CN115155514A - Diatomite-based magnetic adsorption phosphorus removal agent and preparation method thereof - Google Patents
Diatomite-based magnetic adsorption phosphorus removal agent and preparation method thereof Download PDFInfo
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- CN115155514A CN115155514A CN202210663131.2A CN202210663131A CN115155514A CN 115155514 A CN115155514 A CN 115155514A CN 202210663131 A CN202210663131 A CN 202210663131A CN 115155514 A CN115155514 A CN 115155514A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/14—Diatomaceous earth
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- 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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- 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
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus 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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal 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
- C02F2101/00—Nature of the contaminant
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Abstract
The invention discloses a diatomite-based magnetic adsorption phosphorus removal agent and a preparation method thereof, and relates to the technical field of phosphorus removal agents. The magnetic diatomite-based cerium-loaded adsorption phosphorus removal agent and the preparation method thereof use low-grade diatomite as a raw material to prepare a green and environment-friendly water treatment agent, embody the principles of recycling wastes and treating wastes with wastes, have low cost, belong to ecological and environment-friendly medicaments, have no secondary pollution, have good removal effect on total phosphorus by the prepared magnetic diatomite-based cerium-loaded adsorption phosphorus removal agent, and have ideal removal effect on total metals, suspended matters, organic matters and the like.
Description
Technical Field
The invention relates to the technical field of phosphorus removing agents, in particular to a diatomite-based magnetic adsorption phosphorus removing agent and a preparation method thereof.
Background
In recent years, with increasingly strict national environmental requirements, higher standards are provided for the quality of effluent water of urban sewage treatment plants, and the currently adopted advanced enhanced phosphorus removal treatment technologies mainly include a membrane separation technology, an ecological purification technology, a physical chemistry technology and the like. The effluent quality of the membrane separation technology is good, but the investment cost and the operation cost are high, and the requirement on operation and maintenance is high; the ecological purification technology occupies a large area; flocculating agents such as polyaluminium or polyferric and the like are added in the flocculation precipitation technology, so that certain ecological risk exists on the effluent quality; the physical and chemical technology represented by the flocculation precipitation or adsorption method is simple in system, convenient to operate and manage, and reasonable in investment cost and operating cost.
Although the urban sewage is treated by the deep treatment technology of the urban sewage treatment plant by adopting the coagulating sedimentation filtration, the reagents used by the flocculating sedimentation comprise an aluminum system and an iron system, and the iron system flocculating agent in the common flocculating agent has simple operation and low cost, but ferrous salt can be generated in the using process, and the ferric salt can cause the excessive Fe & lt 3+ & gt in the effluent to cause the effluent chromaticity to exceed the standard, so that the water body has the phenomena of yellowing and blackening and the pipeline is corroded; the aluminum flocculant has very small alum floc, sometimes the effluent turbidity is higher than that of raw water, and A13+ in aluminum salt can generate adverse effect on the ecological environment after being discharged to water. Researches prove that aluminum iron and ferric salt flocculating agents have toxic effects on microorganisms in a biochemical system, and in addition, the pH range of application of aluminum salt and ferric salt is narrow, but the conventional activated carbon adsorption method has the defects of high cost and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a diatomite-based magnetic adsorption phosphorus removal agent and a preparation method thereof, which solve the problems that ferrous salt is generated in the use process of a flocculating agent, and the excessive Fe & lt 3+ & gt in the effluent causes the effluent chromaticity to exceed the standard, so that the water body has yellowing and blackening phenomena and the pipeline is corroded; the aluminum flocculating agent has small alum floc, sometimes the effluent turbidity is higher than that of raw water, and the A13+ in the aluminum salt generates unfavorable problems to the ecological environment after being discharged to the water body.
In order to achieve the purpose, the invention is realized by the following technical scheme: the components of the phosphorus removing agent comprise natural diatomite, deionized water, hydrochloric acid, a cerium sulfate solution, an iron chloride solution and a NaOH solution.
Further, a preparation method of the diatomite-based magnetic adsorption phosphorus removal agent comprises a formula of the magnetic diatomite-based cerium-loaded adsorption phosphorus removal agent, and the preparation method comprises the following steps:
s1, pretreating diatomite: putting natural diatomite into a pulverizer to be pulverized, pulverizing the pulverized natural diatomite to 95-105 meshes, stirring and mixing the pulverized natural diatomite and deionized water according to the ratio of 1;
s2, purifying and preparing diatomite by an acid boiling method: placing the mixed slurry after the pretreatment in the step S1 in a beaker, adding 10% hydrochloric acid into the mixed slurry, wherein the ratio of the hydrochloric acid to the mixed slurry is 5;
s3, magnetic modification and cerium modification by a coprecipitation method: putting the diatomite prepared in the step S2 into a beaker, adding a cerium sulfate solution and a ferric chloride solution into the beaker, magnetically stirring the added solution, slowly adding 1.0mol/L NaOH solution while stirring, testing the pH value of the solution while adding the NaOH solution until the pH value reaches 10, stopping adding the NaOH solution, stirring and soaking the solution for 30-45 min, then putting the solution into a medium-speed filter tank for filtering, then washing the filtered product with deionized water until the washed filtrate is neutral, and after washing, putting the filtrate into a drying oven to dry at 100 ℃;
s4, activating and forming: and (4) putting the dried product in the step (S3) into a muffle furnace, roasting at the temperature of 700-900 ℃, taking out the product after roasting is finished, cooling to room temperature, grinding the product, and sieving through a 230-mesh sieve to obtain the product, namely the magnetic diatomite-based cerium-loaded adsorption phosphorus removal agent.
Further, in the step S1, when the natural diatomite and the deionized water are stirred, the stirring speed is 80r/min, and the stirring time is 45-60 min.
Further, in the step S2, the water bath heating time of the filtrate is 2-5 h.
Further, in the step S3, the ratio of the cerium sulfate solution to the ferric chloride solution is 50.
Further, in the step S3, the drying temperature of the drying oven is 105 ℃.
Further, in the step S4, the roasting time is 2 hours, and the heat preservation time is 30min.
Advantageous effects
The invention provides a diatomite-based magnetic adsorption phosphorus removal agent and a preparation method thereof, and compared with the prior art, the diatomite-based magnetic adsorption phosphorus removal agent has the following beneficial effects:
1. the diatomite-based magnetic adsorption phosphorus removal agent and the preparation method thereof use low-grade diatomite as a raw material to prepare a green and environment-friendly water treatment agent, reflect the principles of waste resource recycling and waste treatment by waste, have low cost, belong to an ecological environment-friendly medicament, and have no secondary pollution.
2. The diatomite-based magnetic adsorption phosphorus removal agent and the preparation method thereof have good removal effect on total phosphorus by the prepared magnetic diatomite-based cerium-loaded adsorption phosphorus removal agent, and simultaneously have ideal removal effect on heavy metals, suspended matters, organic matters and the like.
3. The diatomite-based magnetic adsorption phosphorus removal agent and the preparation method thereof have a strong superparamagnetic effect, and can be efficiently recovered and repeatedly utilized by adopting a magnetic recovery device.
Drawings
FIG. 1 is a schematic view of the preparation process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Referring to fig. 1, the present invention provides three technical solutions:
example one
A diatomite-based magnetic adsorption phosphorus removal agent comprises natural diatomite, deionized water, hydrochloric acid, a cerium sulfate solution, an iron chloride solution and a NaOH solution.
In the embodiment of the invention, a preparation method of a diatomite-based magnetic adsorption phosphorus removal agent comprises a formula of the diatomite-based magnetic adsorption phosphorus removal agent, and the preparation method comprises the following steps:
s1, pretreating diatomite: the method comprises the following steps of (1) putting natural diatomite into a grinder for grinding, grinding to 95 meshes, stirring and mixing the ground natural diatomite and deionized water according to a ratio of 1;
s2, purifying and preparing diatomite by an acid boiling method: placing the mixed slurry after the pretreatment in the step S1 in a beaker, adding 10% hydrochloric acid into the mixed slurry, wherein the ratio of the hydrochloric acid to the mixed slurry is 5;
s3, magnetic modification and cerium modification by a coprecipitation method: putting the diatomite prepared in the step S2 into a beaker, adding a cerium sulfate solution and a ferric chloride solution into the beaker, magnetically stirring the added solution, slowly adding a 1.0mol/L NaOH solution while stirring, testing the pH value of the solution while adding, stopping adding the NaOH solution until the pH value reaches 10, stirring and soaking the solution for 30min, then putting the solution into a medium-speed filter for filtering, then washing the filtered product with deionized water until the washed filtrate is neutral, and after washing, putting the filtrate into a drying oven to dry at 100 ℃;
s4, activating and forming: and (4) putting the dried product in the step (S3) into a muffle furnace, roasting at 700 ℃, taking out the product after roasting, cooling to room temperature, grinding the product, and sieving with a 230-mesh sieve to obtain the product, namely the magnetic diatomite-based cerium-loaded adsorption phosphorus removal agent.
In the embodiment of the invention, in the step S1, when the natural diatomite and the deionized water are stirred, the stirring speed is 80r/min, and the stirring time is 45min.
In the embodiment of the invention, in the step S2, the water bath heating time of the filtrate is 2 hours.
In the embodiment of the present invention, in step S3, the ratio of the cerium sulfate solution to the ferric chloride solution is 50.
In the embodiment of the invention, in the step S3, the drying temperature of the drying oven is 105 ℃.
In the embodiment of the invention, in the step S4, the roasting time is 2 hours, and the heat preservation time is 30min.
Example two
A diatomite-based magnetic adsorption phosphorus removal agent comprises natural diatomite, deionized water, hydrochloric acid, a cerium sulfate solution, an iron chloride solution and a NaOH solution.
In the embodiment of the invention, the preparation method of the diatomite-based magnetic adsorption phosphorus removal agent comprises a formula of the diatomite-based magnetic adsorption phosphorus removal agent, and the preparation method comprises the following steps:
s1, pretreating diatomite: putting natural diatomite into a pulverizer to be pulverized into 105 meshes, then stirring and mixing the pulverized natural diatomite and deionized water according to the proportion of 1;
s2, purifying and preparing diatomite by an acid boiling method: placing the mixed slurry after the pretreatment in the step S1 in a beaker, adding 10% hydrochloric acid into the mixed slurry, wherein the ratio of the hydrochloric acid to the mixed slurry is 5;
s3, magnetic modification and cerium modification are carried out by a coprecipitation method: putting the diatomite prepared in the step S2 into a beaker, adding a cerium sulfate solution and a ferric chloride solution into the beaker, magnetically stirring the added solution, slowly adding 1.0mol/L NaOH solution while stirring, testing the pH value of the solution while adding the NaOH solution until the pH value reaches 10, stopping adding the NaOH solution, stirring and soaking the solution for 45min, then putting the solution into a medium-speed filter for filtering, then washing the filtered product with deionized water until the washed filtrate is neutral, and after washing, putting the filtrate into a drying oven to be dried at 100 ℃;
s4, activating and forming: and (4) putting the dried product obtained in the step (S3) into a muffle furnace, roasting at the temperature of 900 ℃, taking out the roasted product after roasting, cooling to room temperature, grinding the product, and sieving the product with a 230-mesh sieve to obtain the magnetic diatomite-based cerium-loaded adsorption phosphorus removal agent.
In the embodiment of the invention, in the step S1, when the natural diatomite and the deionized water are stirred, the stirring speed is 80r/min, and the stirring time is 60min.
In the embodiment of the invention, in the step S2, the water bath heating time of the filtrate is 5h.
In the embodiment of the invention, in step S3, the ratio of the cerium sulfate solution to the ferric chloride solution is 50.
In the embodiment of the invention, in the step S3, the drying temperature of the drying oven is 105 ℃.
In the embodiment of the invention, in the step S4, the roasting time is 2h, and the heat preservation time is 30min.
EXAMPLE III
A diatomite-based magnetic adsorption phosphorus removal agent comprises natural diatomite, deionized water, hydrochloric acid, a cerium sulfate solution, an iron chloride solution and a NaOH solution.
In the embodiment of the invention, the preparation method of the diatomite-based magnetic adsorption phosphorus removal agent comprises a formula of the magnetic diatomite-based cerium-loaded adsorption phosphorus removal agent, and the preparation method comprises the following steps:
s1, pretreating diatomite: putting natural diatomite into a pulverizer to be pulverized, pulverizing the pulverized natural diatomite into 100 meshes, stirring and mixing the pulverized natural diatomite and deionized water according to a ratio of 1;
s2, purifying and preparing diatomite by an acid boiling method: placing the mixed slurry after the pretreatment in the step S1 in a beaker, adding 10% hydrochloric acid into the mixed slurry, wherein the ratio of the hydrochloric acid to the mixed slurry is 5;
s3, magnetic modification and cerium modification by a coprecipitation method: putting the diatomite prepared in the step S2 into a beaker, adding a cerium sulfate solution and a ferric chloride solution into the beaker, magnetically stirring the added solution, slowly adding 1.0mol/L NaOH solution while stirring, testing the pH value of the solution while adding the NaOH solution until the pH value reaches 10, stopping adding the NaOH solution, stirring and soaking the solution for 37min, then putting the solution into a medium-speed filter for filtering, then washing the filtered product with deionized water until the washed filtrate is neutral, and after washing, putting the filtrate into a drying oven to be dried at 100 ℃;
s4, activating and forming: and (4) putting the dried product obtained in the step (S3) into a muffle furnace, roasting at the temperature of 800 ℃, taking out the roasted product after roasting, cooling to room temperature, grinding the product, and sieving the product with a 230-mesh sieve to obtain the magnetic diatomite-based cerium-loaded adsorption phosphorus removal agent.
In the embodiment of the invention, in the step S1, when the natural diatomite and the deionized water are stirred, the stirring speed is 80r/min, and the stirring time is 53min.
In the embodiment of the invention, in the step S2, the water bath heating time of the filtrate is 3h.
In the embodiment of the invention, in step S3, the ratio of the cerium sulfate solution to the ferric chloride solution is 50.
In the embodiment of the invention, in the step S3, the drying temperature of the drying oven is 105 ℃.
In the embodiment of the invention, in the step S4, the roasting time is 2 hours, and the heat preservation time is 30min.
And those not described in detail in this specification are well within the skill of those in the art.
It should be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Claims (7)
1. A diatomite-based magnetic adsorption phosphorus removal agent is characterized in that: the phosphorous removing agent comprises the components of natural diatomite, deionized water, hydrochloric acid, a cerium sulfate solution, an iron chloride solution and a NaOH solution.
2. A preparation method of a diatomite-based magnetic adsorption phosphorus removal agent is characterized by comprising the following steps: the formulation comprising the diatomite-based magnetic adsorption phosphorus removal agent of claim 1, wherein the preparation method comprises the following steps:
s1, pretreating diatomite: putting natural diatomite into a pulverizer to be pulverized, pulverizing the pulverized natural diatomite to 95-105 meshes, stirring and mixing the pulverized natural diatomite and deionized water according to the ratio of 1;
s2, purifying and preparing diatomite by an acid boiling method: placing the mixed slurry after the pretreatment in the step S1 in a beaker, adding 10% hydrochloric acid into the mixed slurry, wherein the ratio of the hydrochloric acid to the mixed slurry is 5;
s3, magnetic modification and cerium modification by a coprecipitation method: putting the diatomite prepared in the step S2 into a beaker, adding a cerium sulfate solution and a ferric chloride solution into the beaker, magnetically stirring the added solution, slowly adding 1.0mol/L NaOH solution while stirring, testing the pH value of the solution while adding the NaOH solution until the pH value reaches 10, stopping adding the NaOH solution, stirring and soaking the solution for 30-45 min, then putting the solution into a medium-speed filter tank for filtering, then washing the filtered product with deionized water until the washed filtrate is neutral, and after washing, putting the filtrate into a drying oven to dry at 100 ℃;
s4, activating and forming: and (4) putting the dried product obtained in the step (S3) into a muffle furnace, roasting at the temperature of 700-900 ℃, taking out the roasted product after roasting is finished, cooling to room temperature, grinding the product, and sieving the product with a 230-mesh sieve to finally obtain the product, namely the magnetic diatomite-based cerium-loaded adsorption phosphorus removal agent.
3. The preparation method of the diatomite-based magnetic adsorption phosphorus removal agent as claimed in claim 2, wherein the preparation method comprises the following steps: in the step S1, when the natural diatomite and the deionized water are stirred, the stirring speed is 80r/min, and the stirring time is 45-60 min.
4. The preparation method of the diatomite-based magnetic adsorption phosphorus removal agent as claimed in claim 2, wherein: in the step S2, the water bath heating time of the filtrate is 2-5 h.
5. The preparation method of the diatomite-based magnetic adsorption phosphorus removal agent as claimed in claim 2, wherein: in the step S3, the ratio of the cerium sulfate solution to the ferric chloride solution is 50.
6. The preparation method of the diatomite-based magnetic adsorption phosphorus removal agent as claimed in claim 2, wherein: in the step S3, the drying temperature of the drying oven is 105 ℃.
7. The preparation method of the diatomite-based magnetic adsorption phosphorus removal agent as claimed in claim 2, wherein the preparation method comprises the following steps: in the step S4, the roasting time is 2 hours, and the heat preservation time is 30min.
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