CN111530415A - Iron-manganese-magnesium-loaded layered hydroxide composite semicoke and preparation method thereof - Google Patents
Iron-manganese-magnesium-loaded layered hydroxide composite semicoke and preparation method thereof Download PDFInfo
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- CN111530415A CN111530415A CN202010324943.5A CN202010324943A CN111530415A CN 111530415 A CN111530415 A CN 111530415A CN 202010324943 A CN202010324943 A CN 202010324943A CN 111530415 A CN111530415 A CN 111530415A
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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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- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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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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- 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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- 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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- 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
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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
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Abstract
The invention relates to the technical field of wastewater treatment, and discloses iron-manganese-magnesium-loaded layered hydroxide composite semicoke and a preparation method thereof3+、Mn2+、Mg2+Ions are introduced into the inner surface and the outer surface of the biomass pyrolysis semicoke through the ion diffusion effect; then through coprecipitation reaction, Fe3+、Mn2+、Mg2+Ions are precipitated on the inner surface and the outer surface of the biomass pyrolysis semicoke to generate layered hydroxide, and finally the iron-manganese-magnesium-loaded layered hydroxide composite semicoke is obtained through washing and freeze drying. The invention combines the biomass pyrolysis semicoke into the water bodyThe Donnan preconcentration effect of inorganic anion pollutants and the high-efficiency removal of phosphorus in wastewater by using the ferrimanganic layered hydroxide are integrated, the defects that the ferrimanganic layered hydroxide is difficult to recover, small in particle size, large in head loss and the like are overcome, the characteristic of quickly and efficiently adsorbing and removing the phosphorus in the wastewater is realized, and the cost is low.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, and particularly relates to iron-manganese-magnesium-loaded layered hydroxide composite semicoke and a preparation method thereof.
Background
The semicoke is a product of coal pyrolysis at a lower temperature (600-; the semicoke must become a novel adsorbent with great market attraction.
The layered hydroxide is commonly called hydrotalcite and has the characteristics of adjustable and controllable chemical components and corresponding adjustable and controllable physical and chemical properties. In recent years, layered hydroxides have become a research hotspot, and benefit from wide application in the aspects of catalysis, ion exchange materials, flame retardant materials, polymer composite materials and the like.
In addition, the metal layered hydroxide can absorb phosphorus in the wastewater, but due to the defects of small metal layered hydroxide particles, large head loss, difficult recovery and the like, in the actual operation process, a lot of defects still exist, and the effect of deep phosphorus removal of the wastewater is directly influenced.
Disclosure of Invention
Based on the problems, the invention provides the iron-manganese-magnesium-loaded layered hydroxide composite semicoke and the preparation method thereof, which combine the Donnan pre-enrichment effect of the biomass pyrolysis semicoke on inorganic anion pollutants in a water body and the efficient removal of phosphorus in wastewater by using the iron-manganese-magnesium layered hydroxide into a whole, overcome the defects of difficult recovery, small particles, large head loss and the like of the iron-manganese-magnesium layered hydroxide, have the characteristics of rapid and efficient adsorption removal of the phosphorus in the wastewater, and have lower cost.
In order to solve the technical problems, the invention provides an iron-manganese-magnesium-loaded layered hydroxide composite semicoke which comprises a biomass pyrolysis semicoke with pore passages distributed in the interior and electron constraint characteristics, wherein iron-manganese-magnesium layered hydroxides with layered structures are immobilized on the inner surface and the outer surface of the biomass pyrolysis semicoke.
Furthermore, the aperture of the inner pore channel of the biomass pyrolysis semicoke is 10-500 nm.
Further, the ferrimanganic magnesium layered hydroxide is of a lamellar structure, and the size of the layered hydroxide is 50-200 nm.
Further, the framework of the biomass pyrolysis semicoke is an incompletely carbonized fixed carbon chain, and the fixed carbon chain contains basic oxygen-containing groups, wherein the basic oxygen-containing groups comprise carbonyl or phenolic hydroxyl.
Further, the biomass pyrolysis semicoke raw material is agricultural waste, and the agricultural waste comprises corn, wheat or rice straws.
In order to solve the technical problem, the invention also provides a preparation method of the iron-manganese-magnesium-loaded layered hydroxide composite semicoke, which comprises the following steps:
s1, adding 2-10 g of biomass pyrolysis semicoke into 50-150 ml of water, simultaneously adding 5-15 ml of ethanol into the water, stirring for 20-40 min, and performing suction filtration and washing to obtain a sample 1;
s2, preparing 150-200 ml FeCl-containing3、MnCl2、MgCl2The mixed solution of (1), FeCl in the mixed solution3、MnCl2、MgCl2The total substance amount concentration is 2mol/L, 15-25ml of hydrochloric acid with the mass fraction of 37% is added into the mixed solution, 2-10 g of the sample 1 is added into the mixed solution, and the mixed solution is stirred for 2-6 hours to obtain a mixed sample 2;
s3, under the protection of nitrogen atmosphere, continuously stirring the mixed sample 2, gradually dropwise adding alkali liquor into the mixed sample 2, adjusting the pH value to 9-10, continuously stirring for 2-4 h after dropwise adding is completed, performing suction filtration washing, and performing freeze drying to obtain the iron-manganese-magnesium-loaded layered hydroxide composite semicoke; wherein the alkali liquor is prepared by dissolving NaOH or KOH in oxygen-free water, the concentration is 1-6 mol/L, and the dropping speed is 0.5 ml/min.
Further, in step S2, FeCl3：MnCl2：MgCl2The ratio of the amounts of the substances of (a) to (b) is 1:1: 2.
Further, in step S3, the freeze-drying condition is freeze-drying for 72 hours at a temperature of-40 to-20 ℃ and a vacuum degree of 30 to 100 Pa.
Compared with the prior art, the invention has the beneficial effects that: the method combines the Donnan preconcentration effect of the biomass pyrolysis semicoke on inorganic anion pollutants in the water body and the high-efficiency removal of phosphorus in the wastewater by the ferrimanganic layered hydroxide, overcomes the defects of difficult recovery, small particles, large head loss and the like of the ferrimanganic layered hydroxide, has the characteristics of quick and high-efficiency adsorption removal of the phosphorus in the wastewater, and has low cost.
Drawings
FIG. 1 is an electron microscope scan of the biomass pyrolysis semicoke of example 1;
FIG. 2 is a scanning electron microscope image of the layered hydroxide of Fe, Mn and Mg with magnification of 40000 times in example 1;
FIG. 3 is an electron micrograph of the FeMnMgLDHs of example 1 magnified 100000 times.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1:
referring to fig. 1-3, the iron-manganese-magnesium-loaded layered hydroxide composite semicoke comprises a biomass pyrolysis semicoke with pore channels distributed inside and electron-binding characteristics, wherein iron-manganese-magnesium layered hydroxides with layered structures are immobilized on the inner and outer surfaces of the biomass pyrolysis semicoke.
In the embodiment, the pore diameter of the inner pore channel of the biomass pyrolysis semicoke is 10-500 nm, the biomass pyrolysis semicoke with good pore channel distribution and huge specific surface area is used as a carrier, and Fe is used as the carrier3+、Mn2+、Mg2+Ions are introduced into the inner surface and the outer surface of the biomass pyrolysis semicoke through the ion diffusion effect; then through coprecipitation reaction, Fe3+、Mn2+、Mg2+Ion pyrolysis of biomassPrecipitating the inner surface and the outer surface of the coke to generate a lamellar iron-manganese-magnesium layered hydroxide, wherein the size of the layered hydroxide is 50-200 nm; and finally, washing, freezing and drying to obtain the iron-manganese-magnesium-loaded layered hydroxide composite semicoke. The removal mechanism of the ferromanganese magnesium layered hydroxide to the phosphorus in the wastewater is the interlayer anion exchange and the coordination of the phosphate ions on the surface and Fe/Mn/Mg ions; and the particle size distribution of the layered hydroxide is in a nanometer or submicron scale (as shown in figures 2 and 3), the particles of the semicoke are often in a micron or millimeter scale (as shown in figure 1), and the layered manganese-magnesium layered hydroxide is deposited on the inner and outer surfaces of the biomass pyrolysis semicoke, including the inner and surface of a pore channel of a half corner, so that solid-liquid separation is easier and recovery is easier. The method combines the Donnan preconcentration effect of the biomass pyrolysis semicoke on inorganic anion pollutants in a water body and the high-efficiency removal of phosphorus in the wastewater by using the ferrimanganic layered hydroxide, overcomes the defects of difficult recovery, small particles, large head loss and the like of the ferrimanganic layered hydroxide, and has the characteristics of quick, high-efficiency and low-cost adsorption removal of the phosphorus in the wastewater.
The biomass pyrolysis semicoke raw material of the embodiment is agricultural waste, the agricultural waste comprises corn, wheat or rice straws, the raw material is thermally pyrolyzed to form biomass pyrolysis semicoke with a framework of a fixed carbon chain, and the biomass pyrolysis semicoke is incompletely carbonized, the fixed carbon chain contains alkaline oxygen-containing groups, and the alkaline oxygen-containing groups comprise carbonyl or phenolic hydroxyl groups, so that the deposition of iron-manganese-magnesium layered hydroxide on the surface of the biomass pyrolysis semicoke is facilitated.
Example 2:
a preparation method of iron-manganese-magnesium-loaded layered hydroxide composite semicoke comprises the following steps:
s1, adding 2-10 g of biomass pyrolysis semicoke into 50-150 ml of water, simultaneously adding 5-15 ml of ethanol into the water, stirring for 20-40 min, and performing suction filtration and washing to obtain a sample 1;
s2, preparing 150-200 ml FeCl-containing3、MnCl2、MgCl2The mixed solution of (1), FeCl in the mixed solution3、MnCl2、MgCl2The total substance amount concentration is 2mol/L, 15-25ml hydrochloric acid with the mass fraction of 37 percent is added into the mixed solution,adding 2-10 g of the sample 1 into the mixed solution, and stirring for 2-6 h to obtain a mixed sample 2; the hydrochloric acid is added to keep the mixed solution in an acidic state during stirring, prevent hydroxide precipitation from occurring in the mixed solution and facilitate Fe3+、Mn2+、Mg2+The ions are uniformly dispersed in the mixed solution.
And S3, under the protection of nitrogen atmosphere, continuously stirring the mixed sample 2, gradually dropwise adding an alkali liquor into the mixed sample 2, adjusting the pH value to 9-10, and continuously stirring for 2-4 hours after dropwise adding, wherein the alkali liquor is prepared by dissolving NaOH or KOH in oxygen-free water, the concentration is 1-6 mol/L, and the dropwise adding speed is 0.5 ml/min. By coprecipitation reaction, Fe3+、Mn2+、Mg2+Ions are precipitated on the inner surface and the outer surface of the biomass pyrolysis semicoke to generate the lamellar iron-manganese-magnesium layered hydroxide. Finally, carrying out suction filtration washing and freeze drying to obtain the iron-manganese-magnesium-loaded layered hydroxide composite semicoke; in the embodiment, the freeze drying condition is that the freeze drying is carried out for 72 hours at the temperature of minus 40 to minus 20 ℃ and the vacuum degree of 30 to 100 Pa.
Example 3
A preparation method of iron-manganese-magnesium-loaded layered hydroxide composite semicoke comprises the following steps:
s1, taking 5g of biomass pyrolysis semicoke with good pore channel distribution and stable skeleton, adding 10ml of ethanol and 100ml of water into a three-neck flask, stirring for 30min, and repeatedly performing suction filtration and washing for 3 times to obtain a sample 1.
S2, sample 1 was transferred to a three-necked flask, and 10ml of 37% concentrated hydrochloric acid and 190ml of FeCl were added3/MnCl2/MgCl2Mixing the solution in which FeCl is3：MnCl2：MgCl2The amount ratio of the substances is 1:1:2, stirring for 4h to obtain a mixed sample 2;
s3, under the protection of nitrogen atmosphere and under the condition of continuous stirring, dropwise adding 2mol/L NaOH into the prepared mixed sample 2, adjusting the pH value to 10, continuously stirring for 2h after dropwise adding, carrying out suction filtration and washing, and then carrying out freeze drying for 72h at-40 ℃ and 40Pa to obtain the iron-manganese-magnesium-loaded layered hydroxide composite semicoke 1.
Taking the prepared iron-manganese-magnesium-loaded layered hydroxide composite semicoke 1 to perform a phosphorus removal test on sample wastewater, wherein the phosphorus content in the sample wastewater is 1-10 mgP/L, putting the iron-manganese-magnesium-loaded layered hydroxide composite semicoke 1 into the sample wastewater, and detecting and calculating the removal rate, wherein the removal rate is shown in the following table:
the invention has the following beneficial effects: the method combines the Donnan preconcentration effect of the biomass pyrolysis semicoke on inorganic anion pollutants in the water body and the high-efficiency removal of phosphorus in the wastewater by the ferrimanganic layered hydroxide, overcomes the defects of small ferrimanganic layered hydroxide particles, large head loss, difficult recovery and the like, and has the characteristics of quick, high-efficiency and low-cost adsorption removal of the phosphorus in the wastewater.
The above is an embodiment of the present invention. The embodiments and specific parameters in the embodiments are only for the purpose of clearly illustrating the verification process of the invention and are not intended to limit the scope of the invention, which is defined by the claims, and all equivalent structural changes made by using the contents of the specification and the drawings of the present invention should be covered by the scope of the present invention.
Claims (8)
1. The iron-manganese-magnesium-loaded layered hydroxide composite semicoke is characterized in that: the biomass pyrolysis semicoke comprises a biomass pyrolysis semicoke with pore channels distributed in the biomass pyrolysis semicoke and electron-binding characteristics, wherein iron-manganese-magnesium layered hydroxides with layered structures are immobilized on the inner surface and the outer surface of the biomass pyrolysis semicoke.
2. The iron-manganese-magnesium-loaded layered hydroxide composite semicoke according to claim 1, wherein: the aperture of the inner pore canal of the biomass pyrolysis semicoke is 10-500 nm.
3. The iron-manganese-magnesium-loaded layered hydroxide composite semicoke according to claim 1, wherein: the iron-manganese-magnesium layered hydroxide is of a lamellar structure, and the size of the layered hydroxide is 50-200 nm.
4. The iron-manganese-magnesium-loaded layered hydroxide composite semicoke according to any one of claims 1 to 3, wherein: the framework of the biomass pyrolysis semicoke is a fixed carbon chain which is not completely carbonized, and the pyrolyzed fixed carbon chain contains alkaline oxygen-containing groups, wherein the alkaline oxygen-containing groups comprise carbonyl or phenolic hydroxyl.
5. The iron-manganese-magnesium-loaded layered hydroxide composite semicoke according to claim 4, wherein: the biomass pyrolysis semicoke raw material is agricultural waste, and the agricultural waste comprises corn, wheat or rice straw.
6. The preparation method of the iron-manganese-magnesium-loaded layered hydroxide composite semicoke is characterized by comprising the following steps of:
s1, adding 2-10 g of biomass pyrolysis semicoke into 50-150 ml of water, simultaneously adding 5-15 ml of ethanol into the water, stirring for 20-40 min, and performing suction filtration and washing to obtain a sample 1;
s2, preparing 150-200 ml FeCl-containing3、MnCl2、MgCl2The mixed solution of (1), FeCl in the mixed solution3、MnCl2、MgCl2The total substance amount concentration is 2mol/L, 15-25ml of hydrochloric acid with the mass fraction of 37% is added into the mixed solution, 2-10 g of the sample 1 is added into the mixed solution, and the mixed solution is stirred for 2-6 hours to obtain a mixed sample 2;
s3, under the protection of nitrogen atmosphere, continuously stirring the mixed sample 2, gradually dropwise adding alkali liquor into the mixed sample 2, adjusting the pH value to 9-10, continuously stirring for 2-4 h after dropwise adding is completed, performing suction filtration washing, and performing freeze drying to obtain the iron-manganese-magnesium-loaded layered hydroxide composite semicoke; wherein the alkali liquor is prepared by dissolving NaOH or KOH in oxygen-free water, the concentration is 1-6 mol/L, and the dropping speed is 0.5 ml/min.
7. The preparation method of the iron-manganese-magnesium-loaded layered hydroxide composite semicoke according to claim 6, characterized by comprising the following steps: in step (b)In step S2, FeCl3：MnCl2：MgCl2The ratio of the amounts of the substances of (a) to (b) is 1:1: 2.
8. The preparation method of the iron-manganese-magnesium-loaded layered hydroxide composite semicoke according to claim 6, characterized by comprising the following steps: in step S3, the freeze-drying condition is freeze-drying for 72h at-40 to-20 ℃ and 30 to 100Pa vacuum degree.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113274550A (en) * | 2021-05-31 | 2021-08-20 | 福州大学 | Vascularized bone bionic multifunctional tissue engineering scaffold with anti-inflammatory effect and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113274550A (en) * | 2021-05-31 | 2021-08-20 | 福州大学 | Vascularized bone bionic multifunctional tissue engineering scaffold with anti-inflammatory effect and preparation method thereof |
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