CN115155517A - Molecular sieve confinement loaded nano iron oxide composite adsorbent and preparation method and application thereof - Google Patents
Molecular sieve confinement loaded nano iron oxide composite adsorbent and 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
- B01J20/10—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
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
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- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28095—Shape or type of pores, voids, channels, ducts
- B01J20/28097—Shape or type of pores, voids, channels, ducts being coated, filled or plugged with specific 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
Abstract
The invention relates to a molecular sieve confinement-loaded nano iron oxide composite adsorbent and a preparation method thereof. The molecular sieve confinement nano iron oxide is prepared by adopting a high-temperature calcination method as a composite adsorbent, and the antimony-containing wastewater is used as an application object. Through the preparation method of the molecular sieve loaded nano iron oxide composite adsorbent, an iron oxide precursor can be loaded inside a pore channel of a mesoporous molecular sieve, high-temperature calcination is carried out, the nano iron oxide grows by utilizing the mesoporous limited domain of the molecular sieve, and the characteristic pore channel characteristics of the mesoporous molecular sieve are kept at the same time, so that the highly stable molecular sieve loaded nano iron oxide composite adsorbent is obtained.
Description
Technical Field
The invention belongs to a heavy metal removal technology in the field of environmental protection, and particularly relates to a molecular sieve loaded nano iron oxide composite adsorbent and a preparation method and application thereof.
Background
Antimony is a widely distributed toxic metal element, the element symbol Sb, mainly exists in sulfide mineral stibnite in nature, coexists with sulfide and oxide of arsenic, and mainly exists in the form of oxyanions of Sb (III) and Sb (V) in water. Antimony and compounds thereof have wide application and can be used for the industries of producing ceramics, glass, batteries, flame retardants and the like, however, because a large amount of antimony-containing substances are not effectively recovered and treated in the production, antimony-containing pollutants are discharged into natural water bodies as waste water wastes, which causes great harm to human health and ecological environment.
At present, the technical methods for treating the antimony-containing wastewater mainly comprise a coagulating sedimentation method, a membrane separation technology, an electrochemical method, a biological enrichment method, an adsorption method and the like, wherein the adsorption method is concerned because of high antimony removal efficiency, simple operation and low cost. The adsorption refers to a process of enriching molecules or ions in surrounding liquid or gas medium on the surface of a solid substance, and the antimony heavy metal ions in the water body are captured by using an adsorbent, so that the aim of removing the antimony heavy metal ions in the water is fulfilled, and the method is one of the most rapid and effective methods. The nano-adsorption material has a large specific surface area and a large surface adsorption activity, and thus, the nano-adsorption material is widely concerned and commonly comprises a carbon-based nano-adsorption material, a nano-metal oxide adsorption material and the like. The nano metal oxide material such as nano iron oxide and the like is proved to be capable of directly or indirectly forming a chemical bond with antimony, shows a stable adsorption effect macroscopically, has the advantages of high adsorption rate, large adsorption capacity, deep removal and the like, becomes a hot spot of an environment adsorption material, has the defects of high cost, easy agglomeration, instability and the like, and becomes a practical problem in the current practical application.
Patent applicationApplication 201910701672.8 discloses a nano zero-valent iron @ molecular sieve composite material, a preparation method and application thereof, comprising the following steps: preparing an iron salt solution, adding a molecular sieve into the iron salt solution, and mechanically stirring under the protection of nitrogen to exchange iron ions into the molecular sieve to obtain a mixed solution A of the molecular sieve and iron salt; carrying out solid-liquid separation on the mixed solution A, mixing the separated solid with water to obtain a mixed reaction solution, adding a reducing agent solution into the mixed reaction solution under the conditions of nitrogen protection and mechanical stirring, and continuously stirring to obtain a mixed solution B; and carrying out solid-liquid separation on the mixed solution B, and washing and drying the separated solid to obtain the nano zero-valent iron @ molecular sieve composite material. However, the growth of the nano zero-valent iron in the invention needs specific nitrogen protection and additional reducing agent, and provides more severe condition limitation on the preparation of the adsorbent; in addition, the nano zero-valent iron @ molecular sieve composite adsorbent is specific to Pb 2+ 、Cu 2+ The heavy metal cations and anions such as arsenite radical and dichromate radical have certain removal effect, and do not show specific adsorption effect on a toxic metal element Sb element.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a molecular sieve confinement-loaded nano iron oxide composite adsorbent which is not easy to agglomerate and has good stability, and a preparation method and application thereof. The enrichment and agglomeration effects of the nano iron oxide adsorbent are solved, effective mass transfer can be realized through the open molecular sieve pore channel, and the adsorption and removal of antimony ions are improved.
The purpose of the invention can be realized by the following technical scheme: a molecular sieve confinement loaded nano iron oxide composite adsorbent comprises a mesoporous molecular sieve and nano iron oxide particles, wherein the nano iron oxide particles are uniformly confined in pore channels of the mesoporous molecular sieve, and the composite adsorbent can be used for removing (similar) metals in wastewater.
A preparation method of a molecular sieve confinement-loaded nano iron oxide composite adsorbent comprises the following steps:
(1) Adding a certain amount of ferric salt into distilled water, and promoting the ferric salt to be fully dissolved by ultrasonic or stirring to obtain a ferric salt solution, wherein the concentration of the ferric salt solution is 1-10g/L generally;
(2) Adding a molecular sieve into the ferric salt solution, and stirring for 3-5 hours by ultrasonic to fully mix the molecular sieve and the ferric salt solution;
(3) Placing the mixed solution in a forced air drying box, and drying;
(4) Fully grinding solid powder, wherein the particle size of the ground solid powder is 1-10 microns, calcining at high temperature, maintaining for a certain time, and naturally cooling;
(5) And (3) cleaning the calcined sample for several times, and drying in vacuum to obtain the molecular sieve loaded nano iron oxide composite adsorbent.
The ferric salt in the step 1 comprises one or a mixture of more of ferric nitrate, ferric sulfate, ferric chloride and ferric acetylacetonate.
The molecular sieve in the step 2 comprises SBA-15, or MCM-41 and the like, and theoretically, mesoporous materials comprise mesoporous silicon, mesoporous alumina, mesoporous titanium oxide and the like, and the purpose can be achieved.
The mass ratio of the molecular sieve to the iron salt in the step 2 is 1.
And 3, the drying temperature of the air drying oven in the step 3 is 30-80 ℃.
The calcining temperature in the step 4 is 200-600 ℃, and the calcining time is 0.5-6 hours.
An application of a molecular sieve confinement loaded nano iron oxide composite adsorbent, which is used for removing antimony pollutants in wastewater. The method specifically comprises the following steps:
adding the composite adsorbent into the wastewater, wherein the adding amount is as follows: the mass ratio of the composite adsorbent to the wastewater is 1:1000-1, 5000, fully mixing, and shaking on a shaking table for 30-60 min to realize effective removal of metal.
Compared with the prior art, the invention has the following advantages:
1. the mesoporous molecular sieve is used as a carrier, has extremely high specific surface area, regular and ordered pore channel structure and narrow pore size distribution, provides sites for the nano iron oxide, and can realize the limited-domain growth of nano iron oxide particles.
2. In the preparation process of the molecular sieve loaded nano iron oxide composite adsorbent, firstly, precursor iron salt of nano iron oxide is fully mixed with the molecular sieve, and Fe is fully mixed in the mixing process 3+ Ions can spontaneously diffuse into the inside of the pore channel of the molecular sieve; then drying the sample, and fully grinding the sample to uniformly mix the sample; calcining at high temperature in air to convert iron salt into nanometer iron oxide, and storing in the pore canal inside the molecular sieve. The mesoporous molecular sieve plays a key role, on one hand, the agglomeration effect of the nano ferric oxide is effectively avoided, the stability of the composite adsorbent is improved, meanwhile, the open pore channel of the molecular sieve provides a high-efficiency mass transfer channel, the mesoporous molecular sieve has high selectivity and sensitivity on heavy metal ions, and the high-efficiency treatment on the wastewater is realized.
3. The preparation method has the advantages of simple preparation process, easy control, larger antimony adsorption capacity, convenient recovery and great reduction of cost.
Drawings
Fig. 1 is a TEM image of the molecular sieve-supported nano iron oxide composite adsorbent prepared in example 1.
Fig. 2 is a TEM image of the molecular sieve-supported nano iron oxide composite adsorbent prepared in example 2.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the concept of the invention. All falling within the scope of the present invention.
Example 1
(1) Weighing 1g of ferric nitrate, putting the ferric nitrate into a beaker filled with 100mL of distilled water, and performing ultrasonic treatment to completely dissolve the ferric nitrate to obtain a corresponding ferric salt solution;
(2) Then adding 5g of SBA-15 molecular sieve into the ferric salt solution (the mass ratio of the molecular sieve to the ferric salt is 5:1), and carrying out ultrasonic treatment and stirring treatment for 4 hours to uniformly mix the molecular sieve and the ferric salt solution;
(3) Placing the mixed solution in a forced air drying oven, setting the temperature of the drying oven at 60 ℃, and drying for 12 hours to obtain solid powder;
(4) Fully grinding the solid powder, uniformly paving the powder in a corundum crucible, placing the corundum crucible in a high-temperature furnace, heating to 200 ℃ at a heating rate of 5 ℃/min, maintaining the temperature for 2 hours, and naturally cooling to room temperature;
(5) And fully grinding the reacted product, washing the product with water and ethanol for several times in sequence, placing the washed sample in a vacuum drying oven, and drying the sample for 12 hours at the temperature of 60 ℃ to obtain the molecular sieve loaded nano iron oxide composite adsorbent.
And (3) performing micro-morphology characterization on the SBA-15 molecular sieve loaded nano iron oxide composite adsorbent prepared in the example 1. Fig. 1 is a TEM image of the prepared composite adsorbent, and it can be seen that the nano iron oxide is uniformly distributed in the inside of the pores of the SBA-15 molecular sieve.
Example 2
(1) Weighing 1g of ferric nitrate, putting the ferric nitrate into a beaker filled with 100mL of distilled water, and performing ultrasonic treatment to completely dissolve the ferric nitrate to obtain a corresponding ferric salt solution;
(2) Then adding 10g of SBA-15 molecular sieve into the iron salt solution (the mass ratio of the molecular sieve to the iron salt is 10: 1), performing ultrasonic treatment and stirring for 4 hours, and uniformly mixing;
(3) Placing the mixed solution in a forced air drying oven, setting the temperature of the drying oven at 60 ℃, and drying for 12 hours to obtain solid powder;
(4) Fully grinding the solid powder, uniformly paving the powder in a corundum crucible, placing the corundum crucible in a high-temperature furnace, heating to 300 ℃ at a heating rate of 5 ℃/min, maintaining the temperature for 2 hours, and naturally cooling to room temperature;
(5) And fully grinding the reacted product, washing the product with water and ethanol for several times in sequence, placing the washed sample in a vacuum drying oven, and drying the sample for 12 hours at the temperature of 60 ℃ to obtain the molecular sieve loaded nano iron oxide composite adsorbent.
And (3) performing micro-morphology characterization on the SBA-15 molecular sieve loaded nano iron oxide composite adsorbent prepared in the example 2. Fig. 2 is a TEM image of the prepared composite adsorbent, and it can be seen that the nano iron oxide is uniformly distributed in the interior of the pore channels of the SBA-15 molecular sieve.
Example 3
(1) Weighing 1g of ferric nitrate, putting the ferric nitrate into a beaker filled with 100mL of distilled water, and performing ultrasonic treatment to completely dissolve the ferric nitrate to obtain a corresponding ferric salt solution;
(2) Then adding 10g of MCM-41 molecular sieve into the ferric salt solution (the mass ratio of the molecular sieve to the ferric salt is 10: 1), performing ultrasonic treatment and stirring for 4 hours, and uniformly mixing;
(3) Placing the mixed solution in a forced air drying oven, setting the temperature of the drying oven at 60 ℃, and drying for 12 hours to obtain solid powder;
(4) Fully grinding the solid powder, uniformly paving the powder in a corundum crucible, placing the corundum crucible in a high-temperature furnace, heating to 200 ℃ at a heating rate of 5 ℃/min, maintaining the temperature for 2 hours, and naturally cooling to room temperature;
(5) And fully grinding the reacted product, washing the product with water and ethanol for several times in sequence, placing the washed sample in a vacuum drying oven, and drying the sample for 12 hours at the temperature of 60 ℃ to obtain the molecular sieve loaded nano iron oxide composite adsorbent.
Example 4
(1) Weighing 1g of ferric sulfate, putting the ferric sulfate into a beaker filled with 100mL of distilled water, and performing ultrasonic treatment to completely dissolve the ferric sulfate to obtain a corresponding ferric salt solution;
(2) Then adding 10g of SBA-15 molecular sieve into the iron salt solution (the mass ratio of the molecular sieve to the iron salt is 10: 1), performing ultrasonic treatment and stirring for 4 hours, and uniformly mixing;
(3) Placing the mixed solution in a forced air drying oven, setting the temperature of the drying oven at 60 ℃, and drying for 12 hours to obtain solid powder;
(4) Fully grinding the solid powder, uniformly paving the solid powder in a corundum crucible, placing the corundum crucible in a high-temperature furnace, heating to 200 ℃ at a heating rate of 5 ℃/min, maintaining the temperature for 2 hours, and naturally cooling to room temperature;
(5) And (3) fully grinding the reacted product, washing the product for a plurality of times by using water and ethanol in sequence, placing the washed sample in a vacuum drying oven, and drying the sample for 12 hours at the temperature of 60 ℃ to obtain the molecular sieve loaded nano iron oxide composite adsorbent.
Example 5
(1) Weighing 1g of ferric chloride, placing the ferric chloride in a beaker filled with 100mL of distilled water, and performing ultrasonic treatment to completely dissolve the ferric chloride to obtain a corresponding ferric salt solution;
(2) Then adding 0.05g of SBA-15 molecular sieve into the ferric salt solution (the mass ratio of the molecular sieve to the ferric salt is 1;
(3) Placing the mixed solution in a forced air drying oven, setting the temperature of the drying oven at 30 ℃, and drying for 12 hours to obtain solid powder;
(4) Fully grinding the solid powder, uniformly paving the powder in a corundum crucible, placing the corundum crucible in a high-temperature furnace, heating to 400 ℃ at the heating rate of 5 ℃/min, maintaining the temperature for 6 hours, and naturally cooling to room temperature;
(5) And fully grinding the reacted product, washing the product with water and ethanol for several times in sequence, placing the washed sample in a vacuum drying oven, and drying the sample for 12 hours at 30 ℃ to obtain the molecular sieve loaded nano iron oxide composite adsorbent.
Example 6
(1) Weighing 1g of ferric nitrate, putting the ferric nitrate into a beaker filled with 100mL of distilled water, and performing ultrasonic treatment to completely dissolve the ferric nitrate to obtain a corresponding ferric salt solution;
(2) Then adding 20g of SBA-15 molecular sieve into the iron salt solution (the mass ratio of the molecular sieve to the iron salt is 20: 1), performing ultrasonic treatment and stirring for 4 hours, and uniformly mixing;
(3) Placing the mixed solution in a forced air drying oven, setting the temperature of the drying oven at 80 ℃, and drying for 12 hours to obtain solid powder;
(4) Fully grinding the solid powder, uniformly paving the powder in a corundum crucible, placing the corundum crucible in a high-temperature furnace, heating to 600 ℃ at the heating rate of 5 ℃/min, maintaining the temperature for 0.5 hour, and naturally cooling to room temperature;
(5) And fully grinding the reacted product, washing the product with water and ethanol for several times in sequence, placing the washed sample in a vacuum drying oven, and drying the sample for 12 hours at 80 ℃ to obtain the molecular sieve loaded nano iron oxide composite adsorbent.
The molecular sieve loaded nano iron oxide composite adsorbent prepared by the embodiment is used for removing heavy metals such as antimony and the like in wastewater, and comprises the following specific steps:
firstly, preparing antimony-containing waste water and actual smelting electroplating waste water with initial concentration of 20mg/L, adjusting the pH value to 2-11 by hydrochloric acid and sodium hydroxide solution, then adding 50mg of molecular sieve loaded nano iron oxide composite adsorbent into a test tube containing 50ml of antimony solution, fully mixing the composite adsorbent with the waste water, oscillating the mixture on a shaking table for more than 30min, and determining the concentration of metal pollutants in the solution before and after adsorption. Subsequently, the recovery of the composite adsorbent can be performed by centrifugation.
The results are as follows:
the invention is not the best known technology.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The molecular sieve confinement-loaded nano iron oxide composite adsorbent is characterized by comprising a mesoporous molecular sieve and nano iron oxide particles, wherein the nano iron oxide particles are uniformly confined in the pore canal of the mesoporous molecular sieve.
2. A method for preparing the molecular sieve confinement-loaded nano iron oxide composite adsorbent as claimed in claim 1, which is characterized by comprising the following steps:
(1) Dissolving iron salt in water to obtain an iron salt solution;
(2) Adding a molecular sieve into the ferric salt solution, and carrying out ultrasonic stirring for 3-5 hours to fully mix the molecular sieve and the ferric salt solution;
(3) Placing the mixed solution in a forced air drying box, and drying;
(4) Fully grinding the solid powder, then calcining at high temperature, maintaining for a certain time, and then naturally cooling;
(5) And (3) cleaning the calcined sample for several times, and drying in vacuum to obtain the molecular sieve loaded nano iron oxide composite adsorbent.
3. The molecular sieve confinement-supported nano-iron oxide composite adsorbent of claim 2, wherein the iron salt comprises one or more of ferric nitrate, ferric sulfate, ferric chloride and ferric acetylacetonate.
4. The molecular sieve confinement-loaded nano-iron oxide composite adsorbent of claim 2, wherein the molecular sieve comprises SBA-15, or MCM-41.
5. The molecular sieve confinement-loaded nano iron oxide composite adsorbent according to claim 1, wherein the mass ratio of the molecular sieve to the iron salt is 1.
6. The molecular sieve confinement-loaded nano iron oxide composite adsorbent according to claim 1, wherein the drying temperature of the forced air drying oven is 30-80 ℃.
7. The molecular sieve confinement-loaded nano-iron oxide composite adsorbent according to claim 1, wherein the calcination temperature is 200-600 ℃, and the calcination time is 0.5-6 hours.
8. The application of the molecular sieve confinement-loaded nano-iron oxide composite adsorbent as claimed in claim 1, wherein the composite adsorbent is used for removing antimony pollutants in wastewater.
9. The application of the molecular sieve confinement-loaded nano-iron oxide composite adsorbent according to claim 8, wherein the composite adsorbent is added into wastewater in the following amount: the mass ratio of the composite adsorbent to the wastewater is 1:1000-1, 5000, and fully mixing to realize effective removal of metals.
10. The application of the molecular sieve confinement-loaded nano-iron oxide composite adsorbent according to claim 9, wherein the composite adsorbent and wastewater are vibrated on a shaking table for 30-60 min.
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