 ℃ for 10h to obtain 2.19g of the heavy metal adsorbent.
Example 2
Preparation of heavy metal adsorbent:
(1) adding 20g of diatomite into 200mL of 35% sulfuric acid aqueous solution by mass fraction, adding 0.4g of dispersing agent sodium hexametaphosphate, stirring to uniformly disperse the diatomite, placing the diatomite into a microwave heating device, heating the diatomite by microwave at 400W for 25min, filtering the diatomite after microwave heating, washing filter residues to be neutral by water, drying the filter residues at 80 ℃ for 10h, crushing the filter residues, sieving the filter residues by a 200-mesh sieve, and measuring the pore volume of the obtained diatomite to be 0.93cm3/g。
(2) 2g of the diatomite treated in the step (1) is added into 200mL of ammonia water with the mass fraction of 25%, then 0.1g (1mmol) of zinc hydroxide is added, and the mixture is stirred at 400rpm for 10 min.
(3) And (3) adding 5mL of methanol solution in which 0.287g (3.5mmol) of 2-methylimidazole is dissolved into the solution obtained in the step (2), stirring at the normal temperature of 400rpm for 20min, filtering, washing filter residues with methanol, and drying at 80 ℃ for 10h to obtain 2.18g of the heavy metal adsorbent.
Example 3
Preparation of the heavy metal adsorbent:
(1) adding 20g of diatomite into 200mL of 45% sulfuric acid aqueous solution by mass fraction, adding 0.4g of dispersing agent sodium hexametaphosphate, stirring to uniformly disperse the diatomite, placing the diatomite into a microwave heating device, heating the diatomite by microwave at 400W for 30min, filtering the diatomite after microwave heating, washing filter residues to be neutral by water, drying the filter residues at 80 ℃ for 10h, crushing the filter residues, sieving the filter residues by a 200-mesh sieve, and measuring the pore volume of the obtained diatomite to be 1.03cm3/g。
(2) 2g of the diatomite treated in the step (1) is added into 200mL of ammonia water with the mass fraction of 30%, then 0.1g (1mmol) of zinc hydroxide is added, and the mixture is stirred at 400rpm for 10 min.
(3) And (3) adding 5mL of methanol solution in which 0.246g (3mmol) of 2-methylimidazole is dissolved into the solution obtained in the step (2), stirring at normal temperature of 400rpm for 18min, filtering, washing filter residues with methanol, and drying at 80 ℃ for 10h to obtain 2.20g of the heavy metal adsorbent.
Comparative example 1
Preparation of heavy metal adsorbent:
compared with the example 1, the microwave acid leaching process in the step (1) is omitted, the subsequent preparation steps are directly carried out by adopting 2g of initial diatomite, the dosage of the added reagent is the same as that in the example 1, and 2.15g of heavy metal adsorbent is obtained.
Comparative example 2
Preparation of zeolitic imidazolate framework material:
adding 0.1g (1mmol) of zinc hydroxide into 200mL of 25 mass percent ammonia water, and stirring at 400rpm for 10 min; adding 5.0mL of methanol solution containing 0.328g (4mmol) of 2-methylimidazole, stirring at normal temperature of 400rpm for 15min, filtering, washing the filter residue with methanol, and drying at 80 ℃ for 10h to obtain 0.22g of zeolite imidazole ester framework material.
The heavy metal ion adsorption capacity of various heavy metal adsorbents prepared by the method is determined as follows:
preparation of Cu-containing2+300mg/L and Pb2+Adding 0.1g of adsorbent into 100mL of 400mg/L aqueous solution, stirring for 4h, centrifuging at 10000rpm for 30min, measuring the concentration of heavy metal ions in the aqueous solution after adsorption, and calculating the adsorption amount of each adsorbent, wherein the calculation results are shown in Table 1.
TABLE 1 adsorption amount of heavy metal ions of each adsorbent
As can be seen from table 1, after the acid washing treatment, the pore volume of the diatomite is increased, the adsorption surface area is increased, and the ability of adsorbing heavy metal ions is enhanced, and when the diatomite is further compounded with the zeolitic imidazolate framework material to prepare the heavy metal adsorbent after the acid washing, the heavy metal ion adsorption ability of the prepared heavy metal adsorbent can be greatly improved. If the diatomite and the zeolitic imidazolate framework material are simply mixed after acid washing, the adsorption capacity cannot be well improved, because the zeolitic imidazolate framework material is loaded on the surface of the diatomite after acid washing in the heavy metal adsorbent prepared by the invention, on one hand, a high-concentration heavy metal ion environment is provided for the adsorption of the diatomite, on the other hand, the heavy metal ions adsorbed by the diatomite are prevented from diffusing outwards, so that the two generate a synergistic effect, and the heavy metal ion adsorption capacity of the heavy metal adsorbent prepared by compounding the diatomite and the zeolitic imidazolate framework material is greatly improved.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (9)
1. The preparation method of the heavy metal adsorbent is characterized by comprising the following steps:
(1) microwave acid leaching of diatomite;
(2) dispersing the diatomite subjected to microwave acid leaching into ammonia water, adding zinc hydroxide, and stirring for dissolving;
(3) and (3) adding a 2-methylimidazole methanol solution into the solution obtained in the step (2), filtering after the reaction is finished, and drying filter residues to obtain the heavy metal adsorbent.
2. The preparation method of the heavy metal adsorbent according to claim 1, wherein the particle size of the diatomite is less than or equal to 0.075 mm.
3. The preparation method of the heavy metal adsorbent according to claim 1, wherein the acid leaching solution is a 35-45% sulfuric acid solution in mass fraction, the microwave power is 300-400W, and the acid leaching time is 25-35 min.
4. The preparation method of the heavy metal adsorbent according to claim 1, wherein the mass ratio of the diatomite subjected to microwave acid leaching to the zinc hydroxide is (20-25): 1.
5. The method for preparing the heavy metal adsorbent according to claim 1, wherein the mass fraction of the ammonia water is 25-30%.
6. The preparation method of the heavy metal adsorbent according to claim 5, wherein the mass-to-volume ratio of the zinc hydroxide to the ammonia water is 1g (2-2.5) L.
7. The method for preparing the heavy metal adsorbent according to claim 1, wherein the molar ratio of the zinc hydroxide to the 2-methylimidazole is 1 (3-4).
8. The preparation method of the heavy metal adsorbent according to claim 1, wherein the reaction time in the step (3) is 15-20 min.
9. A heavy metal adsorbent prepared by the preparation method of the heavy metal adsorbent according to any one of claims 1 to 8.
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| CN112516968A (en) * | 2020-12-16 | 2021-03-19 | 东北电力大学 | Preparation method of metal organic framework material loaded modified diatomite adsorbent |
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2022
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| CN104525104A (en) * | 2014-12-09 | 2015-04-22 | 厦门理工学院 | Method for removing heavy metals in garbage percolate by using microwave modified diatomite |
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