CN109647351B - Bagasse loaded iron hydroxide adsorbent and preparation method and application thereof - Google Patents
Bagasse loaded iron hydroxide adsorbent and preparation method and application thereof Download PDFInfo
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- CN109647351B CN109647351B CN201910013033.2A CN201910013033A CN109647351B CN 109647351 B CN109647351 B CN 109647351B CN 201910013033 A CN201910013033 A CN 201910013033A CN 109647351 B CN109647351 B CN 109647351B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—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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- 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
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
Abstract
The invention discloses a preparation method of bagasse loaded iron hydroxide adsorbent and application of the bagasse loaded iron hydroxide adsorbent in treating phosphate in wastewater. The bagasse and the ferric salt solution are used as main raw materials, the effective load of the active component of the ferric hydroxide on the bagasse and the construction of the porous structure of the bagasse can be synchronously realized, the obtained adsorbent has large adsorption capacity and strong adaptability, the defects of weak adsorption capacity, difficult recovery and the like when the bagasse and the ferric hydroxide are used independently can be effectively avoided, and the method has important research and application values; the related preparation method is simple, convenient to operate and environment-friendly, can realize the resource utilization of bagasse, and has important economic and environmental benefits.
Description
Technical Field
The invention belongs to the interdisciplinary fields of chemistry, biology, materials, environmental science and the like, and particularly relates to a preparation method of a bagasse loaded iron hydroxide adsorbent and application of the bagasse loaded iron hydroxide adsorbent in treating phosphate in wastewater.
Background
Phosphorus is one of essential nutrient elements for growth of animals and plants, but excessive phosphorus easily causes water eutrophication. Phosphate-containing wastewater from industry and life is discharged into rivers, lakes and seas through various ways, and water bloom or red tide phenomena are very easily generated in a water area with poor mobility, so that a large amount of aquatic animals and plants die, and serious environmental pollution is caused. The existing methods for treating phosphate in water bodies comprise physical methods, chemical methods, ion exchange methods, membrane technology methods, biological adsorption methods and the like. The biological adsorption method has the advantages of simple preparation, low cost, easy popularization, good adsorption effect, no toxicity, no secondary pollution, easy biodegradation and the like, and becomes a research hotspot in the field.
Bagasse is a main byproduct in the sugar industry, and only 700 ten thousand tons of bagasse are produced in south China annually. At present, bagasse in China is mainly used for papermaking, incineration and even direct discarding, which not only causes a great deal of resource waste, but also causes environmental pollution. In addition, the iron hydroxide used alone adsorbs phosphate, which is likely to cause agglomeration during the preparation process, and the adsorption effect is poor and difficult to recover. Therefore, further exploring an adsorbent which is cheap and has a good phosphate adsorption effect and a preparation method thereof have important research and application significance.
Disclosure of Invention
The invention aims to provide a bagasse-loaded iron hydroxide adsorbent and application thereof in treating phosphate in wastewater, wherein bagasse and iron hydroxide are effectively compounded, so that the obtained adsorbing material can effectively adsorb phosphate with higher concentration in the wastewater, the environmental pollution caused by the bagasse can be solved, and the resource utilization of the bagasse is realized; the related preparation method is simple, the raw materials are cheap and easy to obtain, and the method has important economic benefit and environmental benefit and wide application prospect.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of bagasse loaded iron hydroxide adsorbent comprises the following steps:
1) Bagasse pretreatment; washing the collected and squeezed bagasse with water, decocting in water, filtering, repeating the decocting and filtering step for 3-4 times to remove soluble saccharides and other impurities, washing with water to further remove saccharides and other impurities, draining, oven drying, pulverizing, and collecting 100-200 mesh bagasse powder;
2) Adding bagasse powder into a ferric salt solution, and uniformly stirring and mixing to obtain a mixed solution I;
3) Adding alkali liquor into the mixed liquor I, adjusting the pH value of the obtained mixed liquor to 4.5-5.0, and carrying out ultrasonic stirring reaction;
4) And (3) carrying out centrifugal separation on the reaction liquid obtained in the step 3), collecting the obtained precipitate, washing with water, drying and grinding to obtain the bagasse loaded iron hydroxide adsorbent.
In the scheme, the bagasse powder contains 95-99% of dry substances, and the bagasse powder comprises the following components in percentage by mass: 43-51% of cellulose, 24-32% of hemicellulose, 20-27% of lignin, 1.5-2.3% of crude protein, 0.2-0.8% of crude fat and 0.9-1.5% of crude ash.
In the scheme, the pH value of the iron salt solution is 1.4-2.2.
In the above scheme, the iron salt is ferric nitrate or ferric chloride.
In the scheme, the mass ratio of the iron source to the bagasse powder is (1.5-10): 1.
In the scheme, the alkali liquor is Na with the concentration of 3-5wt% 2 CO 3 Or NaHCO 3 And (3) solution.
In the scheme, the drying step in the step 1) is drying for 24-48h at 40-50 ℃ in an electric heating forced air drying oven.
In the above scheme, the bagasse powder has a particle size of 100-200 mesh.
In the scheme, the concentration of the iron salt solution is 7-49.55mmol/L.
In the scheme, the ultrasonic stirring reaction time is 20-30min, and the ultrasonic power is 80-250w.
In the scheme, the adding flow rate of the alkali liquor is 5-8mL/min.
The bagasse-loaded iron hydroxide adsorbent prepared according to the scheme is applied to treatment of phosphate in wastewater, can realize efficient adsorption of phosphate, is easy to recover, and is suitable for popularization and application.
The mechanism of the invention is as follows: ferric ions are uniformly dispersed on the surface of bagasse by adopting a loading method, because of Fe (NO) 3 ) 3 、FeCl 3 When the solution formed in the preparation process has strong acidity (the pH value is 1.4-2.2) and is not beneficial to loading, the invention adopts a constant flow pump to slowly drop dilute Na 2 CO 3 The acidity of ferric nitrate and ferric chloride in aqueous solution and Na are utilized 2 CO 3 Reaction to produceAnd (2) carbon oxide gas, monitoring the pH value of the mixed solution by a pH meter, performing ultrasonic stirring treatment, centrifuging, and performing freeze drying to obtain bagasse-loaded iron hydroxide adsorbent powder, so as to synchronously realize effective loading of an iron hydroxide active component on the bagasse and construction of a bagasse porous structure.
Compared with the prior art, the invention has the beneficial effects that:
1) The invention takes bagasse and ferric salt solution as main raw materials, and Na is introduced into the bagasse and the ferric salt solution 2 CO 3 Or NaHCO 3 The solution and the pH value of the obtained reaction solution are controlled, the effective load of the active component of the iron hydroxide on the bagasse and the construction of the porous structure of the bagasse can be synchronously realized, the obtained adsorbent has large adsorption capacity and strong adaptability, the defects of weak adsorption capacity, difficult recovery and the like when the bagasse and the iron hydroxide are used independently can be effectively avoided, and the important research and application values are realized.
2) The preparation method provided by the invention is simple, convenient to operate, environment-friendly and suitable for popularization and application.
3) The raw materials related by the invention have wide sources, low cost, low price and easy obtainment, can realize the resource utilization of bagasse, and have important economic benefit and environmental benefit.
Drawings
FIG. 1 is an SEM image of iron hydroxide adsorbent loaded on bagasse obtained in example 1 of the present invention.
FIG. 2 is an SEM picture of the bagasse obtained in example 1 of the present invention after adsorption of phosphate by iron hydroxide adsorbent.
FIG. 3 is an EDS picture of bagasse-loaded iron hydroxide adsorbent obtained in example 1 of the present invention.
FIG. 4 is an EDS picture of bagasse loaded iron hydroxide adsorbent obtained in example 1 of the present invention after adsorption of phosphate.
Detailed Description
For better understanding of the present invention, the following examples are given for further illustration of the present invention, but the present invention is not limited to the following examples.
In the following examples, the pretreatment steps in the bagasse employed included the following steps: washing the collected and squeezed bagasse with water, decocting in water, filtering, repeating the decocting and filtering step for 3-4 times to remove soluble saccharides and other impurities, washing with water to further remove saccharides and other impurities, filtering, drying, pulverizing, and collecting 100-200 mesh bagasse powder; the dry matter content of the obtained bagasse powder is 98.7wt%, and the components and the mass percentage thereof comprise: 46.1% of cellulose, 25.4% of hemicellulose, 23.5% of lignin, 1.2% of crude protein, 0.7% of crude fat and 1.3% of crude ash.
Example 1
A bagasse loaded iron hydroxide adsorbent is prepared by the following steps:
1) 1.0g of bagasse powder was added to 500ml of 37.1mmol/L Fe (NO) 3 ) 3 Putting the solution (with initial pH value of 1.51) into an ultrasonic machine, and stirring the mixed solution with a mechanical stirrer for 30min to obtain a mixed solution I;
2) Adding Na with the concentration of 5wt% into the obtained mixed solution I by a constant flow pump under the monitoring of a pH meter 2 CO 3 Controlling the flow rate of the solution at 6.25mL/min, and stopping Na when the pH of the obtained mixed solution is 5 2 CO 3 Adding the solution, and continuing to perform ultrasonic treatment and stirring for 30min under the condition that the power is 150 w;
3) Centrifuging at 4000r/min for 20min, collecting precipitate, washing the precipitate with small amount of distilled water for several times, freeze drying, and grinding to obtain bagasse loaded iron hydroxide adsorbent.
The product obtained in the embodiment is applied to removing phosphate in wastewater, and the specific steps comprise: measuring phosphate in the water solution by adopting an ammonium molybdate spectrophotometry, adding 0.04g of bagasse loaded iron hydroxide adsorbent into 50ml of simulated wastewater (sodium phosphate solution) with the concentration of 25mg/L, shaking for 2h by a shaking table at 250r/min, standing for 0.5h, and taking supernatant to detect the concentration of the phosphate; the results show that the removal rate of phosphate reaches 99.1%.
Fig. 1 and fig. 2 are SEM images of the bagasse-loaded iron hydroxide adsorbent obtained in this example before and after adsorption of phosphate, respectively, and the results show that: the existence of a large number of fine particles on the surface of fig. 1 shows that iron hydroxide is well loaded on the surface of bagasse, and the existence of fine particles still exists in fig. 2, and although the fact that whether phosphate is adsorbed on the surface cannot be visually seen, the fine particles can be proved by the aid of EDS characterization.
Fig. 3 and 4 are EDS graphs of the bagasse-loaded iron hydroxide adsorbent obtained in this example before and after adsorption of phosphate, respectively, and the results show that: the phosphorus content before adsorption is only 0.20wt%, and after adsorption, the phosphorus content reaches 2.83wt%, which indicates that the phosphate can be well adsorbed on the bagasse loaded iron hydroxide adsorbent.
Example 2
The preparation method of the bagasse loaded iron hydroxide adsorbent comprises the following steps:
1) 1.0g of bagasse powder was added to 500ml of 49.5mmol/L Fe (NO) 3 ) 3 Putting the solution (with initial pH value of 1.42) into an ultrasonic machine, and stirring the mixed solution with a mechanical stirrer for 30min to obtain a mixed solution I;
2) Adding Na with the concentration of 4wt% into the obtained mixed solution I by a constant flow pump under the monitoring of a pH meter 2 CO 3 Controlling the flow rate of the solution at 5mL/min, and stopping Na when the pH of the obtained mixed solution is 4.5 2 CO 3 Adding the solution, and continuing to perform ultrasonic treatment and stirring for 30min under the condition that the power is 120 w;
3) Centrifuging at 4000r/min for 20min, collecting precipitate, washing the precipitate with small amount of distilled water for several times, freeze drying, and grinding to obtain bagasse loaded iron hydroxide adsorbent.
The product obtained in the embodiment is applied to removing phosphate in wastewater, and the specific steps comprise: measuring phosphate in the water solution by adopting an ammonium molybdate spectrophotometry, adding 0.04g of bagasse loaded iron hydroxide adsorbent into 50ml of simulated wastewater (sodium phosphate solution) with the concentration of 25mg/L, shaking for 2h by a shaking table at 250r/min, standing for 0.5h, and taking supernatant to detect the concentration of the phosphate; the results show that the phosphate removal rate reaches 99.8%.
Example 3
A bagasse loaded iron hydroxide adsorbent is prepared by the following steps:
1) 1.0g of bagasse powder was added to 500ml of 49.5mmol/L Fe (NO) 3 ) 3 Adding the solution (initial pH value is 1.42) into an ultrasonic machine, and stirring the mixed solution for 30min by using a mechanical stirrer to obtain a mixed solution I;
2) Adding NaHCO with the concentration of 4wt% into the obtained mixed solution I by a constant flow pump under the monitoring of a pH meter 3 Controlling the flow rate of the solution at 6.25mL/min, and stopping Na when the pH of the obtained mixed solution is 4.5 2 CO 3 Adding the solution, and continuing to perform ultrasonic treatment and stirring for 30min under the condition that the power is 150 w;
3) Centrifuging at 4000r/min for 20min, collecting precipitate, washing the precipitate with small amount of distilled water for several times, freeze drying, and grinding to obtain bagasse loaded iron hydroxide adsorbent.
The product obtained in the embodiment is applied to removing phosphate in wastewater, and the specific steps comprise: measuring phosphate in the aqueous solution by adopting an ammonium molybdate spectrophotometry, adding 0.04g of bagasse loaded iron hydroxide adsorbent into 50ml of simulated wastewater (sodium phosphate solution) with the pH of 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 and 12 respectively and the concentration of 25mg/L, shaking by a shaking table at 250r/min for 2h, standing for 0.5h, and taking supernatant to detect the concentration of phosphate; the results indicated that the phosphate removal rates were 99.7%, 99.8%, 99.6%, 99.3%, 99.6%, 99.3%, 98.7%, 93.4%, 50.2%, and 33.4%, respectively.
The results show that the bagasse-loaded iron hydroxide adsorbent prepared by the method has large adsorption capacity and wide adaptability to the pH condition of wastewater solution.
Comparative example 1
The preparation method of the bagasse loaded iron hydroxide adsorbent comprises the following steps:
1) 1.0g of bagasse powder was added to 500ml of Fe (NO) with a concentration of 37.1mmol/L 3 ) 3 Putting the solution (with initial pH value of 1.51) into an ultrasonic machine, and stirring the mixed solution with a mechanical stirrer for 30min to obtain a mixed solution I;
2) Adding NaHCO with the concentration of 6.25wt% into the obtained mixed solution I by a constant flow pump under the monitoring of a pH meter 3 Controlling the flow rate of the solution at 5mL/min, and stopping Na when the pH of the obtained mixed solution is 2 2 CO 3 Adding the solution, and continuing to perform ultrasonic treatment and stirring for 30min under the condition that the power is 180 w;
3) Centrifuging at 4000r/min for 20min, collecting precipitate, washing the precipitate with small amount of distilled water for several times, freeze drying, and grinding to obtain bagasse loaded iron hydroxide adsorbent.
The product obtained in the embodiment is applied to removing phosphate in wastewater, and the specific steps comprise: measuring phosphate in the water solution by adopting an ammonium molybdate spectrophotometry, adding 0.04g bagasse-loaded iron hydroxide adsorbent into 50ml of simulated wastewater (sodium phosphate solution) with the concentration of 25mg/L, shaking for 2h at a shaking table of 250r/min, standing for 0.5h, and taking supernatant to detect the concentration of the phosphate; the results show that the adsorbent has little effect on adsorbing phosphate.
Comparative example 2
The preparation method of the bagasse loaded iron hydroxide adsorbent comprises the following steps:
1) 1.0g of bagasse powder was added to 500ml of 49.5mmol/L Fe (NO) 3 ) 3 Putting the solution (with initial pH value of 1.42) into an ultrasonic machine, and stirring the mixed solution with a mechanical stirrer for 30min to obtain a mixed solution I;
2) Adding Na with the concentration of 4wt% into the obtained mixed solution I by a constant flow pump under the monitoring of a pH meter 2 CO 3 Controlling the flow rate of the solution at 5mL/min, and stopping Na when the pH of the obtained mixed solution is 7 2 CO 3 Adding the solution, and continuing to perform ultrasonic treatment and stirring for 30min under the condition that the power is 200 w;
3) Centrifuging at 4000r/min for 20min, collecting precipitate, washing the precipitate with small amount of distilled water for several times, freeze drying, and grinding to obtain bagasse-loaded iron hydroxide adsorbent.
The product obtained in the embodiment is applied to removing phosphate in wastewater, and the specific steps comprise: measuring phosphate in the water solution by adopting an ammonium molybdate spectrophotometry, adding 0.04g of bagasse loaded iron hydroxide adsorbent into 50ml of simulated wastewater (sodium phosphate solution) with the concentration of 25mg/L, shaking for 2h by a shaking table at 250r/min, standing for 0.5h, and taking supernatant to detect the concentration of the phosphate; the results showed that the phosphate removal rate reached 9.6%.
The invention can be realized by all the listed raw materials, and the invention can be realized by the upper and lower limit values and interval values of all the raw materials; the examples are not to be construed as limiting the scope of the invention. The upper and lower limit values and interval values of the process parameters can realize the invention, and the embodiments are not listed.
Claims (5)
1. A preparation method of bagasse loaded iron hydroxide adsorbent is characterized by comprising the following steps:
1) Pretreating bagasse; washing the collected and juiced bagasse with water, boiling in water, filtering, washing with water, drying, and crushing to obtain bagasse powder;
2) Adding bagasse powder into a ferric salt solution, and uniformly stirring and mixing to obtain a mixed solution I;
3) Adding alkali liquor into the mixed liquor I, adjusting the pH value of the obtained mixed liquor to 4.5-5.0, and carrying out ultrasonic stirring reaction;
4) Carrying out centrifugal separation on the reaction liquid obtained in the step 3), collecting the obtained precipitate, washing with water, and drying to obtain a bagasse loaded iron hydroxide adsorbent;
the pH value of the ferric salt solution is 1.4-2.2;
the alkali liquor is 3-5wt% of Na 2 CO 3 Or NaHCO 3 A solution;
the concentration of the ferric salt solution is 7-49.55mmol/L;
the ultrasonic stirring reaction time is 20-30min;
the adding flow rate of the alkali liquor is 5-8mL/min.
2. The preparation method of claim 1, wherein the bagasse powder contains 95-99% of dry matter, and the components and mass percentages thereof comprise: 43-51% of cellulose, 24-32% of hemicellulose, 20-27% of lignin, 1.5-2.3% of crude protein, 0.2-0.8% of crude fat and 0.9-1.5% of crude ash.
3. The preparation method according to claim 1, wherein the mass ratio of the iron salt to the bagasse powder is (1.5-10): 1.
4. Bagasse-loaded iron hydroxide adsorbent, obtainable by the process according to any one of claims 1 to 3.
5. The application of the bagasse-loaded iron hydroxide adsorbent in treating phosphate in wastewater as claimed in claim 4.
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| CN110314655B (en) * | 2019-06-03 | 2022-05-10 | 武汉工程大学 | Bagasse-loaded zero-valent iron adsorbent and preparation method and application thereof |
| CN111229171B (en) * | 2020-01-19 | 2022-05-10 | 武汉工程大学 | Straw-loaded MOF material adsorbent and preparation method and application thereof |
| CN113926422A (en) * | 2020-07-13 | 2022-01-14 | 广西大学 | Preparation and application of magnetic bagasse carbon-loaded ferrihydrite composite adsorbent |
| CN113648976B (en) * | 2021-09-08 | 2023-11-28 | 云南铂鑫环保技术有限公司 | Preparation method of biochar capable of efficiently adsorbing carbon dioxide |
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