CN106345397B - Adsorbing material for efficiently removing phosphorus in water body - Google Patents

Adsorbing material for efficiently removing phosphorus in water body Download PDF

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CN106345397B
CN106345397B CN201611000708.2A CN201611000708A CN106345397B CN 106345397 B CN106345397 B CN 106345397B CN 201611000708 A CN201611000708 A CN 201611000708A CN 106345397 B CN106345397 B CN 106345397B
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phosphorus
lanthanum
aluminum
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adsorbent
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CN106345397A (en
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潘纲
徐睿
张美一
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Yantai Hubble algal bloom control and Ecological Restoration Technology Co., Ltd
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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
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0248—Compounds of B, Al, Ga, In, Tl
    • 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
    • B01J20/08—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 comprising aluminium oxide or hydroxide; comprising bauxite
    • 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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  • Inorganic Chemistry (AREA)
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  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
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  • Water Supply & Treatment (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The invention relates to a novel adsorbing material for efficiently removing phosphorus in a water body, and belongs to the technical field of environmental protection. The invention selects lanthanum compound and aluminum compound as raw materials, prepares a high-efficiency phosphorus removal adsorbent by a coprecipitation method, and can effectively remove different types of phosphorus in water body through electrostatic attraction, ligand exchange and the action of oxygen vacancy on the surface of the adsorbent. Compared with the existing phosphorus removal adsorbent, the phosphorus removal adsorbent has the advantages of simple preparation process, low production cost, high phosphorus removal efficiency, lasting phosphorus fixation effect, low ecological safety risk, wide pH application range and convenience in storage, transportation and use.

Description

Adsorbing material for efficiently removing phosphorus in water body
(I) technical field
The invention relates to an adsorbing material for efficiently removing phosphorus in a water body, and belongs to the technical field of environmental protection.
(II) background of the invention
Eutrophication of water has become one of the important water resource problems facing mankind. At present, about 30 to 40 percent of lakes and reservoirs worldwide have eutrophication levels of different degrees. The eutrophication problem of lakes in China is more severe, and the area is more than 1km2More than 56% of the 2300 lakes are in eutrophication state or are threatened by eutrophication. More than 80% of eutrophic lakes in the world belong to phosphorus-limited lakes, and the eutrophication process of most lakes in China is controlled by phosphorus nutritive salt. Therefore, the control and removal of phosphorus in the water body become a key link for controlling the eutrophication of the water body.
The water eutrophication treatment measures mainly comprise two aspects of exogenous pollution control and endogenous pollution control. The adsorption method has been widely studied as a method for efficiently removing phosphorus from a water body. Commonly used phosphorus removal materials include clay minerals, zeolites, industrial residues, biochar, and the like. However, the conventional adsorbent has the following disadvantages: although the natural material has excellent adsorption performance, the natural material has higher cost and difficult regeneration; the industrial and agricultural waste residue has poor adsorption effect despite of easily available raw materials and low price. Therefore, the artificial synthesis of new adsorbents with economic and effective effects is receiving close attention from researchers in all countries around the world.
Since the rare earth element lanthanum has the advantages of strong phosphorus fixing capacity, wide pH application range, lower price than other rare earth elements and the like, the lanthanum modified phosphorus removal adsorbent becomes a hotspot and a heavy burden of research in the fieldAnd (4) point. Various lanthanum-modified adsorbents have appeared, such as lanthanum-modified bentonite
Figure RE-BDA0001152460730000011
Lanthanum modified vermiculite, lanthanum modified MCM-41, lanthanum aluminum modified montmorillonite, lanthanum aluminum modified zeolite and the like, and is used for research on removal of phosphorus in eutrophic water. Wherein
Figure RE-BDA0001152460730000012
Has been popularized and applied in large area in eutrophic water bodies in Europe, America, New Zealand, Australia and the like. Although it is not limited to
Figure RE-BDA0001152460730000013
The phosphorus-rich water plays a certain part in foreign markets, but the popularization and the application of the phosphorus-rich water in eutrophic water in China are limited due to higher market price and relatively lower phosphorus adsorption amount in China. However, other reported lanthanum-modified phosphorus removal adsorbents are only limited to the indoor experimental stage and are not put into use in the domestic market. At present, the lanthanum modified adsorbent capable of effectively treating the eutrophication water body for a long time does not appear in domestic markets, and the development of the relative treatment work of the eutrophication water body in China is greatly hindered.
Disclosure of the invention
The purpose of the invention is: the efficient phosphorus removal adsorbent is prepared by selecting a phosphorus removal raw material with low price and wide application and producing the raw material by a coprecipitation method. The phosphorus removal adsorbent is low in production cost, simple in production process, high in phosphorus removal efficiency and low in ecological safety risk, can efficiently remove different types of phosphorus in a water body, and effectively slows down the eutrophication process of the water body.
The utility model provides an adsorbing material of phosphorus in high-efficient removal water which characterized in that: the composition comprises, by weight, 4-30% of lanthanum hydroxide, 65-95% of aluminum hydroxide and 1-5% of lanthanum aluminate, wherein the lanthanum oxide coordination number of a first coordination layer in a molecular structure is 6.0-8.0, and the powder product is a coordinated unsaturated structure and contains oxygen vacancies.
An adsorbing material for efficiently removing phosphorus in a water body is characterized by comprising the following preparation steps:
(1) dissolving a certain amount of lanthanum compound and aluminum compound according to the molar ratio of lanthanum to aluminum of 1: 5-40;
(2) adding a precipitator into the step (1), keeping the temperature of the system at 50-90 ℃, and continuously stirring;
(3) and stopping stirring when the pH value of the solution is 8-11, keeping the temperature of the system at 50-90 ℃, continuing heating for 2-10 hours, washing, freeze-drying or drying and grinding the solid precipitate to obtain a solid powder product, namely the phosphorus adsorbent.
The utility model provides an adsorbing material of phosphorus in high-efficient removal water which characterized in that: the lanthanum compound is one or two of lanthanum chloride or lanthanum nitrate.
The utility model provides an adsorbing material of phosphorus in high-efficient removal water which characterized in that: the aluminum compound is one or more of aluminum chloride, aluminum nitrate, aluminum sulfate or alum.
The utility model provides an adsorbing material of phosphorus in high-efficient removal water which characterized in that: the precipitator is one or more of sodium hydroxide, potassium hydroxide, ammonium hydroxide or urea.
The preferred technical scheme of the invention is as follows: based on the dry basis of the powdery product, the contents of the components are 18 percent of lanthanum hydroxide, 77 percent of aluminum hydroxide and 5 percent of lanthanum aluminate according to the weight ratio.
The invention has the following effects:
the invention adopts a simple preparation method to produce the phosphorus removal adsorbent with low price and good effect. The dephosphorizing adsorbent has a high removing effect on different phosphorus compounds in a water body through the actions of electrostatic attraction, ligand exchange and oxygen vacancies on the surface of the adsorbent. Wide pH application range, high ecological safety, convenient storage, transportation and use, lasting phosphorus fixing effect and obvious economic benefit.
(IV) description of the drawings
FIG. 1 is a scanning electron micrograph of an adsorbing material for efficiently removing phosphorus from a water body
FIG. 2 is an XRD diffraction pattern of an adsorption material for efficiently removing phosphorus in a water body
FIG. 3 is a schematic view of a method for efficiently removing water from a body of waterLa L of phosphorus-adsorbing materialIIIEdge EXAFS map
(V) detailed description of the preferred embodiments
Example 1:
weighing 4g of lanthanum chloride and 13g of aluminum chloride into a 1L conical flask (1); adding 200mL of deionized water, and stirring for 10min under the water bath condition of 60 ℃ to completely dissolve (2); 2mol of L are added-1The addition of (3) is stopped when the pH of the sodium hydroxide solution is 9; keeping the temperature of the system at 60 ℃ and continuing heating for 10 hours (4); washing the product 3 to 4 times with about 1L of deionized water, centrifuging to remove the supernatant, and freeze-drying (5); grinding to obtain the phosphorus removal adsorbent powder product (6). Wherein, the content of lanthanum hydroxide accounts for 18 percent of the dry basis weight of the product, and the content of aluminum hydroxide accounts for 77 percent of the dry basis weight of the product; lanthanum aluminate accounts for 5% of the dry basis weight of the product; the pH is applicable in the range of 4-10.
In the powder obtained: la content is 13%; the content of Al is 27%.
Example 2:
weighing 4g of lanthanum chloride and 20g of aluminum chloride into a 1L conical flask (1); the steps (2) to (6) in example 1 were repeated for the remaining preparation processes. Wherein, the content of lanthanum hydroxide accounts for 14 percent of the dry basis weight of the product, and the content of aluminum hydroxide accounts for 85 percent of the dry basis weight of the product; lanthanum aluminate accounts for 1% of the dry basis weight of the product; the pH is applicable in the range of 4-10.
In the powder obtained: the La content is 10 percent; the content of Al is 29%.
Example 3:
weighing 4g lanthanum chloride and 27g aluminum chloride into a 1L Erlenmeyer flask (1); the steps (2) to (6) in example 1 were repeated for the remaining preparation processes. Wherein, the content of lanthanum hydroxide accounts for 11 percent of the dry basis weight of the product, and the content of aluminum hydroxide accounts for 86 percent of the dry basis weight of the product; lanthanum aluminate accounts for 3% of the dry basis weight of the product; the pH is applicable in the range of 4-10.
In the powder obtained: the La content is 8 percent; the content of Al is 30%.
Example 4:
weighing 4g lanthanum chloride and 33g aluminum chloride into a 1L Erlenmeyer flask (1); the steps (2) to (6) in example 1 were repeated for the remaining preparation processes. Wherein, the content of lanthanum hydroxide accounts for 8 percent of the dry basis weight of the product, and the content of aluminum hydroxide accounts for 91 percent of the dry basis weight of the product; lanthanum aluminate accounts for 1% of the dry basis weight of the product; the pH is applicable in the range of 4-10.
In the powder obtained: la content is 6%; the content of Al is 31%.
Example 5:
weighing 4g of lanthanum chloride and 40g of aluminum chloride into a 1L conical flask (1); the steps (2) to (6) in example 1 were repeated for the remaining preparation processes. Wherein, the content of lanthanum hydroxide accounts for 7 percent of the dry basis weight of the product, and the content of aluminum hydroxide accounts for 92 percent of the dry basis weight of the product; lanthanum aluminate accounts for 1% of the dry basis weight of the product; the pH is applicable in the range of 4-10.
In the powder obtained: la content is 5%; the content of Al is 32%.
Application example 1:
preparing a series of P L with initial phosphorus concentrations of 10, 20, 30, 40, 50 and 60mg-140mL of potassium dihydrogen phosphate solution, and 0.04g of the phosphorus-removing adsorbent (solid concentration: 1.0g L) obtained in example 1 above were added to each of the potassium dihydrogen phosphate solutions-1). After shaking at 170rpm at 25 ℃ for 24 hours, the solution was filtered to determine the removal rate of phosphate from the solution.
The initial concentration of phosphorus is 10, 20, 30, 40, 50, 60mg PL-1The removal rates of the phosphorus removal adsorbent for phosphate were 97%, 98%, 96%, 98%, 95%, and 95%, respectively.
Application example 2:
preparing a series of P L with initial phosphorus concentrations of 10, 20, 30, 40, 50 and 60mg-140mL of the sodium pyrophosphate solution, and 0.04g of the phosphorus removal adsorbent (solid concentration: 1.0g L) obtained in example 1 above were added to each of the solutions-1). After shaking at 170rpm at 25 ℃ for 24 hours, the solution was filtered to determine the removal rate of pyrophosphate in the solution.
The initial concentration of phosphorus is 10, 20, 30, 40, 50, 60mg PL-1The removal rates of pyrophosphate by the phosphorus removal adsorbent were 100%, 92%, 69%, 55%, 43%, and 36%, respectively.
Application example 3:
preparing a series of P L with initial phosphorus concentrations of 10, 20, 30, 40, 50 and 60mg-140mL of the sodium phytate solution, and 0.04g of the phosphorus removal adsorbent (solid concentration of 1.0g L) in example 1 above was added-1). After shaking at 170rpm at 25 ℃ for 24h, the solution was filtered and assayedThe removal rate of the phytic acid.
The initial concentration of phosphorus is 10, 20, 30, 40, 50, 60mg PL-1The removal rates of the phosphorus removal adsorbent for phytic acid were 99%, 98%, 91% and 77%, respectively.
Application example 4:
preparing a series of P L with initial phosphorus concentrations of 10, 20, 30, 40, 50 and 60mg-140mL of potassium dihydrogen phosphate solution, and 0.04g of the phosphorus-removing adsorbent (solid concentration: 1.0g L) obtained in example 3 above were added thereto-1). After shaking at 170rpm at 25 ℃ for 24 hours, the solution was filtered to determine the removal rate of phosphate from the solution.
The initial concentration of phosphorus is 10, 20, 30, 40, 50, 60mg PL-1The removal rates of the phosphorus removal adsorbent for phosphate were 90%, 92%, 90%, and 91%, respectively.
Application example 5:
preparing a series of P L with initial phosphorus concentrations of 10, 20, 30, 40, 50 and 60mg-140mL of potassium dihydrogen phosphate solution, and 0.04g of the phosphorus-removing adsorbent (solid concentration: 1.0g L) obtained in example 5 above was added thereto-1). After shaking at 170rpm at 25 ℃ for 24 hours, the solution was filtered to determine the removal rate of phosphate from the solution.
The initial concentration of phosphorus is 10, 20, 30, 40, 50, 60mg PL-1The removal rates of phosphate by the phosphorus removal adsorbent were 92%, 90%, 89%, 86%, 81%, and 77%, respectively.

Claims (4)

1. The application of the phosphorus removal adsorption material for efficiently removing phosphorus in water is characterized in that: the preparation steps of the dephosphorization adsorption material are as follows:
(1) dissolving a certain amount of lanthanum compound and aluminum compound according to the molar ratio of lanthanum to aluminum of 1: 5-40;
(2) adding a precipitator into the step (1), keeping the temperature of the system at 50-90 ℃, and continuously stirring;
(3) stopping stirring when the pH value of the solution is 8-11, keeping the temperature of the system at 50-90 ℃, continuing heating for 2-10 hours, washing, freeze-drying or drying and grinding the solid precipitate to obtain a solid powder product, namely the phosphorus removal adsorption material; the phosphorus removal adsorption material comprises, by weight, 4-30% of lanthanum hydroxide, 65-95% of aluminum hydroxide and 1-5% of lanthanum aluminate, wherein the content of each component is calculated on a dry basis of a powdery product, the lanthanum oxygen coordination number of a first coordination layer in a molecular structure is 6.0-8.0, and the phosphorus removal adsorption material is a coordination unsaturated structure and contains oxygen vacancies.
2. The application of the dephosphorization adsorbent material in the high-efficiency removal of phosphorus in water according to claim 1, which is characterized in that: the lanthanum compound is one or two of lanthanum chloride or lanthanum nitrate.
3. The application of the dephosphorization adsorbent material in the high-efficiency removal of phosphorus in water according to claim 1, which is characterized in that: the aluminum compound is one or more of aluminum chloride, aluminum nitrate, aluminum sulfate or alum.
4. The application of the dephosphorization adsorbent material in the high-efficiency removal of phosphorus in water according to claim 1, which is characterized in that: the precipitator is one or more of sodium hydroxide, potassium hydroxide, ammonium hydroxide or urea.
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CN107010705A (en) * 2017-05-05 2017-08-04 中国科学院生态环境研究中心 A kind of preparation method of rare earth aluminium polychloride water treatment agent
CN110038511A (en) * 2018-01-17 2019-07-23 华中科技大学 A kind of preparation method and applications carrying lanthanum modified alta-mud dephosphorization material
CN112044393B (en) * 2019-06-06 2021-05-04 中南大学 Two-dimensional clay-based composite phosphorus removal agent and preparation method and application thereof
CN110759451A (en) * 2019-10-18 2020-02-07 东北石油大学 Rare earth cationic-composite aluminum organic heteropolymeric flocculant
CN113087028A (en) * 2021-02-25 2021-07-09 苏州威德姆生态科技有限公司 Endogenous phosphorus passivation material and method for repairing eutrophic water body by using same
CN113457618A (en) * 2021-07-27 2021-10-01 北京师范大学珠海校区 Lanthanum-doped ordered mesoporous molecular sieve for environmental remediation and preparation method and application thereof
CN114749163A (en) * 2022-04-18 2022-07-15 南京大学 Preparation method of Ce-Al dephosphorization material
CN114669270B (en) * 2022-04-19 2024-04-02 中南民族大学 Composite material for efficiently passivating sediment phosphorus and preparation method thereof

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US6764672B2 (en) * 2001-04-03 2004-07-20 Alcoa Inc. Thermally stable alumina particulates
US20100227758A1 (en) * 2005-05-12 2010-09-09 Basf Corporation Alumina-Based Perovskite Catalysts and Catalyst Supports
CN101912790A (en) * 2010-08-05 2010-12-15 威海佰德信新材料有限公司 Production method of high-temperature resistant and anti-sulfurization catalyst carrier material
CN102247804A (en) * 2011-05-20 2011-11-23 上海大学 Preparation method of active carbon fiber phosphorous removing agent carrying lanthanum hydroxide
CN102320680B (en) * 2011-06-14 2012-12-12 中国水产科学研究院淡水渔业研究中心 Method for preparing ion exchanger for removing available phosphorous in water body
CN105578875A (en) * 2013-07-26 2016-05-11 瑞芬特瑞兹公司 New hybrid biodegradable polymer for efficient nitrogen and phosphate reduction

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