CN115155538A - Process for extracting heavy metal ions in sewage - Google Patents
Process for extracting heavy metal ions in sewage Download PDFInfo
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- CN115155538A CN115155538A CN202210966455.3A CN202210966455A CN115155538A CN 115155538 A CN115155538 A CN 115155538A CN 202210966455 A CN202210966455 A CN 202210966455A CN 115155538 A CN115155538 A CN 115155538A
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
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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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Abstract
The invention relates to an extraction process of heavy metal ions in sewage, which comprises the steps of firstly preparing an adsorbent formed by modifying and mixing bacterial cellulose and chitosan, then introducing the sewage containing heavy metals after primary treatment into a microbial pool to remove organic matters in a water body, and then passing through an adsorption column filled with the adsorbent; discharging the effluent after the heavy metal content reaches the standard after the effluent is adsorbed by the adsorption column, and returning to the adsorption column for continuous adsorption treatment if the heavy metal content does not reach the standard; finally, washing the adsorption column by EDTA-2Na, and collecting the eluent to obtain the liquid containing heavy metal ions. The novel heavy metal ion adsorbent is prepared based on bacterial cellulose and chitosan, contains abundant nitrogen, sulfur, selenium, hydroxyl and the like, can form stable coordination with heavy metals, can efficiently extract the heavy metals in industrial wastewater, is desorbed by eluent, has high desorption rate, and can subsequently recover the metal ions in the desorption solution by an electrochemical method and the like, thereby realizing resource recycling.
Description
Technical Field
The invention relates to the technical field of sewage treatment and recovery, in particular to an extraction process of heavy metal ions in sewage.
Background
The discharge of domestic sewage and industrial wastewater causes serious water body pollution, and further threatens the life health and safety of human beings, animals and plants. In recent years, researchers have developed a plurality of methods for treating plasmid domestic sewage and industrial wastewater, and the methods are commonly known as an adsorption method, a flocculation precipitation method, a biomass method, a membrane separation method and the like.
With the rapid development of society and the continuous consumption of resources, people begin to explore the recycling of available resources in sewage. Heavy metal pollution cannot be degraded in ecological environment, water pollution is enriched in animals and plants, and the water enters human bodies through food chains, so that anemia, an uncomfortable nitration system and the like are easily caused, and the health of the human bodies is seriously harmed. On the other hand, heavy metals are non-renewable resources, and have wide application and play an important role in many fields. At present, adsorption dissociation is considered as one of the most effective methods for extracting heavy metal ions, and many studies have been made on chitosan as an adsorbing material. The chitosan is used as a natural biological polymer, has quite rich sources, is easy to degrade in natural environment, and is a green material. The structure of the composite material contains abundant hydroxyl and amino, has good adsorption selectivity on specific metal ions, and has good application prospect on solving and treating various kinds of wastewater containing heavy metal ions. However, chitosan has problems of small specific surface area, low porosity, etc., and thus has low adsorption efficiency, and chitosan is not acid-resistant and has poor stability, so that it is required to be modified.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an extraction process for heavy metal ions in sewage; the adsorbent is prepared based on bacterial cellulose and chitosan, has high extraction rate and can be recycled.
In order to achieve the purpose, the invention provides the following technical scheme:
a process for extracting heavy metal ions in sewage comprises the following steps:
s1: preparation of the adsorbent
1) Adding bacterial cellulose hydrogel, 2-acrylamide-2-methylpropanesulfonic acid, an initiator ammonium persulfate and a cross-linking agent N, N' -methylene bisacrylamide into a reaction bottle, and heating to react for 3-5 hours under the protection of nitrogen;
2) Dissolving N-carboxymethyl chitosan in a reaction bottle by adding an organic solvent, dropwise adding acrylic glycidyl ether into the reaction bottle for ring-opening reaction, continuously adding acrylonitrile, p-vinylbenzyl phenyl selenide and ammonium persulfate into the reaction bottle after the reaction is finished, and heating for reaction for 2-4 hours under the protection of nitrogen;
3) Cooling and mixing the final reaction systems obtained in the steps 1) and 2), adjusting the pH value to be alkaline, adding glycol selenide, heating to 70 ℃, and stirring for 5-6 hours; washing the obtained solid with water, freeze-drying, and pulverizing to obtain adsorbent;
s2: introducing the sewage containing heavy metals after primary treatment into a microbial pool to remove organic matters in a water body, and then passing through an adsorption column filled with an adsorbent;
s3: discharging the effluent after the heavy metal content reaches the standard after the effluent is adsorbed by the adsorption column, and returning to the adsorption column for continuous adsorption treatment if the heavy metal content does not reach the standard; finally, washing the adsorption column by EDTA-2Na, and collecting the eluent.
Further, the mass ratio of the bacterial cellulose hydrogel in the step 1) to the 2-acrylamido-2-methylpropanesulfonic acid, the initiator ammonium persulfate and the crosslinking agent N, N' -methylenebisacrylamide is 10-30.
Further, the mass ratio of the N-carboxymethyl chitosan to the glycidyl acrylate in the step 2) is 1:2.5 to 3.5; the mass ratio of the acrylonitrile to the p-vinylbenzylphenylselenane to the ammonium persulfate to the N-carboxymethyl chitosan is 1-5.
Further, the reaction temperature of the step 1) and the step 2) is 60-70 ℃.
Furthermore, the water inlet flow rate of the adsorption column is 10-20 BV/h.
Further, the heavy metal ions include Pd 2+ And Cu 2+ 。
Furthermore, the concentration of the EDTA-2Na is 1.5mmol/L, and the flow rate is 0.5-2 BV/h.
The invention has the beneficial effects that: the invention prepares a novel heavy metal ion adsorbent based on bacterial cellulose and chitosan, the industrial wastewater is subjected to primary treatment and microbial treatment and then is introduced into an adsorption column containing the adsorbent, the adsorbent contains abundant nitrogen, sulfur, selenium, hydroxyl and the like, and can form stable coordination with heavy metals, the heavy metals in the industrial wastewater can be efficiently extracted, the desorption is carried out through EDTA-2Na solution, the desorption rate is high, the obtained desorption solution can subsequently recover the metal ions therein through an electrochemical method and the like, and the cyclic utilization of resources is realized.
Drawings
FIG. 1 is an SEM photograph of the adsorbent prepared in example 1.
FIG. 2 shows the comparison of Pd in simulated wastewater by the adsorbent prepared in example 1 2+ And Cu 2+ The adsorption amount of (2) is plotted as a function of pH.
FIG. 3 shows the comparison of Pd in simulated wastewater by the adsorbent prepared in example 1 2+ And Cu 2+ Is a graph showing the change of the adsorption amount of (2) with time.
Detailed Description
The technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1:
preparing adsorbent, wherein the synthesis of N-carboxymethyl chitosan as main raw material refers to Carbohydrate Research,1982,107 (2): 199-214. Synthesis, chitosan (degree of deacetylation > 95%, viscosity 100-200mPas, M = 180kDa); bacterial cellulose (dry weight 0.5g, available from Hainan Yide food Co., ltd.); the rest of the conventional reagents are commercially available.
1) Adding 20g of bacterial cellulose hydrogel (BC), 1g of 2-acrylamide-2-methylpropanesulfonic acid, 0.5g of initiator ammonium persulfate and 0.15g of cross-linking agent N, N' -Methylene Bisacrylamide (MBA) into a reaction bottle, and reacting for 3-5 h at 60 ℃ under the protection of nitrogen;
2) Dissolving 20g N-carboxymethyl chitosan (CMC) in an organic solvent in a reaction bottle, dropwise adding 50g of acrylic glycidyl ether into the reaction bottle for ring-opening reaction, continuously adding 2g of acrylonitrile, 1g of p-vinyl benzyl phenyl selenide and 0.1g of ammonium persulfate into the reaction bottle after the reaction is finished, and reacting for 2-4 h at 60 ℃ under the protection of nitrogen;
3) Cooling and mixing the final reaction systems obtained in the steps 1) and 2), adjusting the pH value to be alkaline, adding glycol selenide, heating to 70 ℃, and stirring for 5-6 hours; washing the obtained solid with water, freeze-drying, and pulverizing to obtain adsorbent;
a large amount of hydroxyl exists in the bacterial cellulose structure selected in the step 1), and the bacterial cellulose structure has a higher specific surface area compared with cellulose and has better adsorption performance on metal ions in a water body; according to the scheme, the BC is subjected to chemical modification, an amido group and a sulfonic group are introduced, and MBA is used for crosslinking, so that the electrostatic acting force, the complexing action and the like of the BC and metal ions are further improved.
In the step 2), firstly, introducing an active double bond through the open loop of the active hydroxyl of acrylic glycidyl ether and CMC, and then grafting acrylonitrile and p-vinylbenzylphenylselenol in a molecular structure through in-situ free radical polymerization, wherein cyano groups brought by the acrylonitrile have an adsorption effect on heavy metal ions in a water body; the p-vinylbenzylphenylselene can increase steric hindrance effect and improve the contact area with metal ions, wherein selenium, oxygen and sulfur are elements of the same group, so that the p-vinylbenzylphenylselene has better affinity with the metal ions and also has higher adsorption performance.
The modified bacterial cellulose prepared in the steps 1) and 2) and the modified chitosan are mixed to form an adsorbent which can effectively extract Pd in sewage 2+ And Cu 2+ However, the physically mixed system has poor stability, and the diol is used for crosslinking to form hydrogen bond acting force with carboxyl, amino and the like in the molecular structure to form bridging, so that molecules are mutually bridgedThe modified bacterial cellulose and the modified chitosan are connected more firmly by electrostatic adsorption, and more holes are formed on the surface (as shown in figure 1) to form a three-dimensional mesh hole structure, so that the contact area with metal ions is effectively increased, the adsorption capacity is improved, and the adsorption rate is accelerated.
< sorbent adsorption Performance test >
Test adsorbent for heavy metal ion Cu 2+ And Pd 2+ The adsorption performance of the catalyst is simulated, and the wastewater containing heavy metal ions and Cu are simulated 2+ And Pd 2+ The initial concentration of (2) was 1.5mmol/L, and 0.02g of adsorbent was added to 100ml of the simulated solution, followed by shaking for a certain period of time. The pH of the solution was adjusted, as can be seen in FIG. 2, the adsorbent was on Cu 2+ And Pd 2+ The adsorption capacity of the adsorbent is gradually increased along with the increase of pH, the adsorption capacity is low under the strong acid condition, the adsorbent is unstable in a strong acid solution, and the adsorption capacity is rapidly increased under the weak acid condition along with the increase of the pH value and reaches the maximum value when the adsorbent is neutral; as can be seen from FIG. 3, the adsorbent is on Cu 2+ And Pd 2+ The amount of adsorption of (b) gradually increases with time.
Adsorption amount = (C) 0 -C)V/m，C 0 C is the concentration (mg/L) of metal ions in the solution before and after adsorption, and V is the volume (L) of the added solution; m is the mass (g) of the adsorbent.
< adsorbent recyclability >
Filtering the adsorbent (pH =7, adsorbing for 2 h) after the saturation adsorption, adding the filtered adsorbent into 100ml of EDTA-2Na, oscillating for 2h, testing the concentration of the heavy metal ions released in the liquid, repeating for 10 times, and calculating the desorption rate = (C 'V'/mq), wherein C 'is the concentration (mg/L) of the heavy metal ions in the desorbed solution, V' is the volume (L) of the solution, m is the mass (g) of the adsorbent, and q is the adsorption capacity (mg/g). First desorption rate of Cu 2+ And Pd 2+ 96.4% and 95.6%.
The test proves that the adsorbent prepared by the scheme has heavy metal ion Cu 2+ And Pd 2+ Has higher adsorption performance, the adsorption capacity can respectively reach 352.8mg/g and 503.6mg/g, the stability is high, and the heavy metal ions still have higher performance after ten times of adsorption-desorptionThe adsorption performance of (3).
< comparative experiment >
In order to verify the high efficiency of the adsorbent, the following comparative experiment is also carried out.
Comparative example 1:
the commercially available 1:1 mixture of chitosan and bacterial cellulose was used as the adsorbent to adsorb heavy metal ions, and the test method was the same as above. Heavy metal ion Cu 2+ And Pd 2+ The adsorption amounts of (A) and (B) were 38.55mg/g and 30.12mg/g, respectively, and the stability of the adsorbent was poor, so that it was impossible to recycle it.
Comparative example 2:
directly mixing the modified bacterial cellulose prepared in the step 1) and the modified chitosan prepared in the step 2) according to 1:1 to prepare an adsorbent, and adsorbing heavy metal ions by the adsorbent, wherein the test method is the same as the above. Heavy metal ion Cu 2+ And Pd 2+ The adsorption amounts of the components are 268.4mg/g and 350.47mg/g respectively; the stability of the adsorbent is not high, and the adsorption rate of heavy metal ions decreases after the third adsorption-desorption cycle.
< application >
Introducing the sewage containing heavy metals after primary treatment into a microbial pool to remove organic matters in the water body, and measuring Cu in the sewage 2+ And Pd 2+ Was adjusted to pH 7, and then passed through an adsorption column packed with an adsorbent at a rate of 10 BV/h;
discharging the effluent after the heavy metal content reaches the standard after the effluent is adsorbed by the adsorption column, and returning to the adsorption column for continuous adsorption treatment if the heavy metal content does not reach the standard; finally, washing the adsorption column by using 1.5mmol/L EDTA-2Na at the flow rate of 1BV/h, collecting eluent, and obtaining liquid containing heavy metal ions in the eluent, wherein the recovery rate is more than 95%.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (7)
1. A process for extracting heavy metal ions in sewage is characterized by comprising the following steps:
s1: preparation of the adsorbent
1) Adding bacterial cellulose hydrogel, 2-acrylamide-2-methylpropanesulfonic acid, an initiator ammonium persulfate and a cross-linking agent N, N' -methylene bisacrylamide into a reaction bottle, and heating to react for 3-5 hours under the protection of nitrogen;
2) Dissolving N-carboxymethyl chitosan in a reaction bottle by adding an organic solvent, dropwise adding glycidyl acrylate into the reaction bottle to perform an open-loop reaction, continuously adding acrylonitrile, p-vinylbenzyl phenyl selenide and ammonium persulfate into the reaction bottle after the reaction is finished, and heating to react for 2-4 hours under the protection of nitrogen;
3) Cooling and mixing the final reaction systems obtained in the steps 1) and 2), adjusting the pH value to be alkaline, adding glycol selenide, heating to 70 ℃, and stirring for 5-6 hours; washing the obtained solid with water, freeze-drying, and pulverizing to obtain adsorbent;
s2: introducing the sewage containing heavy metals after primary treatment into a microbial pool to remove organic matters in a water body, and then passing through an adsorption column filled with an adsorbent;
s3: discharging the effluent after the heavy metal content reaches the standard after the effluent is adsorbed by the adsorption column, and returning to the adsorption column for continuous adsorption treatment if the heavy metal content does not reach the standard; finally, washing the adsorption column by EDTA-2Na, and collecting the eluent.
2. The process for extracting heavy metal ions from sewage as claimed in claim 1, wherein the mass ratio of the bacterial cellulose hydrogel to 2-acrylamido-2-methylpropanesulfonic acid, the initiator ammonium persulfate and the crosslinking agent N, N' -methylenebisacrylamide in step 1) is from 10 to 30.
3. The process for extracting heavy metal ions from sewage as claimed in claim 1, wherein the mass ratio of the N-carboxymethyl chitosan to the glycidyl acrylate in the step 2) is 1:2.5 to 3.5; the mass ratio of the acrylonitrile to the p-vinylbenzylphenylselenane to the ammonium persulfate to the N-carboxymethyl chitosan is 1-5.
4. The process for extracting heavy metal ions from sewage as claimed in claim 1, wherein the reaction temperature of step 1) and step 2) is 60-70 ℃.
5. The process for extracting heavy metal ions from sewage as claimed in claim 1, wherein the flow rate of the feed water to the adsorption column is 10-20 BV/h.
6. The process for extracting heavy metal ions from wastewater as claimed in claim 1, wherein the heavy metal ions comprise Pd 2+ And Cu 2+ 。
7. The process for extracting heavy metal ions in sewage as claimed in claim 1, wherein the concentration of EDTA-2Na is 1.5mmol/L, and the flow rate is 0.5-2 BV/h.
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