CN111701568A - Eggshell straw biochar composite microsphere phosphorus removal adsorbent with high adsorption performance and preparation method and application thereof - Google Patents
Eggshell straw biochar composite microsphere phosphorus removal adsorbent with high adsorption performance 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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—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 form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4881—Residues from shells, e.g. eggshells, mollusk shells
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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 high-adsorption-performance eggshell straw biochar composite microsphere dephosphorization adsorbent and a preparation method and application thereof, wherein eggshell straw biochar composite microspheres are prepared by using eggshells and straws as raw materials through calcium alginate embedding ball forming and high-temperature carbonization methods, the diameter of the microsphere is 1.5-2.5mm, the microsphere has ultrahigh adsorption capacity on phosphate, the microsphere has good mass transfer performance and high adsorption speed; the straw can improve the crosslinking performance and mechanical strength of the microspheres, and the eggshell biochar is wrapped in the porous microspheres, so that the loss of effective components is prevented, the mass transfer performance of the microspheres is improved, and the settling performance of the adsorbent is improved; the preparation method has the advantages of easily available raw materials, simple and convenient process and mild conditions, and is suitable for large-scale industrial production and use.
Description
Technical Field
The invention belongs to the field of adsorbent preparation and wastewater treatment, and relates to an eggshell straw biochar composite microsphere phosphorus removal adsorbent with high adsorption performance, and a preparation method and application thereof.
Background
Phosphorus is a main factor causing eutrophication of water bodies, and when the content of phosphorus in water is more than 0.018 mg. P/L, plankton can be greatly increased. Therefore, the control of the content of phosphorus in the wastewater is very important for preventing and controlling the eutrophication of the water body. The adsorption method is a common method for removing phosphorus in water, and the selection of a cheap and efficient adsorbent becomes a key factor for treating phosphorus-containing wastewater by the adsorption method.
The eggshell, a domestic waste, has a porous, complex layered structure with a calcium carbonate content of 93%. The natural eggshell powder has limited adsorption capacity to phosphorus, but after high-temperature pyrolysis, calcium carbonate in the eggshell can be decomposed to generate calcium oxide, and the calcium oxide reacts with phosphate in the solution under alkaline conditions to generate calcium hydroxy phosphate, so that the phosphate adsorption capacity of the eggshell is improved to a certain extent. However, the powdered eggshell biochar is easy to agglomerate and cause the blockage of the fixed bed, and the factors limit the application of the biochar in practical engineering and the development of material industrialization.
The embedding technology is a common method for increasing the size and solid-liquid separation capacity of the adsorbent, and the gel beads with a net structure can be obtained by coating the powder adsorbent in a high polymer. The method is simple to operate, and the obtained gel spheres are uniform in shape and controllable in structure. Sodium alginate is a natural polysaccharide compound extracted from kelp or seaweed, has the advantages of low price, biodegradability, high stability, no toxicity, no harm and the like, and is a common embedding base material.
However, the eggshell biochar is difficult to be embedded into balls with alginate due to high inorganic components. The straw biochar has rich pore structures and surface functional groups, and is easily wrapped in alginate microspheres. The straw biochar has wide sources and low price, and about 7 hundred million tons of agricultural straw wastes are generated in China every year. In addition, the biochar can improve the physical and chemical properties of soil, and the composite adsorbent saturated in phosphorus adsorption can be used as a soil conditioner and a phosphorus slow-release fertilizer.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide the eggshell straw biochar composite microsphere dephosphorization adsorbent with high adsorption performance, and the preparation method and the application thereof, so that the loss of effective components is prevented, the mechanical strength of the microsphere is increased, and the size of the adsorbent is improved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of an eggshell straw biochar composite microsphere phosphorus removal adsorbent with high adsorption performance comprises the following steps:
s1: adding the eggshell straw biomass powder into water, and fully mixing to obtain a biochar precursor, wherein the eggshell straw biomass powder comprises eggshells and corn straws in a mass ratio of (0.2-0.6): 1, the mass volume ratio of the eggshell straw biomass powder to water is 1 (10-30) g/mL;
s2: adding the biochar precursor obtained in the step S1 into a sodium alginate aqueous solution with the mass concentration of 3% -6% w/v to obtain mixed slurry, dripping the mixed slurry into a calcium chloride cross-linking solution with the mass concentration of 4% -6% w/v by using a dropper to obtain cross-linked pellets, and hardening, cleaning and drying the pellets;
s3: and (3) placing the dried small spheres in a tubular furnace, and pyrolyzing the small spheres for 1-3h at the temperature of 600-900 ℃ under the protection of nitrogen or inert gas to obtain the eggshell straw biochar composite microsphere dephosphorization adsorbent.
Further, respectively cleaning, drying, crushing and mixing the eggshells and the corn straws to obtain the eggshell straw biomass powder.
An eggshell straw biochar composite microsphere dephosphorization adsorbent with high adsorption performance, wherein the diameter of the microsphere is 1.5-2.5 mm.
An application of an eggshell straw biochar composite microsphere phosphorus removal adsorbent with high adsorption performance in treating phosphorus-containing wastewater.
Compared with the prior art, the invention has the advantages that:
1. according to the invention, the eggshell and the corn straw are used as raw materials, the eggshell straw biochar composite microspheres are obtained by embedding sea into balls through alginate and then carbonizing the balls at high temperature, and the eggshell straw biochar composite microspheres have ultrahigh phosphorus adsorption performance, are easy to obtain raw materials, and are simple in process and low in cost;
2. the straw can improve the crosslinking performance and mechanical strength of the microspheres, the eggshell biochar is wrapped in the porous microspheres, the loss of effective components is prevented, the dispersion performance of the effective components can be improved, and the straw has the advantages of good mass transfer, short adsorption balance time, high adsorption efficiency and the like;
3. the mechanical strength of the microspheres is improved, the size of the adsorbent is improved, the eggshell straw biochar composite microspheres can avoid blockage of a fixed bed by utilizing the advantage of large size of the microspheres, and industrial application of the adsorbent is realized.
Drawings
FIG. 1 is a scanning electron micrograph and a real photograph of the products obtained in example 2 and comparative examples 1 to 4
Wherein, a is a photo of the product prepared in comparative example 1; b, photo of product prepared in comparative example 2; c, photo of product prepared in comparative example 3; d, photo of product prepared in comparative example 4; e, photo of product prepared in example 2; scanning electron microscope image of the product prepared in comparative example 1; scanning electron microscope images of the product prepared in comparative example 2; h, scanning electron microscope images of the product prepared in the comparative example 3; scanning electron microscope images of the product prepared in comparative example 4; scanning electron micrograph of example 2 preparation.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the invention thereto.
1. The preparation process of the eggshell straw biochar composite microspheres comprises the following steps:
(1) respectively cleaning eggshells and corn straws, drying, crushing and mixing to obtain eggshell straw biomass powder. Then adding the mixture into water, fully oscillating and uniformly mixing to obtain a biochar precursor; wherein the mass ratio of the egg shells to the corn straws is (0.2-0.6): 1, the mass volume ratio of the eggshell straw biomass powder to water is 1 (10-30) g/mL;
(2) adding the charcoal precursor into a sodium alginate aqueous solution, and uniformly stirring; dripping the mixed slurry into calcium chloride cross-linking solution by using a dropper to obtain cross-linked pellets, hardening for 10-20h, cleaning and drying; the mass concentration of the sodium alginate is 3-6% w/v, and the concentration of the calcium chloride solution is 4-6% w/v;
(3) and putting the dried small balls into a tubular furnace, and pyrolyzing for 1-3h at the temperature of 600-900 ℃ under the protection of nitrogen or inert gas to obtain the eggshell straw biochar composite microspheres.
2. Test of phosphorus adsorption performance of eggshell straw biochar composite microspheres
Water treatment: phosphorus-containing simulated wastewater
Adsorption conditions: the phosphate concentration is 100mg P/L, and the adsorption temperature is room temperature; the ratio (mass ratio of the adsorbent to the phosphorus-containing wastewater) is 3: 5000; adsorbing for 50-150 min.
The equilibrium adsorption capacity of the adsorbent is calculated according to the following formula:
example 1:
10g of egg shell and corn stalk biomass powder (the mass ratio of the egg shell to the corn stalk is 0.2: 1) are added into 200mL of purified water, and the mixture is fully oscillated and uniformly mixed. Then adding sodium alginate aqueous solution (mass concentration is 5% w/v), stirring uniformly, dripping the mixed slurry into calcium chloride (mass concentration is 5% w/v) crosslinking solution by using a dropper to obtain crosslinking pellets, hardening for 15h, cleaning and drying. And putting the dried small balls into a tubular furnace, and pyrolyzing for 2 hours at 700 ℃ under the protection of nitrogen to obtain the eggshell straw biochar composite microspheres.
Example 2:
10g of egg shell and corn stalk biomass powder (the mass ratio of the egg shell to the corn stalk is 0.4: 1) are added into 200mL of purified water, and the mixture is fully oscillated and uniformly mixed. Then adding sodium alginate aqueous solution (mass concentration is 5% w/v), stirring uniformly, dripping the mixed slurry into calcium chloride (mass concentration is 5% w/v) crosslinking solution by using a dropper to obtain crosslinking pellets, hardening for 15h, cleaning and drying. And putting the dried small balls into a tubular furnace, and pyrolyzing for 2 hours at 700 ℃ under the protection of nitrogen to obtain the eggshell straw biochar composite microspheres.
Example 3:
10g of egg shell and corn stalk biomass powder (the mass ratio of the egg shell to the corn stalk is 0.4: 1) are added into 200mL of purified water, and the mixture is fully oscillated and uniformly mixed. Then adding sodium alginate aqueous solution (mass concentration is 5% w/v), stirring uniformly, dripping the mixed slurry into calcium chloride (mass concentration is 5% w/v) crosslinking solution by using a dropper to obtain crosslinking pellets, hardening for 15h, cleaning and drying. And putting the dried small balls into a tubular furnace, and pyrolyzing the small balls for 2 hours at 800 ℃ under the protection of nitrogen to obtain the eggshell straw biochar composite microspheres.
Example 4:
10g of egg shell and corn stalk biomass powder (the mass ratio of the egg shell to the corn stalk is 0.6: 1) are added into 100mL of purified water, and the mixture is fully oscillated and uniformly mixed. Then adding sodium alginate aqueous solution (the mass concentration is 3% w/v), stirring uniformly, dripping the mixed slurry into calcium chloride (the mass concentration of egg shells and corn straws is 4% w/v) crosslinking solution by using a dropper to obtain crosslinking pellets, hardening for 15h, cleaning and drying. And putting the dried small balls into a tubular furnace, and pyrolyzing for 3 hours at 600 ℃ under the protection of nitrogen to obtain the eggshell straw biochar composite microspheres.
Example 5:
10g of egg shell and corn straw biomass powder (the mass ratio of the egg shell to the corn straw is 0.5: 1) are added into 300mL of purified water, and the mixture is fully oscillated and uniformly mixed. Then adding sodium alginate aqueous solution (mass concentration is 6% w/v), stirring uniformly, dripping the mixed slurry into calcium chloride (mass concentration is 6% w/v) crosslinking solution by using a dropper to obtain crosslinking pellets, hardening for 15h, cleaning and drying. And putting the dried small balls into a tubular furnace, and pyrolyzing for 1h at 900 ℃ under the protection of nitrogen to obtain the eggshell straw biochar composite microspheres.
Comparative example 1
5.0g of eggshell biomass powder is put into a tube furnace and pyrolyzed for 2 hours at 700 ℃ under the protection of nitrogen to obtain the eggshell biomass powder.
Comparative example 2
And (3) putting 5.0g of corn straw biomass powder into a tubular furnace, and pyrolyzing the corn straw biomass powder for 2 hours at 700 ℃ under the protection of nitrogen to obtain the corn straw biomass powder.
Comparative example 3
10g of eggshell biomass powder is added into 200mL of purified water, and the mixture is fully shaken and uniformly mixed. Then adding sodium alginate aqueous solution (mass concentration is 5% w/v), stirring uniformly, dripping the mixed slurry into calcium chloride (mass concentration is 5% w/v) crosslinking solution by using a dropper to obtain crosslinking pellets, hardening for 15h, cleaning and drying. And putting the dried small spheres into a tubular furnace, and pyrolyzing for 2 hours at 700 ℃ under the protection of nitrogen to obtain the eggshell biochar composite microspheres.
Comparative example 4
10g of eggshell biomass powder is added into 200mL of purified water, and the mixture is fully shaken and uniformly mixed. Then adding sodium alginate aqueous solution (mass concentration is 5% w/v), stirring uniformly, dripping the mixed slurry into calcium chloride (mass concentration is 5% w/v) crosslinking solution by using a dropper to obtain crosslinking pellets, hardening for 15h, cleaning and drying. And putting the dried pellets into a tubular furnace, and pyrolyzing for 2 hours at 700 ℃ under the protection of nitrogen to obtain the straw biochar composite microspheres.
Comparative example 5
Crushing the microspheres of example 2 to obtain the eggshell straw biochar composite powder. The mass transfer and adsorption performance of the microspheres is examined by comparing the mass transfer performance with the microspheres.
Test one:
the prepared examples 1 to 3 and comparative examples 1 to 5 were subjected to phosphate adsorption performance tests, 30mL of fluoride ion solution with an initial concentration of 100mg P/L was added to a PVC reaction flask, the amount of the adsorbent added was 15mg, the mixture was magnetically stirred for 60min, and after stirring, the mixture was centrifuged to measure the phosphate concentration in the supernatant, and the adsorption results are shown in table 1.
TABLE 1
As can be seen from table 1, the prepared eggshell straw biochar composite microspheres (examples 1-3) have ultrahigh adsorption capacity to phosphate, and the adsorption capacity increases with the proportion of eggshell and the increase of pyrolysis temperature. The eggshell powder (comparative example 1) has low phosphorus adsorption capacity, the straw powder (comparative example 2) has almost no phosphorus adsorption effect, and the phosphorus adsorption capacity after calcium alginate cross-linking to balls is improved (comparative examples 3 and 4), and the fact that calcium in the cross-linking agent reacts with phosphorus is presumed. Compared with the crushed powder (comparative example 5), the prepared eggshell straw biochar composite microspheres have the similar phosphorus adsorption amount. The effective components in the egg shells are uniformly dispersed by the microspheres, so that the adsorption capacity of the microspheres on phosphate is improved, and the microspheres have good mass transfer performance.
As can be seen from figure 1, the eggshell charcoal powder is yellow brown and has a porous structure (a, f in figure 1), and the corn stalk charcoal is black powder and has a porous rod-shaped structure (b, g in figure 1). The biological carbon microsphere of the eggshell has poor balling effect and loose texture, the pores on the surface of the eggshell are covered after balling (c and h in figure 1), while the biological carbon microsphere of the straw has good balling effect and hard texture, and the porous structure of the straw still exists after balling (d and i in figure 1). As can be seen from e, j in FIG. 1, example 2 has a good effect of balling, the diameter of the microsphere is between 1.5 mm and 2.5mm, and a small amount of eggshell carbon fragments are attached to the surface of the straw carbon. The crosslinking effect with eggshells and calcium alginate is poor and the balling effect is poor, and the balling effect and the mechanical strength of the microspheres can be improved by adding the straws.
The present invention is described in detail with reference to the above embodiments, and those skilled in the art will understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.
Claims (5)
1. A preparation method of an eggshell straw biochar composite microsphere phosphorus removal adsorbent with high adsorption performance is characterized by comprising the following steps:
s1: adding the eggshell straw biomass powder into water, and fully mixing to obtain a biochar precursor, wherein the eggshell straw biomass powder comprises eggshells and corn straws in a mass ratio of (0.2-0.6): 1, the mass volume ratio of the eggshell straw biomass powder to water is 1 (10-30) g/mL;
s2: adding the biochar precursor obtained in the step S1 into a sodium alginate aqueous solution with the mass concentration of 3% -6% w/v to obtain mixed slurry, dripping the mixed slurry into a calcium chloride cross-linking solution with the mass concentration of 4% -6% w/v by using a dropper to obtain cross-linked pellets, and hardening, cleaning and drying the pellets;
s3: and (3) placing the dried small spheres in a tubular furnace, and pyrolyzing the small spheres for 1-3h at the temperature of 600-900 ℃ under the protection of nitrogen or inert gas to obtain the eggshell straw biochar composite microsphere dephosphorization adsorbent.
2. The preparation method of the eggshell straw biochar composite microsphere phosphorus removal adsorbent with high adsorption performance according to claim 1, which is characterized by comprising the following steps: the eggshell and the corn straw are respectively cleaned, dried, crushed and mixed to obtain the eggshell straw biomass powder.
3. The eggshell straw biochar composite microsphere phosphorus removal adsorbent with high adsorption performance prepared by the preparation method according to claim 1 or 2.
4. The eggshell straw biochar composite microsphere phosphorus removal adsorbent with high adsorption performance according to claim 3, which is characterized in that: the diameter of the microsphere is 1.5-2.5 mm.
5. The application of the eggshell straw biochar composite microsphere phosphorus removal adsorbent with high adsorption performance in treating phosphorus-containing wastewater according to claim 3 or 4.
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| CN112694146A (en) * | 2021-01-05 | 2021-04-23 | 上海万狮环保科技有限公司 | Efficient composite phosphorus removal agent, preparation method and application |
| CN112705165A (en) * | 2021-01-05 | 2021-04-27 | 中国科学院青岛生物能源与过程研究所 | Preparation method and application of shell-straw-based calcium-rich biochar |
| CN114480247A (en) * | 2022-02-23 | 2022-05-13 | 北京工业大学 | Immobilized biochar composite material and application thereof |
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| CN114950364A (en) * | 2022-05-23 | 2022-08-30 | 四川大学 | Biomass fast pyrolysis residue-based porous carbon sphere and preparation method and application thereof |
| CN115106063A (en) * | 2022-07-06 | 2022-09-27 | 重庆大学 | Porous biochar prepared from eggshells and orange peels and application of porous biochar in phosphorus removal |
| CN115722190A (en) * | 2022-11-17 | 2023-03-03 | 同济大学 | Preparation method of crop straw hydrothermal biochar by modifying eggshells |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112456627A (en) * | 2020-11-06 | 2021-03-09 | 中南大学 | Calcium phosphorus removal agent with slow release function and preparation method and application thereof |
| CN112694146A (en) * | 2021-01-05 | 2021-04-23 | 上海万狮环保科技有限公司 | Efficient composite phosphorus removal agent, preparation method and application |
| CN112705165A (en) * | 2021-01-05 | 2021-04-27 | 中国科学院青岛生物能源与过程研究所 | Preparation method and application of shell-straw-based calcium-rich biochar |
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| CN114890842A (en) * | 2022-05-17 | 2022-08-12 | 华中农业大学 | Environment-friendly slow-release phosphate fertilizer based on agricultural solid waste value-added utilization and preparation method thereof |
| CN114890842B (en) * | 2022-05-17 | 2023-02-03 | 华中农业大学 | Environment-friendly slow-release phosphate fertilizer based on agricultural solid waste value-added utilization and preparation method thereof |
| CN114950364A (en) * | 2022-05-23 | 2022-08-30 | 四川大学 | Biomass fast pyrolysis residue-based porous carbon sphere and preparation method and application thereof |
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