CN113351162B - Preparation method and application of carbon-based phosphorus-doped ferrihydrite - Google Patents

Preparation method and application of carbon-based phosphorus-doped ferrihydrite Download PDF

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CN113351162B
CN113351162B CN202110630935.8A CN202110630935A CN113351162B CN 113351162 B CN113351162 B CN 113351162B CN 202110630935 A CN202110630935 A CN 202110630935A CN 113351162 B CN113351162 B CN 113351162B
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carbon
mixed solution
solution
based phosphorus
doped ferrihydrite
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CN113351162A (en
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张颖
江群
李辉
李绍峰
王欢
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Northeast Agricultural University
Shenzhen Polytechnic
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Shenzhen Polytechnic
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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
    • B01J20/20—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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • 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
    • 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
    • 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
    • B01J2220/4812—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
    • 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
    • B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
    • 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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Abstract

A preparation method and application of carbon-based phosphorus-doped ferrihydrite, relating to the technical field of water treatment. The invention aims to solve the problem that the traditional adsorbent has low adsorption efficiency on heavy metal lead. The method comprises the following steps: 1 mol. L ‑1 KH of 2 PO 4 The solution is added to 5 mol.L ‑1 Uniformly stirring in the KOH solution to obtain a mixed solution B; dropwise adding the mixed solution A into the mixed solution B at the temperature of 60-80 ℃, and continuously stirring for 48-72 hours after dropwise adding to obtain a mixed solution C, wherein the molar ratio of Fe/P elements in the mixed solution C is 1:1; aging the mixed solution C for 24-48 h at the temperature of 60-80 ℃, washing with deionized water for 3-5 times, centrifuging, drying, grinding, and sieving with a 100-mesh sieve to obtain the carbon-based phosphorus-doped ferrihydrite. The invention can obtain a preparation method and application of the carbon-based phosphorus-doped ferrihydrite.

Description

Preparation method and application of carbon-based phosphorus-doped ferrihydrite
Technical Field
The invention relates to the technical field of water treatment, in particular to a preparation method and application of carbon-based phosphorus-doped ferrihydrite.
Background
In recent years, with the rapid development of industry and agriculture, a plurality of serious environmental pollution problems appear. Heavy metal pollution is typical environmental pollution, can exist in natural environment for a long time, cannot be degraded, has great harm to natural ecology, and can finally enter human bodies through accumulation of microorganisms, animals and plants. Lead is a common heavy metal pollutant in the environment, has long half-life period in a human body, can act on various systems and organs of the whole body due to toxicity, and mainly affects the nervous system, the hematopoietic system, the digestive system, the cardiovascular system, the kidney system, the immune system and other systems. It is therefore desirable to find an efficient, economical and stable adsorbent for the treatment of lead pollution.
At present, the common heavy metal adsorbents comprise lime materials, phosphates, iron-based materials, silicates, high-molecular organic curing agents and the like. However, the conventional adsorbents have limited adsorption capacity due to limited specific surface area, few active sites or few pores, and thus, the development of excellent modified adsorbents is the focus of research. The iron-based material is convenient and easy to obtain, has a large specific surface area and abundant active sites, but the iron-based nano material is easy to agglomerate to limit the large-scale application of the iron-based nano material. Biochar has proved to be a large specific surface, porous, multilayer material, applicable to material supports. Therefore, how to use the biochar as a substrate and develop a high-efficiency heavy metal adsorbent by combining with the iron oxide material is a significant research.
Disclosure of Invention
The invention aims to solve the problem that the traditional adsorbent has low adsorption efficiency on heavy metal lead, and provides a preparation method and application of carbon-based phosphorus-doped ferrihydrite.
A preparation method of carbon-based phosphorus-doped ferrihydrite comprises the following steps:
1. placing biomass powder in a tubular furnace, heating to 600-800 ℃ under the atmosphere of inert gas, preserving heat for 1-2 h at the temperature of 600-800 ℃, cooling to room temperature after heat preservation, grinding, and sieving with a 150-mesh sieve to obtain biochar; adding biochar to Fe (NO) 3 ) 3 Uniformly mixing the solution to obtain a mixed solution A, wherein the mass of the biochar is equal to that of Fe (NO) 3 ) 3 The volume ratio of the solution is (2-3 g): (50-75 mL);
2. 1 mol. L -1 KH (K) 2 PO 4 The solution is added to 5 mol.L -1 The KOH solution is evenly stirred to obtain a mixed solution B, and the KH solution B is 2 PO 4 The volume ratio of the solution to the KOH solution is (50-75): (100 to 150); dropping the mixed solution A at the temperature of 60-80 DEG CAdding the mixture into the mixed solution B, and continuously stirring for 48-72 hours after the dropwise adding is finished to obtain a mixed solution C, wherein the molar ratio of Fe/P elements in the mixed solution C is 1:1; and aging the mixed solution C for 24-48 h at the temperature of 60-80 ℃, washing with deionized water for 3-5 times, centrifuging, drying, grinding, and sieving with a 100-mesh sieve to obtain the carbon-based phosphorus-doped ferrihydrite.
The application of the carbon-based phosphorus-doped ferrihydrite is used for adsorbing heavy metal lead in wastewater, and when the concentration of the lead in the wastewater is 250mg/L, the adding amount of the carbon-based phosphorus-doped ferrihydrite is 1g/L.
The invention has the beneficial effects that:
(1) According to the preparation method of the carbon-based phosphorus-doped ferrihydrite, biochar prepared by pyrolysis is used as an adsorbent carrier, and phosphorus-doped ferrihydrite nano particles are uniformly dispersed on the surface of the biochar by a hydration method, so that the condition that adsorption action is influenced due to easy agglomeration of phosphorus-doped ferrihydrite nano materials is avoided, meanwhile, the biochar has the advantage of large specific surface area, so that the adsorption performance of an adsorption material is more excellent, the prepared carbon-based phosphorus-doped ferrihydrite can efficiently remove heavy metal lead in wastewater, and the efficiency of removing the lead in the wastewater by using the carbon-based phosphorus-doped ferrihydrite adsorbent is up to more than 91%.
(2) According to the invention, the agricultural typical biomass waste corn straw is used as a carrier, the ferrihydrite material is obtained in a phosphorus-doped mode, and the prepared carbon-based phosphorus-doped ferrihydrite has higher adsorption effect and higher economical efficiency compared with other adsorbents, can be used for treating wastewater containing heavy metal, provides improved conditions for application of charcoal, and has important application value for removing heavy metal with low cost, high efficiency and environmental friendliness.
(3) The preparation method is simple, the raw materials are easy to obtain, the price is low, the production cost is reduced, and the resource utilization of the waste biomass is realized.
The invention can obtain a preparation method and application of carbon-based phosphorus-doped ferrihydrite.
Drawings
FIG. 1 is an SEM photograph of the carbon-based phosphorus-doped ferrihydrite prepared in example 1;
FIG. 2 is a graph showing the adsorption of lead by the carbon-based phosphorus-doped ferrihydrite prepared in example 1 as a function of time;
FIG. 3 is a first order kinetics fit plot of the adsorption kinetics curve for the carbon-based phosphorus-doped ferrihydrite prepared in example 1;
fig. 4 is a pseudo-second order kinetic fit of the adsorption kinetic curve of the carbon-based phosphorus-doped ferrihydrite prepared in example 1.
Detailed Description
The first specific implementation way is as follows: the preparation method of the carbon-based phosphorus-doped ferrihydrite comprises the following steps:
1. placing biomass powder in a tubular furnace, heating to 600-800 ℃ under the atmosphere of inert gas, preserving heat for 1-2 h at the temperature of 600-800 ℃, cooling to room temperature after heat preservation, grinding, and sieving with a 150-mesh sieve to obtain biochar; adding biochar to Fe (NO) 3 ) 3 Uniformly mixing the solution to obtain a mixed solution A, wherein the mass of the biochar is equal to that of Fe (NO) 3 ) 3 The volume ratio of the solution is (2-3 g): (50-75 mL);
2. 1 mol. L -1 KH (K) 2 PO 4 The solution is added to 5 mol.L -1 The KOH solution is evenly stirred to obtain a mixed solution B, and the KH solution B is 2 PO 4 The volume ratio of the solution to the KOH solution is (50-75): (100 to 150); dropwise adding the mixed solution A into the mixed solution B at the temperature of 60-80 ℃, and continuously stirring for 48-72 hours after dropwise adding to obtain a mixed solution C, wherein the molar ratio of Fe/P elements in the mixed solution C is 1:1; and aging the mixed solution C for 24-48 h at the temperature of 60-80 ℃, washing with deionized water for 3-5 times, centrifuging, drying, grinding, and sieving with a 100-mesh sieve to obtain the carbon-based phosphorus-doped ferrihydrite.
The beneficial effects of the embodiment are as follows:
(1) According to the preparation method of the carbon-based phosphorus-doped ferrihydrite, biochar prepared by pyrolysis is used as an adsorbent carrier, and phosphorus-doped ferrihydrite nanoparticles are uniformly dispersed on the surface of the biochar by a hydration method, so that the condition that adsorption is influenced due to the fact that phosphorus-doped ferrihydrite nano materials are easy to agglomerate is avoided, meanwhile, the biochar has the advantage of being large in specific surface area, and the adsorption performance of an adsorption material is more excellent, so that the prepared carbon-based phosphorus-doped ferrihydrite can be used for efficiently removing heavy metal lead in wastewater, and the efficiency of removing the lead in the wastewater by using the carbon-based phosphorus-doped ferrihydrite adsorbent is up to more than 91%.
(2) According to the embodiment, the agricultural typical biomass waste corn straw is used as a carrier, the ferrihydrite material is obtained in a phosphorus-doped mode, and compared with other adsorbents, the prepared carbon-based phosphorus-doped ferrihydrite has a higher adsorption effect and is more economical, the adsorbent can be used for treating wastewater containing heavy metals, improved conditions are provided for application of biochar, and the adsorbent has an important application value for removing the heavy metals in a cheap, efficient and environmentally-friendly mode.
(3) The preparation method of the embodiment is simple, the raw materials are easy to obtain, the price is low, the production cost is reduced, and the resource utilization of the waste biomass is realized.
The second embodiment is as follows: the present embodiment differs from the present embodiment in that: the biomass powder in the first step is prepared by the following steps: and (2) drying the biomass at room temperature, completely crushing, sieving by a 100-mesh sieve, and drying at 60-80 ℃ to obtain biomass powder, wherein the biomass is crop straws or livestock and poultry manure.
Other steps are the same as in the first embodiment.
The third concrete implementation mode: the first or second differences from the present embodiment are as follows: in the first step, the biomass powder is placed in a tubular furnace, and the temperature is raised to 600-800 ℃ at the speed of 10-20 ℃/min under the atmosphere of inert gas.
The other steps are the same as those in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: introducing inert gas for 30-60 min in the first step, and then heating; the inert gas is nitrogen or argon.
The other steps are the same as those in the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and the first to the fourth embodiments is: in the first step, the biomass powder is placed in a tubular furnace, the temperature is raised to 800 ℃ under the atmosphere of inert gas, and the temperature is kept for 1h under the temperature condition of 800 ℃.
The other steps are the same as those in the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is as follows: the mass of the biochar and Fe (NO) in step one 3 ) 3 The volume ratio of the solution was 2g:50mL.
The other steps are the same as those in the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: in the second step, KH is added 2 PO 4 The volume ratio of the solution to the KOH solution is 1:2.
the other steps are the same as those in the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: and step two, dropwise adding the mixed solution A into the mixed solution B at the temperature of 60 ℃, and continuously stirring for 72 hours after dropwise adding is finished to obtain a mixed solution C.
The other steps are the same as those in the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: and in the second step, aging the mixed solution C for 24h at the temperature of 60 ℃, washing the mixed solution C for 3 times by using deionized water, centrifuging, drying, grinding and sieving by using a 100-mesh sieve to obtain the carbon-based phosphorus-doped ferrihydrite.
The other steps are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: in the application of the carbon-based phosphorus-doped ferrihydrite, the carbon-based phosphorus-doped ferrihydrite is used for adsorbing heavy metal lead in wastewater, and when the concentration of lead in the wastewater is 250mg/L, the adding amount of the carbon-based phosphorus-doped ferrihydrite is 1g/L.
The following examples were used to demonstrate the beneficial effects of the present invention:
example 1: a preparation method of carbon-based phosphorus-doped ferrihydrite comprises the following steps:
1. air-drying the corn straws at room temperature, completely crushing the corn straws by using a crusher, then sieving the crushed corn straws by using a 100-mesh sieve, then placing the crushed corn straws into an oven, and drying the crushed corn straws at 60 ℃ to obtain corn straw powder; placing the corn straw powder in a tube furnace, introducing argon gas in the atmosphere of the argon gas for 30min, heating to 800 ℃ at the speed of 20 ℃/min, preserving the heat at the temperature of 800 ℃ for 1h, cooling to room temperature after the heat preservation is finished, grinding by using a mortar, and sieving by using a 150-mesh sieve to obtain the corn straw-based biochar BC; 2g of corn stover-based biochar BC was added to 50mL of Fe (NO) 3 ) 3 Uniformly mixing the solution to obtain a mixed solution A;
2. 50mL of 1 mol. L -1 KH of 2 PO 4 The solution was added to 100mL of 5 mol. L -1 Uniformly stirring in the KOH solution to obtain a mixed solution B; dropwise adding the mixed solution A into the mixed solution B by using a separating funnel under the temperature condition of 60 ℃, and continuously stirring for 72 hours after dropwise adding is finished to obtain a mixed solution C, wherein the molar ratio of Fe/P elements in the mixed solution C is 1:1; aging the mixed solution C at 60 ℃ for 24h, washing with deionized water for 3 times, centrifuging, drying in a freeze dryer, grinding, and sieving with a 100-mesh sieve to obtain the carbon-based phosphorus-doped ferrihydrite, as shown in figure 1, wherein the carbon-based phosphorus-doped ferrihydrite is uniformly loaded on the surface and in the pores of the biochar, the huge surface area and abundant pores of the biochar provide a large number of positions for adsorption, the adsorption is facilitated, and the adsorption efficiency is improved.
3. Adsorption experiment:
weighing a certain mass of carbon-based phosphorus-doped ferrihydrite, adding the carbon-based phosphorus-doped ferrihydrite into a conical flask filled with a certain volume of pollutant lead solution, sealing the conical flask with a breathable sealing film, putting the conical flask into a constant-temperature shaking table at 25 ℃ for oscillation, and sampling and filtering at 5 th, 10 th, 15 th, 30 th, 60 th, 90 th, 120 th, 180 th, 240 th, 300 th and 360 th min respectively for subsequent tests.
According to the test result of the batch adsorption experiment, as shown in fig. 2, the carbon-based phosphorus-doped ferrihydrite adsorbent is in a rapid adsorption stage 120min before being in a lead solution, and the adsorption capacity can reach 280mg/g when the adsorption capacity reaches 120 min; the slow adsorption stage is carried out at 120-240 min, the adsorption capacity reaches 298mg/g at 240min, and the adsorption capacity does not change greatly when the adsorption capacity reaches 360min finally.
The adsorption experiment result of the carbon-based phosphorus-doped ferrihydrite on lead shows that: when the initial concentration of lead is 250mg/L, the adding amount of the carbon-based phosphorus-doped ferrihydrite is 1g/L, and under the test condition, the adsorption efficiency of the carbon-based phosphorus-doped ferrihydrite on lead is up to 91.3 percent after the reaction is carried out for 180 min.
4. Adsorption kinetics experiment:
fig. 3 to 4 are a pseudo-first order kinetics fitting graph and a pseudo-second order kinetics fitting graph of the adsorption kinetics curve of the carbon-based phosphorus-doped ferrihydrite prepared in example 1, in sequence, as shown in fig. 3 to 4, it can be found that the carbon-based phosphorus-doped ferrihydrite more conforms to the pseudo-second order kinetics, which indicates that the adsorption process is chemisorption-dominated, the binding speed is fast, and the chemical properties are more stable.

Claims (7)

1. A preparation method of carbon-based phosphorus-doped ferrihydrite is characterized by comprising the following steps:
1. placing biomass powder in a tubular furnace, heating to 800 ℃ under an inert atmosphere, preserving heat for 1h at the temperature of 800 ℃, cooling to room temperature after heat preservation is finished, grinding, and sieving with a 150-mesh sieve to obtain biochar; adding biochar to Fe (NO) 3 ) 3 Uniformly mixing the solution to obtain a mixed solution A, wherein the mass of the biochar is equal to that of Fe (NO) 3 ) 3 The volume ratio of the solution was 2g:50mL;
2. 1 mol. L -1 KH of 2 PO 4 The solution is added to 5 mol.L -1 The KOH solution is evenly stirred to obtain a mixed solution B, and the KH solution B is 2 PO 4 The volume ratio of the solution to the KOH solution is (50 to 75): (100 to 150); dropwise adding the mixed solution A into the mixed solution B at the temperature of 60-80 ℃, and continuously stirring for 48-72h after the dropwise adding is finished to obtain a mixed solution C, wherein the molar ratio of Fe/P elements in the mixed solution C is1:1; aging the mixed solution C for 24 to 48h at the temperature of 60 to 80 ℃, washing 3~5 times by using deionized water, centrifuging, drying, grinding, and sieving by using a 100-mesh sieve to obtain the carbon-based phosphorus-doped ferrihydrite; the carbon-based phosphorus-doped ferrihydrite is used for adsorbing heavy metal lead in wastewater, and when the concentration of lead in the wastewater is 250mg/L, the adding amount of the carbon-based phosphorus-doped ferrihydrite is 1g/L.
2. The method for preparing carbon-based phosphorus-doped ferrihydrite according to claim 1, wherein the biomass powder in the first step is prepared by the following steps: and (2) drying the biomass at room temperature, completely crushing, sieving by a 100-mesh sieve, and drying at 60-80 ℃ to obtain biomass powder, wherein the biomass is crop straws or livestock and poultry manure.
3. The method for preparing carbon-based phosphorus-doped ferrihydrite as claimed in claim 1, wherein in the first step, the biomass powder is placed in a tube furnace, and the temperature is increased to 800 ℃ at a speed of 10 to 20 ℃/min under an inert atmosphere.
4. The method for preparing the carbon-based phosphorus-doped ferrihydrite according to claim 1 or 3, characterized in that the temperature is raised after the inert atmosphere is introduced for 30 to 60min in the first step; the inert atmosphere is nitrogen or argon.
5. The method for preparing carbon-based phosphorus-doped ferrihydrite according to claim 1, wherein the KH in the second step 2 PO 4 The volume ratio of the solution to the KOH solution is 1:2.
6. the method for preparing carbon-based phosphorus-doped ferrihydrite according to claim 1, characterized in that in the second step, the mixed solution A is dropwise added into the mixed solution B at a temperature of 60 ℃, and stirring is continued for 72 hours after the dropwise addition is finished, so as to obtain a mixed solution C.
7. The method for preparing carbon-based phosphorus-doped ferrihydrite according to claim 1, wherein in the second step, the mixed solution C is aged at 60 ℃ for 24h, washed with deionized water for 3 times, centrifuged, dried, ground and sieved with a 100-mesh sieve to obtain carbon-based phosphorus-doped ferrihydrite.
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