CN107010706B - Method for separating copper salt in water by using peanut shell extract - Google Patents

Method for separating copper salt in water by using peanut shell extract Download PDF

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CN107010706B
CN107010706B CN201710341497.7A CN201710341497A CN107010706B CN 107010706 B CN107010706 B CN 107010706B CN 201710341497 A CN201710341497 A CN 201710341497A CN 107010706 B CN107010706 B CN 107010706B
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peanut shell
solution
extraction
water
peanut
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CN107010706A (en
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孙立权
李林强
姜亚丽
赵峰强
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Shandong Changyi Aoli Salinization Co ltd
Changyi Yinjiang Biotechnology Co ltd
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Shandong Changyi Aoli Salinization Co ltd
Changyi Yinjiang Biotechnology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5263Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention provides a method for separating copper salt in water by using a peanut shell extract, which comprises the following steps: A. selecting a peanut shell without mildew, washing the peanut shell with clear water to remove dirt on the surface, and soaking the peanut shell in an extraction solution; B. taking the soaked materials, putting the soaked materials into a vessel with a mechanical stirring pipe and a spherical condenser pipe, and placing the vessel into a heater for heating reflux extraction; C. after the reflux extraction is finished, performing solid-liquid separation on the peanut shell powder and the extraction solution; D. adjusting the pH value of the peanut shell extracting solution to be alkaline, adding the peanut shell extracting solution into an aqueous solution containing copper ions according to a certain proportion, adjusting the pH value, stirring, and then standing to obtain flocculent precipitates; E. and (4) carrying out solid-liquid separation, taking out the precipitate, and obtaining water with low copper ion concentration. Therefore, the method utilizes the waste agricultural materials, is applied to wastewater treatment, can remove copper ions in water with high selectivity, has stronger adsorption specificity than that of peanut shells, reduces the cost of water treatment, and improves the utilization value of the peanut shells.

Description

Method for separating copper salt in water by using peanut shell extract
Technical Field
The invention relates to the technical field of heavy ion water treatment, in particular to a method for separating copper salt in water by using a peanut shell extract.
Background
Peanuts are an important economic crop in China, and are particularly widely distributed in the north of China as oil crops. After a large amount of peanut kernels are used as oil resources, only a small amount of peanut shells, peanut straws and the like are used as wastes and used as feeds or fuels, and therefore, the utilization value of the peanut shells, the peanut straws and the like as a biomass resource is further improved. From the utilization condition of peanut shells in China at present, a plurality of scientists recognize the value of the peanut shells, but the peanut shells have a long distance from practical application.
In order to reduce resource waste and environmental pollution caused by burning or throwing away peanut shell agricultural waste as agricultural waste, people utilize the peanut shell to adsorb heavy metal ions such as mercury and the like, people further modify the peanut shell, talk about the peanut shell through a physical and chemical method, and utilize the fiber structure of the peanut shell to have stronger adsorption capacity on ions to treat water containing various heavy metal ions.
Disclosure of Invention
In view of the above-mentioned drawbacks, the present invention provides a method for separating copper salt from water by using peanut shell extract, which can effectively remove copper ions from water.
In order to achieve the above object, the present invention provides a method for separating copper salt in water by using peanut shell extract, comprising the following steps:
A. selecting a peanut shell without mildew, washing the peanut shell with clear water to remove dirt on the surface, and soaking the peanut shell in an extraction solution;
B. taking the soaked materials, putting the soaked materials into a vessel with a mechanical stirring pipe and a spherical condenser pipe, and placing the vessel into a heater for heating reflux extraction;
C. after the reflux extraction is finished, performing solid-liquid separation on the peanut shell powder and the extraction solution;
D. adjusting the pH value of the peanut shell extracting solution to be alkaline, adding the peanut shell extracting solution into an aqueous solution containing copper ions according to a certain proportion, adjusting the pH value, stirring, and then standing to obtain flocculent precipitates;
E. and (4) carrying out solid-liquid separation, taking out the precipitate, and obtaining water with low copper ion concentration.
According to the method for separating the copper salt in the water by using the peanut shell extract, the step C also comprises the following steps:
filtering with funnel, adding the residue into the extractive solution again, and extracting for the second time.
According to the method for separating the cupric salt in the water by using the peanut shell extract, the vessel with the mechanical stirring and the spherical condenser pipe is a three-mouth flask.
According to the method for separating the copper salt in the water by using the peanut shell extract, in the step A, the material-liquid ratio of the peanut shell to the extraction solution is 1g/30 ml-1 g/10 ml;
the extraction solution was a 0.001M NaOH solution.
According to the method for separating the copper salt in the water by using the peanut shell extract, the amount and the concentration of the extracting solution adopted by the second extraction in the step C are the same as those of the extracting solution in the step A.
According to the method for separating the copper salt in the water by using the peanut shell extract, the heating temperature in the step B is 60-100 ℃, and the heating time is 20-240 min.
According to the method for separating the cupric salt in the water by using the peanut shell extract, the PH value is controlled to be 7.5-12.5 in the step D.
The invention provides a method for separating copper salt in water by using a peanut shell extract, which comprises the following steps: a. Selecting a peanut shell without mildew, washing the peanut shell with clear water to remove dirt on the surface, and soaking the peanut shell in an extraction solution; B. taking the soaked materials, putting the soaked materials into a vessel with a mechanical stirring pipe and a spherical condenser pipe, and placing the vessel into a heater for heating reflux extraction; C. after the reflux extraction is finished, performing solid-liquid separation on the peanut shell powder and the extraction solution; d. Adjusting the pH value of the peanut shell extracting solution to be alkaline, adding the peanut shell extracting solution into an aqueous solution containing copper ions according to a certain proportion, adjusting the pH value, stirring, and then standing to obtain flocculent precipitates; E. and (4) carrying out solid-liquid separation, taking out the precipitate, and obtaining water with low copper ion concentration. Therefore, the method utilizes the waste agricultural materials, is applied to wastewater treatment, can remove copper ions in water with high selectivity, has stronger adsorption specificity than that of peanut shells, reduces the cost of water treatment, and improves the utilization value of the peanut shells.
Drawings
FIG. 1 is a schematic representation of the structure of luteolin of the present invention;
FIG. 2 is a schematic diagram of the eriodictyol structure of the present invention;
FIG. 3 is a schematic diagram of the structure of 5, 7-dihydroxy chromones of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
On the basis of research on main effective components of peanut shells, the inventor fully utilizes flavonoid compounds in the effective components of the peanut shells and utilizes the characteristics that the extract contains a large amount of flavonoid compounds, and the structure of the extract contains a large amount of hydroxyl, carbonyl and the like. For example, the flavonoids in the peanut shell extract include luteolin (shown in figure 1), eriodictyol (shown in figure 2) and 5, 7-dihydroxy chromone (shown in figure 3), and the outer layer of a large number of heavy metal ion atoms has a plurality of 3d layers and a plurality of electrons, and can easily form complexes with some ligands. The outer electronic configuration of the copper ion Cu2+ ion is 3s 23 p 63 d9, and coordination numbers of 2,4,5 and 6.2 and 5 are rare, mainly 4 and 6 can be formed.
Therefore, a method for separating copper ions from water containing copper ions by using an extract of peanut shells has been developed, which utilizes the characteristic that flavonoids containing carbonyl and hydroxyl groups easily form complexes with copper ions and uses the extract for separating copper ions from water containing copper ions. The method is simple and has excellent separation effect, and can be used in the fields of wastewater treatment work containing a large amount of copper ions, reduction of copper ions in industrial water and the like.
Specifically, the invention provides a method for separating copper salt in water by using a peanut shell extract, which comprises the following steps:
A. selecting peanut shells without mildew, washing with clear water to remove dirt on the surfaces, and soaking in the extraction solution.
In the step, the soaking time is controlled to be 1-48 hours, the soaking solution can be selected from potassium carbonate, sodium bicarbonate, sodium hydroxide, potassium hydroxide and the like, the pH value of the soaking solution is 8-12, and the solid-to-liquid ratio of soaking is 1g/30 ml-1 g/10 ml.
B. Taking the soaked materials, putting the soaked materials into a vessel with a mechanical stirring pipe and a spherical condenser pipe, and placing the vessel into a heater for heating reflux extraction. In the step, a three-mouth beaker is adopted as a vessel, the heating temperature is controlled to be 60-100 ℃, and the heating time is 20-240 min.
C. After the reflux extraction is finished, the peanut shell powder and the extraction solution are subjected to solid-liquid separation.
In this step, a second extraction may be performed, for example, by filtering with a funnel, and adding the residue to the extraction solution again for the second extraction to improve the extraction rate.
D. Adjusting the pH value of the peanut shell extracting solution to be alkaline, adding the peanut shell extracting solution into an aqueous solution containing copper ions according to a certain proportion, adjusting the pH value, stirring, and then standing to obtain flocculent precipitates. In this step, the alkaline pH is controlled to be 7.5-12.5. The molar ratio of the copper ions to the copper ions is 1/1-4/1, and the solution volume ratio is 0.1/1-0.5/1.
E. And (4) carrying out solid-liquid separation, taking out the precipitate, and obtaining water with low copper ion concentration. In the step, solid-liquid separation is carried out by adopting filtration or centrifugal separation.
Because the peanut shells are low in price, the peanut shells are directly extracted without being dried and crushed. The invention simplifies the extraction operation process, reduces the extraction cost and makes the extraction process easier to operate. And the peanut shells are made of local materials in the production place, so that the transportation cost is saved, and the cost is reduced. The selection of the alkali liquor is various, the source is wide, the requirement on equipment is not high, and the energy is saved. The water treatment step is simple, the treatment cost is reduced, and the copper complex can be obtained.
In one embodiment of the invention, the method for separating copper salt in water by using the peanut shell extract comprises the following steps:
A. selecting peanut shells without mildew, washing with clear water to remove dirt on the surfaces, and soaking in the extraction solution.
In the step, the soaking time is 1 hour, the soaking solution is sodium hydroxide, the pH value of the soaking solution is 8, and the solid-liquid ratio of soaking is 1g/30 ml.
B. Taking the soaked materials, putting the soaked materials into a vessel with a mechanical stirring pipe and a spherical condenser pipe, and placing the vessel into a heater for heating reflux extraction. In the step, a three-mouth beaker is adopted as a vessel, the heating temperature is controlled at 60 ℃, and the heating time is 20 min.
C. After the reflux extraction is finished, the peanut shell powder and the extraction solution are subjected to solid-liquid separation.
In this step, a second extraction may be performed, for example, by filtering with a funnel, and adding the residue to the extraction solution again for the second extraction to improve the extraction rate.
D. Adjusting the pH value of the peanut shell extracting solution to be alkaline, adding the peanut shell extracting solution into an aqueous solution containing copper ions according to a certain proportion, adjusting the pH value, stirring, and then standing to obtain flocculent precipitates. The alkaline pH was controlled to 7.5 in this step. The molar ratio to copper ions was 1/1, which was converted to a solution volume ratio of 0.1/1.
E. And (4) carrying out solid-liquid separation, taking out the precipitate, and obtaining water with low copper ion concentration. In the step, solid-liquid separation is carried out by adopting filtration or centrifugal separation.
In another embodiment of the present invention, a method for separating copper salts from water using peanut shell extract comprises the steps of:
A. selecting peanut shells without mildew, washing with clear water to remove dirt on the surfaces, and soaking in the extraction solution.
In the step, the soaking time is controlled to be 48 hours, the soaking solution is sodium hydroxide solution, the pH value of the soaking solution is 12, and the solid-to-liquid ratio of soaking is 1g/10 ml.
B. Taking the soaked materials, putting the soaked materials into a vessel with a mechanical stirring pipe and a spherical condenser pipe, and placing the vessel into a heater for heating reflux extraction. In the step, a three-mouth beaker is adopted as a vessel, the heating temperature is controlled at 100 ℃, and the heating time is 240 min.
C. After the reflux extraction is finished, the peanut shell powder and the extraction solution are subjected to solid-liquid separation.
In this step, a second extraction may be performed, for example, by filtering with a funnel, and adding the residue to the extraction solution again for the second extraction to improve the extraction rate.
D. Adjusting the pH value of the peanut shell extracting solution to be alkaline, adding the peanut shell extracting solution into an aqueous solution containing copper ions according to a certain proportion, adjusting the pH value, stirring, and then standing to obtain flocculent precipitates. The alkaline pH was controlled to 12.5 in this step. The molar ratio to copper ions was 4/1, which was converted to a solution volume ratio of 0.5/1.
E. And (4) carrying out solid-liquid separation, taking out the precipitate, and obtaining water with low copper ion concentration. In the step, solid-liquid separation is carried out by adopting filtration or centrifugal separation.
Because the peanut shells are low in price, the peanut shells are directly extracted without being dried and crushed. The invention simplifies the extraction operation process, reduces the extraction cost and makes the extraction process easier to operate. And the peanut shells are made of local materials in the production place, so that the transportation cost is saved, and the cost is reduced. The selection of the alkali liquor is various, the source is wide, the requirement on equipment is not high, and the energy is saved. The water treatment steps are simple, the treatment cost is reduced, and the copper complex can be obtained
In a specific application of the present invention, the method comprises the following steps:
(1) taking 30g of peanut shells for cleaning, and soaking the cleaned peanut shells in 500mL of 0.001M NaOH solution for 1 hour;
(2) and (2) adding the mixture obtained in the step (1) into a three-neck flask with a mechanical stirrer and a condenser, heating and refluxing for extraction for 2 hours, then filtering by using a Buchner funnel, and separating solid peanut shell residues and an extracting solution.
Extracting the above residue with NaOH solution of the same concentration and volume for 2 hr to obtain extractive solution, and mixing with the first extractive solution.
(3) And (3) cooling 1000mL of the extracting solution obtained in the step (2), adjusting the pH value, adding 100mL of the extracting solution into 1L of 1000mg/L copper ion solution, stirring, standing for 30min after 1 hour. Flocculent precipitate appeared in the solution.
(4) And (4) filtering the solution obtained in the step (3) by using a Buchner funnel, filtering out precipitated substances, and reducing the concentration of copper ions in the solution to 1 mg/L.
The method can effectively remove copper ions in the solution and obtain the complex of the flavonoid compound and the copper ions.
In summary, the present invention provides a method for separating copper salt in water by using peanut shell extract, comprising the following steps: A. selecting a peanut shell without mildew, washing the peanut shell with clear water to remove dirt on the surface, and soaking the peanut shell in an extraction solution; B. taking the soaked materials, putting the soaked materials into a vessel with a mechanical stirring pipe and a spherical condenser pipe, and placing the vessel into a heater for heating reflux extraction; C. after the reflux extraction is finished, performing solid-liquid separation on the peanut shell powder and the extraction solution; D. adjusting the pH value of the peanut shell extracting solution to be alkaline, adding the peanut shell extracting solution into an aqueous solution containing copper ions according to a certain proportion, adjusting the pH value, stirring, and then standing to obtain flocculent precipitates; E. and (4) carrying out solid-liquid separation, taking out the precipitate, and obtaining water with low copper ion concentration. Therefore, the method utilizes the waste agricultural materials, is applied to wastewater treatment, can remove copper ions in water with high selectivity, has stronger adsorption specificity than that of peanut shells, reduces the cost of water treatment, and improves the utilization value of the peanut shells.
The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it should be understood that various changes and modifications can be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (5)

1. A method for separating copper salt in water by using peanut shell extract is characterized by comprising the following steps:
A. selecting a peanut shell without mildew, washing the peanut shell with clear water to remove dirt on the surface, and soaking the peanut shell in an extraction solution;
B. taking the soaked materials, putting the soaked materials into a vessel with a mechanical stirring pipe and a spherical condenser pipe, and placing the vessel into a heater for heating reflux extraction;
C. after the reflux extraction is finished, performing solid-liquid separation on the peanut shell powder and the extraction solution;
D. adjusting the pH value of the peanut shell extracting solution to be alkaline, adding the peanut shell extracting solution into an aqueous solution containing copper ions according to a certain proportion, adjusting the pH value, stirring, and then standing to obtain flocculent precipitates;
E. performing solid-liquid separation, taking out the precipitate, and obtaining water with low copper ion concentration;
in the step A, the material-liquid ratio of the peanut shells to the extraction solution is 1g/30 ml-1 g/10 ml;
the extraction solution is a NaOH solution with the concentration of 0.001M;
and controlling the pH value to be 7.5-12.5 in the step D.
2. The method of claim 1, wherein step C further comprises: filtering with funnel, adding the residue into the extractive solution again, and extracting for the second time.
3. The method of claim 1, wherein the vessel with mechanical agitation and spherical condenser is a three-neck flask.
4. The method of claim 2, wherein the amount and concentration of the extraction solution used in the second extraction in step C is the same as the extraction solution in step A.
5. The method for separating copper salts from water by using the peanut shell extract as claimed in claim 1, wherein the heating temperature in the step B is 60-100 ℃ and the heating time is 20-240 min.
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