CN110586023B - Sulfur-modified chalcopyrite adsorbing material, preparation method and application thereof - Google Patents
Sulfur-modified chalcopyrite adsorbing material, preparation method and application thereof Download PDFInfo
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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Abstract
The invention discloses a sulfur-modified chalcopyrite adsorbing material, a preparation method and application thereof, belonging to the technical field of energy and environment, wherein the preparation method comprises the steps of crushing chalcopyrite and sulfur, and sieving for later use; filling sulfur powder into a container containing cyclohexane, heating to 70-90 ℃, preserving heat until sulfur is completely dissolved, adding brass ore powder, sealing the container, placing the container on an oscillator, carrying out oscillation reaction for 24 hours to obtain a sulfur-modified chalcopyrite adsorbing material, and drying under a nitrogen atmosphere to constant weight to obtain the sulfur-modified chalcopyrite adsorbing material. The sulfur-modified chalcopyrite adsorbing material has good capacity of removing mercury ions in high-salinity industrial wastewater and seawater, and has a high removal rate in a sodium chloride solution with the salinity of 1.55-5.55 g/l; can still effectively remove mercury ions within the range of 20-80 ℃, and can be directly applied to the removal of mercury ions in high-temperature high-salinity industrial wastewater and seawater.
Description
Technical Field
The invention relates to the technical field of energy and environment, in particular to a sulfur-modified chalcopyrite adsorbing material, a preparation method and application thereof.
Background
Mercury is a common pollutant that is released into the environment in large quantities by coal burning, metallurgy, volcanic eruption, and waste disposal. The sewage containing mercury ions is one of factors causing water environment pollution, and mainly comes from waste water discharged by industries such as mining, electro-metallurgy, chemical engineering and the like and filtrate of solid refuse landfills. The mercury-containing wastewater pollution enters animals, plants and even human bodies through the exchange of soil, atmosphere and water, and is enriched by thousands of times under the biological amplification action of a food chain, thereby causing great harm to an ecosystem and human health.
The high salinity industrial mercury polluted wastewater and the polluted seawater are increasingly intensified, and the mercury-containing ions are required to be treated. Common methods for mercury removal for mercury-containing wastewater, such as: precipitation, ion exchange, coagulation sedimentation and activated carbon processes, which are difficult to use for mercury ion removal in high salinity media, are limited by the influence of salinity, secondary pollution or economic cost considerations.
Disclosure of Invention
The invention develops and develops a method for treating industrial high-salinity mercury waste liquid and mercury-polluted seawater pollution by taking two common minerals, namely chalcopyrite and sulfur as raw materials, and realizes the removal of mercury from the high-salinity mercury waste liquid and the mercury-polluted seawater. The material can be repeatedly used after being treated, has better recycling property compared with the traditional adsorbing material, and the used adsorbing agent is easy to separate and recycle, thereby saving the water treatment cost, reducing the possibility of causing secondary pollution and having good economic and environmental benefits.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a preparation method of a sulfur-modified chalcopyrite adsorbing material, which comprises the following steps:
(1) respectively crushing and sieving the chalcopyrite and the sulfur for later use;
(2) filling sulfur powder into a container containing cyclohexane, heating to 70-90 ℃, and keeping the temperature until sulfur is completely dissolved;
(3) adding the brass ore powder into the container obtained in the step (2), sealing the container, placing the container on an oscillator, and carrying out oscillation reaction for 24 hours to obtain a sulfur-modified brass ore adsorbing material;
(4) carrying out suction filtration, and taking out the sulfur-modified chalcopyrite adsorbing material;
(5) and drying the sulfur-modified chalcopyrite adsorbing material under the nitrogen atmosphere to constant weight to obtain the sulfur-modified chalcopyrite adsorbing material.
As a further improvement of the invention, in the step (1), a sieve with 60-80 meshes is screened.
As a further improvement of the invention, the mass ratio of the chalcopyrite to the sulfur is 4: 1.
As a further improvement of the invention, the drying temperature of the step (5) is 80-120 ℃.
The invention also provides a sulfur-modified chalcopyrite adsorbing material prepared by the preparation method.
The invention also provides application of the sulfur-modified chalcopyrite adsorbing material in removing mercury ions, and the sulfur-modified chalcopyrite adsorbing material is applied to removing mercury ions in high-salinity industrial wastewater and seawater.
The high-salinity industrial wastewater is industrial wastewater with salt mass fraction of 3-5%.
The application method of the sulfur-modified chalcopyrite adsorbing material comprises the steps of putting the sulfur-modified chalcopyrite adsorbing material into high-salinity industrial wastewater or seawater, and adsorbing for 10-14 hours at the temperature of 20-80 ℃.
The addition amount of the sulfur-modified chalcopyrite adsorbing material is 20 g/L.
After the sulfur-modified chalcopyrite adsorbing material disclosed by the invention adsorbs mercury, the adsorbing material can be regenerated by adding sodium sulfide. The adsorption material can be regenerated by adding sodium sulfide to elute mercury adsorbed by the chalcopyrite, and then repeating the previous sulfur modification operation on the chalcopyrite again.
The invention discloses the following technical effects:
the chalcopyrite and sulfur are used as raw materials, the raw materials are wide in source, large in storage capacity and convenient to recover, and the developed sulfur modified chalcopyrite adsorbent is cheap and easy to obtain, large in adsorption capacity, good in treatment effect, free of secondary pollution and good in application prospect in the aspect of removing industrial mercury-containing wastewater and marine mercury pollution.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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.
The method for measuring the content of mercury ions is a conventional technical means in the field, is not the essential point of the invention, and is not described herein in detail.
Example 1
(1) Respectively crushing chalcopyrite and sulfur, and sieving with a 60-mesh sieve for later use;
(2) filling sulfur powder into a container containing cyclohexane, heating to 80 ℃, and keeping the temperature until sulfur is completely dissolved;
(3) after the sulfur is completely dissolved, adding the brass ore powder into the container in the step (2), sealing the container, placing the container on an oscillator, and carrying out oscillation reaction for 24 hours to enable the sulfur to be adsorbed on the chalcopyrite to the maximum extent, so as to obtain a sulfur-modified chalcopyrite adsorbing material;
(4) carrying out suction filtration, taking out the sulfur-modified chalcopyrite adsorbing material, and evaporating the solvent on the surface to dryness;
(5) drying the sulfur-modified chalcopyrite adsorbing material at 80 ℃ in a nitrogen atmosphere to constant weight to obtain the sulfur-modified chalcopyrite adsorbing material;
(6) 2g of sulfur-modified chalcopyrite adsorbing material is put into 100mL of mercury-polluted water solution with the mercury ion concentration of 8.6ppm and the sodium chloride concentration of 1.55g/L, the mixture is uniformly stirred and adsorbed at the temperature of 20 ℃ for 12 hours, and the content of residual mercury ions is measured to obtain the mercury removal rate of 96.87%. After the adsorbing material adsorbs mercury, adding sodium sulfide to elute the adsorbed mercury, and then repeating the previous sulfur modification operation on the chalcopyrite again to regenerate the adsorbing material.
Example 2
(1) Respectively crushing chalcopyrite and sulfur, and sieving with a 80-mesh sieve for later use;
(2) filling sulfur powder into a container containing cyclohexane, heating to 80 ℃, and keeping the temperature until sulfur is completely dissolved;
(3) after the sulfur is completely dissolved, adding the brass ore powder into the container in the step (2), sealing the container, placing the container on an oscillator, and carrying out oscillation reaction for 24 hours to enable the sulfur to be adsorbed on the chalcopyrite to the maximum extent, so as to obtain a sulfur-modified chalcopyrite adsorbing material;
(4) carrying out suction filtration, taking out the sulfur-modified chalcopyrite adsorbing material, and evaporating the solvent on the surface to dryness;
(5) drying the sulfur-modified chalcopyrite adsorbing material at 90 ℃ in a nitrogen atmosphere to constant weight to obtain the sulfur-modified chalcopyrite adsorbing material;
(6) 2g of sulfur-modified chalcopyrite adsorbing material is put into 100mL of mercury-polluted water solution with the mercury ion concentration of 8.6ppm and the sodium chloride concentration of 3.55g/L, the mixture is uniformly stirred and adsorbed at 20 ℃ for 12 hours, the content of the residual mercury ions is measured, the mercury removal rate is 94.65%, after the adsorbing material adsorbs the mercury, sodium sulfide is added to elute the adsorbed mercury, and then the chalcopyrite is subjected to the previous sulfur modification operation again, so that the adsorbing material can be regenerated.
Example 3
(1) Crushing chalcopyrite and sulfur, and sieving with a 90-mesh sieve for later use;
(2) filling sulfur powder into a container containing cyclohexane, heating to 80 ℃, and keeping the temperature until sulfur is completely dissolved;
(3) after the sulfur is completely dissolved, adding the brass ore powder into the container in the step (2), sealing the container, placing the container on an oscillator, and carrying out oscillation reaction for 24 hours to enable the sulfur to be adsorbed on the chalcopyrite to the maximum extent, so as to obtain a sulfur-modified chalcopyrite adsorbing material;
(4) carrying out suction filtration, taking out the sulfur-modified chalcopyrite adsorbing material, and evaporating the solvent on the surface to dryness;
(5) drying the sulfur-modified chalcopyrite adsorbing material at 100 ℃ in a nitrogen atmosphere to constant weight to obtain the sulfur-modified chalcopyrite adsorbing material;
(6) 2g of sulfur-modified chalcopyrite adsorbing material is put into 100mL of mercury-polluted water solution with the mercury ion concentration of 8.6ppm and the sodium chloride concentration of 5.55g/L, the mixture is uniformly stirred and adsorbed at 20 ℃ for 12 hours, the content of the residual mercury ions is measured, the mercury removal rate is 90.87%, after the adsorbing material adsorbs the mercury, sodium sulfide is added to elute the adsorbed mercury, and then the chalcopyrite is subjected to the previous sulfur modification operation again, so that the adsorbing material can be regenerated.
Example 4
(1) Crushing chalcopyrite and sulfur, and sieving with a 60-mesh sieve for later use;
(2) filling sulfur powder into a container containing cyclohexane, heating to 80 ℃, and keeping the temperature until sulfur is completely dissolved;
(3) after the sulfur is completely dissolved, adding the brass ore powder into the container in the step (2), sealing the container, placing the container on an oscillator, and carrying out oscillation reaction for 24 hours to enable the sulfur to be adsorbed on the chalcopyrite to the maximum extent, so as to obtain a sulfur-modified chalcopyrite adsorbing material;
(4) carrying out suction filtration, taking out the sulfur-modified chalcopyrite adsorbing material, and evaporating the solvent on the surface to dryness;
(5) drying the sulfur-modified chalcopyrite adsorbing material at 80 ℃ in a nitrogen atmosphere to constant weight to obtain the sulfur-modified chalcopyrite adsorbing material;
(6) 2g of sulfur-modified chalcopyrite adsorbing material is put into 100mL of mercury-polluted water solution with the mercury ion concentration of 8.6ppm and the sodium chloride concentration of 1.55g/L, the mixture is uniformly stirred and adsorbed at 35 ℃ for 12 hours, the content of the residual mercury ions is measured, the mercury removal rate is 94.30%, after the adsorbing material adsorbs the mercury, sodium sulfide is added to elute the adsorbed mercury, and then the previous sulfur modification operation is repeated again on the chalcopyrite, so that the adsorbing material can be regenerated.
Example 5
(1) Crushing chalcopyrite and sulfur, and sieving with a 60-mesh sieve for later use;
(2) filling sulfur powder into a container containing cyclohexane, heating to 80 ℃, and keeping the temperature until sulfur is completely dissolved;
(3) after the sulfur is completely dissolved, adding the brass ore powder into the container in the step (2), sealing the container, placing the container on an oscillator, and carrying out oscillation reaction for 24 hours to enable the sulfur to be adsorbed on the chalcopyrite to the maximum extent, so as to obtain a sulfur-modified chalcopyrite adsorbing material;
(4) carrying out suction filtration, taking out the sulfur-modified chalcopyrite adsorbing material, and evaporating the solvent on the surface to dryness;
(5) drying the sulfur-modified chalcopyrite adsorbing material at 80 ℃ in a nitrogen atmosphere to constant weight to obtain the sulfur-modified chalcopyrite adsorbing material;
(6) 2g of sulfur-modified chalcopyrite adsorbing material is put into 100mL of mercury-polluted water solution with the mercury ion concentration of 8.6ppm and the sodium chloride concentration of 5.55g/L, the mixture is uniformly stirred and adsorbed at 50 ℃ for 12 hours, the content of the residual mercury ions is measured, the mercury removal rate is 87.68 percent, after the adsorbing material adsorbs the mercury, sodium sulfide is added to elute the adsorbed mercury, and then the previous sulfur modification operation is repeated again on the chalcopyrite, so that the adsorbing material can be regenerated.
Example 6
(1) Crushing chalcopyrite and sulfur, and sieving with a 60-mesh sieve for later use;
(2) filling sulfur powder into a container containing cyclohexane, heating to 80 ℃, and keeping the temperature until sulfur is completely dissolved;
(3) after the sulfur is completely dissolved, adding the brass ore powder into the container in the step (2), sealing the container, placing the container on an oscillator, and carrying out oscillation reaction for 24 hours to enable the sulfur to be adsorbed on the chalcopyrite to the maximum extent, so as to obtain a sulfur-modified chalcopyrite adsorbing material;
(4) carrying out suction filtration, taking out the sulfur-modified chalcopyrite adsorbing material, and evaporating the solvent on the surface to dryness;
(5) drying the sulfur-modified chalcopyrite adsorbing material at 80 ℃ in a nitrogen atmosphere to constant weight to obtain the sulfur-modified chalcopyrite adsorbing material;
(6) 2g of sulfur-modified chalcopyrite adsorbing material is put into 100mL of mercury polluted water solution with mercury ion concentration of 8.6ppm and sodium chloride concentration of 5.55g/L, the materials are mixed and stirred uniformly, the mixture is adsorbed for 12 hours at 78 ℃, the content of residual mercury ions is measured, the mercury removal rate is 94.60 percent, after the adsorbing material adsorbs the mercury, sodium sulfide is added to elute the adsorbed mercury, and then the previous sulfur modification operation is repeated again on the chalcopyrite, so that the adsorbing material can be regenerated.
Comparative example 1
2g of chalcopyrite adsorbing material without being modified by sulfur (the pretreatment method and the crushing degree are the same as those in example 1) is put into 100ml of mercury polluted water solution with the mercury ion concentration of 8.6ppm and the sodium chloride concentration of 1.55g/L, the mixture is uniformly mixed and stirred, the mercury is adsorbed for 12 hours at the temperature of 20 ℃, and the content of the residual mercury ions is measured, so that the mercury removal rate is 46.51 percent.
Comparative example 2
2g of chalcopyrite adsorbing material without being modified by sulfur (the pretreatment method and the crushing degree are the same as those in example 1) is put into 100mL of mercury polluted water solution with the mercury ion concentration of 8.6ppm and the sodium chloride concentration of 5.55g/L, the mixture is uniformly stirred and adsorbed for 12 hours at the temperature of 20 ℃, and the content of the residual mercury ions is measured to obtain the mercury removal rate of 35.25 percent.
Comparative example 3
2g of chalcopyrite adsorbing material without being modified by sulfur (the pretreatment method and the crushing degree are the same as those in example 1) is put into 100ml of mercury polluted water solution with the mercury ion concentration of 8.6ppm and the sodium chloride concentration of 5.55g/L, the mixture is uniformly stirred and adsorbed for 12 hours at 50 ℃, and the content of the residual mercury ions is measured to obtain the mercury removal rate of 24.37 percent.
Comparative example 4
2g of chalcopyrite adsorbing material without being modified by sulfur (the pretreatment method and the crushing degree are the same as those in example 1) is put into 100ml of mercury polluted water solution with the mercury ion concentration of 8.6ppm and the sodium chloride concentration of 5.55g/L, the mixture is uniformly stirred and adsorbed for 12 hours at 78 ℃, and the content of the residual mercury ions is measured to obtain the mercury removal rate of 19.26 percent.
Comparative example 5
Putting 2g of a certain commercial activated carbon adsorption material into 100ml of mercury-polluted water solution with the mercury ion concentration of 8.6ppm and the sodium chloride concentration of 1.55g/L, uniformly mixing and stirring, adsorbing at 20 ℃ for 12 hours, and measuring the content of residual mercury ions to obtain the mercury removal rate of 79.26%.
Comparative example 6
Putting 2g of a certain commercial activated carbon adsorption material into 100ml of mercury-polluted water solution with the mercury ion concentration of 8.6ppm and the sodium chloride concentration of 5.55g/L, uniformly mixing and stirring, adsorbing at 78 ℃ for 12 hours, and measuring the content of residual mercury ions to obtain the mercury removal rate of 39.37%.
The invention comprehensively utilizes the surface property of the chalcopyrite and the dual property of the combination of the sulfur (ions) and the mercury ions. Chalcopyrite has a certain adsorption effect, but the adsorption effect is very poor without sulfur modification treatment (see examples and comparative examples). The absorbing material is the chalcopyrite modified by the sulfur, the chalcopyrite is a body, the sulfur is a modifier, the problem of secondary pollution caused by excessive dissolution in the process of absorbing the mercury by the sulfide is avoided, and the sulfide is used for absorbing the waste liquid with complex components and the mercury in a seawater system and hardly causes the secondary pollution. The adsorption material has wide sources and low cost, and the sulfur-modified chalcopyrite is solid, so that the adsorbate and the adsorbent are easy to separate after adsorbing mercury ions, elute and regenerate. Meanwhile, the results show that the sulfur-modified chalcopyrite adsorbing material prepared in the organic solvent medium has good capacity of removing mercury ions in high-salinity industrial wastewater and seawater. Along with the increase of the salinity, the efficiency of removing mercury ions from the chalcopyrite is gradually reduced, and the chalcopyrite has higher removal rate under a sodium chloride solution with the salinity of 1.55-5.55 g/L; can still effectively remove mercury ions within the range of 20-80 ℃, and can be directly applied to the removal of mercury ions in high-temperature high-salinity industrial wastewater and seawater. The optimal concentration for removing mercury ions is salinity of 1.55g/L and temperature of 20 ℃.
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. A preparation method of a sulfur-modified chalcopyrite adsorbing material is characterized by comprising the following steps:
(1) respectively crushing and sieving the chalcopyrite and the sulfur for later use;
(2) filling sulfur powder into a container containing cyclohexane, heating to 70-90 ℃, and keeping the temperature until sulfur is completely dissolved;
(3) adding the brass ore powder into the container obtained in the step (2), sealing the container, placing the container on an oscillator, and carrying out oscillation reaction for 24 hours to obtain a sulfur-modified brass ore adsorbing material;
(4) carrying out suction filtration, and taking out the sulfur-modified chalcopyrite adsorbing material;
(5) drying the sulfur-modified chalcopyrite adsorbing material in a nitrogen atmosphere to constant weight to obtain the sulfur-modified chalcopyrite adsorbing material;
the mass ratio of the chalcopyrite to the sulfur is 4: 1.
2. The preparation method of the sulfur-modified chalcopyrite adsorbing material according to claim 1, wherein the drying temperature in the step (5) is 80-120 ℃.
3. The preparation method of the sulfur-modified chalcopyrite adsorbing material according to claim 1, wherein the step (1) is carried out by sieving with a sieve of 60-80 meshes.
4. A sulfur-modified chalcopyrite adsorbing material, which is characterized by being prepared by the preparation method of any one of claims 1 to 3.
5. The application of the sulfur-modified chalcopyrite adsorbing material in removing mercury ions in claim 4, wherein the sulfur-modified chalcopyrite adsorbing material is applied to removing mercury ions in high-salinity industrial wastewater and seawater.
6. The use according to claim 5, wherein the high salinity industrial wastewater is industrial wastewater with a salt mass fraction of 3% to 5%.
7. The application of claim 5, wherein the application method comprises the step of putting the sulfur-modified chalcopyrite adsorbing material into high-salinity industrial wastewater or seawater, and adsorbing for 10-14 hours at the temperature of 20-80 ℃.
8. The use of claim 5, wherein the sulfur-modified chalcopyrite sorbent material adsorbs mercury and the sorbent material is regenerated by the addition of sodium sulfide.
9. The use according to claim 5, wherein the sulphur-modified chalcopyrite adsorbing material is added in an amount of 20 g/L.
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