CN104607144B - A kind of structure is from growth aqueous phase Phosphateadsorption material and its preparation method and application - Google Patents

A kind of structure is from growth aqueous phase Phosphateadsorption material and its preparation method and application Download PDF

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CN104607144B
CN104607144B CN201510078012.0A CN201510078012A CN104607144B CN 104607144 B CN104607144 B CN 104607144B CN 201510078012 A CN201510078012 A CN 201510078012A CN 104607144 B CN104607144 B CN 104607144B
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egg shell
phosphateadsorption
aqueous phase
preparation
clay
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CN104607144A (en
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于岩
何亚军
张复伟
李�杰
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Fuzhou University
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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
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12—Naturally occurring clays or bleaching earth
    • 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
    • B01J20/04—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
    • B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
    • 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
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Engineering & Computer Science (AREA)
  • Hydrology & Water Resources (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The invention discloses a kind of structure from growth aqueous phase Phosphateadsorption material and its preparation method and application, clay is joined in pre-burned egg shell powder and carry out ball milling mixing, through granulation, old aftershaping, the most sintered, boiling and stoving process, obtain structure from growth aqueous phase Phosphateadsorption material.The present invention solves common adsorbents unavoidable absorption saturation problem from mechanism, achieve the new breakthrough of adsorption mechanism, and utilize diatomite, the waste resources such as the silicon powder of ferroalloy smelting factory generation and the oyster of the market of farm produce are raw material, have developed structure from growth aqueous phase Phosphateadsorption material, phosphate anion in absorption effluent effectively, while solving phosphorus-rich water pollution problem, the problem advantageously accounting for egg shell waste pollution, the preparation method of material is the most effective, low cost, easily promote, there is good economic benefit and environmental benefit, can be produced by scale of input metaplasia well, promote the sustainable development of social economy and environment.

Description

A kind of structure is from growth aqueous phase Phosphateadsorption material and its preparation method and application
Technical field
The invention belongs to environment and Material Field, be specifically related to a kind of structure from growth aqueous phase Phosphateadsorption material and Preparation method and application.
Background technology
The phosphorus-containing wastewater of discharge and the phosphorus-containing wastewater of discharge in industrial production in the daily production of the mankind, cause in a large number rich in The waste water of nitrogen phosphorus enters rivers,lakes and seas, causes body eutrophication, causes large-area red tide.And traditional adsorption method, nothing Opinion is physical absorption or chemisorbed, the most generally there is problem: have selectivity, and effect is single；There is suction Attached saturated problem；Adsorption capacity and the paradox of recyclable regeneration.The phosphorus removing method that research cost is low, efficiency is high is for improving Naural benefit and economic benefit are significantly.
China's annual output bird egg is up to ten thousand t more than 350, and a large amount of of egg shell discard, and not only cause environmental pollution, And be the waste of a kind of resource, and egg shell is a kind of calcic porous mass, has bigger specific surface area and good gas Mutually with liquid phase adsorption performance.Clay is the silicate powder that a kind of distributed pole is wide, and its main component is aqueous manosil AS salt mine Thing, has good plasticity.
Raw material based on egg shell, adulterate a certain amount of clay, after sintered-boiling, by the calcium carbonate in egg shell It is modified as stable performance, not cracky, the hydrate [Ca of the active calcium silicates good with continuation of dephosphorization5(Si6O18H2) 4H2O], bear short flat crystal and tiny pin column crystal in the sample, and be woven into spacial framework so that it is dephosphorization Effect is more preferable.The calcium ion advanced activation on its surface simultaneously, and after contacting with phosphate anion, at the Surface Creation of sample The new aquation phosphorus base calcium phosphate equally with three-dimensional porous structure, product continues on the framework inner edge absorption limit of former sorbing material Continuous build loose structure, it is achieved that sorbing material structure certainly grow optimization, make adsorbent be provided with persistently and inhale efficiently Attached ability.
Through retrieval, at home and abroad there is no with egg shell powder, clay as raw material, preparation structure is from growth aqueous phase Phosphateadsorption The method of material, this project belongs to the technology of first research invention both at home and abroad.Main raw material(s) clay involved in the present invention exists China's rich reserves, egg shell can reclaim in agricultural production and obtain, cheap, is well to prepare raw material, and it is used Preparation method simple, not only prepared new and effective while growth phosphate anion sorbing material, the most rationally Refuse reclamation has been accomplished on ground, provides one have for the problem and rich phosphatization water pollution problems solving egg shell waste pollution Imitate feasible method.
Summary of the invention
It is an object of the invention to provide a kind of structure from growth aqueous phase Phosphateadsorption material and preparation method thereof and to answer With, the structure prepared from growth aqueous phase Phosphateadsorption material can the effective phosphate anion in absorption effluent, also can portion The problem decomposing certainly egg shell waste pollution, it is achieved that the recycling of discarded object.Its preparation cost is low, method simple, easily Being used more widely, economic benefit and environmental benefit are good.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of structure is clay and egg shell from the primary raw material of growth aqueous phase Phosphateadsorption material.
The percetage by weight of primary raw material is: clay 35 ~ 50%, egg shell 50 ~ 65%, and both percetage by weight sums are 100%.Main chemical compositions SiO of clay2And Al2O3Content be 50 ~ 68 wt% and 16 ~ 20 wt%, mainization of egg shell Study a point CaCO3Content be 90 ~ 94 wt%.
Preparation method: clay is joined in pre-burned egg shell powder and carry out ball milling mixing, through granulation, old after become Type, more sintered, boiling and stoving process, obtain structure from growth aqueous phase Phosphateadsorption material.Specifically comprise the following steps that
(1) the egg shell powder after cleaning carries out pre-sintering, calcining heat 550 DEG C, and temperature retention time 1 h, ball milling sieves；
(2) egg shell powder and clay step (1) pre-processed carries out dry ball milling, crosses 60 mesh sieves after mixing, then Add deionized water and carry out granulation, after crossing 50 mesh sieves, carry out old process 24h；
(3) weigh 2 g old after pellet, under the pressure of 2 MPa, carry out compression molding, at 700 DEG C, calcine 2 h；
(4) again through hyperbaric heating boiling 3h, dry, i.e. obtain structure from growth aqueous phase Phosphateadsorption material.
Described material is used for Removal of Phosphorus in Wastewater, it is achieved the structure of sorbing material is from growing optimization.
The remarkable advantage of the present invention is:
(1) raw material and technological innovation: utilize clay and egg shell preparation from growth aqueous phase Phosphateadsorption material, it is achieved useless Thing recycles, and its preparation method is simple, the most expanded.Prepared sorbing material is while efficient absorption, it is possible to Produce new sorbing material, further increase adsorption efficiency.
(2) through retrieval, at home and abroad there is no the structure utilizing egg shell powder, clay to prepare from growth aqueous phase Phosphateadsorption The report of material, this project belongs to the technology of first research invention both at home and abroad.
(3) raw-material characteristic is made full use of: egg shell has abundant natural multistage cavernous structure, and itself i.e. possesses suction Attached ability.Clay has good plasticity, is that a kind of needing not move through pulverizes processing, cheap ultrafine powder.
(4) low production cost: the primary raw material egg shell of this method and clay, results from agricultural production and industrial production, Wide material sources, cheap, it is easy to obtaining, cost is the lowest.This method has good economic benefit.
(5) sorbing material with aluminium hydrosilicate calcium crystal as principal phase prepared, when for Removal of Phosphorus in Wastewater, waste water In phosphoric acid with can react with aluminium hydrosilicate calcium crystal, generate be similar to porous hydroxyapatite structure, this hydroxyapatite In minute hand column structure, can continue to build loose structure based on original absorption carrier, along with the carrying out of absorption, generate Amount of crystals be on the increase, form a kind of structure from growth aqueous phase Phosphateadsorption material.The present invention solves from mechanism Common adsorbents unavoidable absorption saturation problem, it is achieved that the new breakthrough of adsorption mechanism, and utilize diatomite, ferroalloy smelting The waste resources such as the silicon powder of refinery's generation and the oyster of the market of farm produce are raw material, have developed structure from growth aqueous phase phosphate radical Sorbing material, the effectively phosphate anion in absorption effluent, while solving phosphorus-rich water pollution problem, advantageously account for egg The problem of shell waste pollution, the preparation method of material is simply effective, and low cost is easily promoted, had good economic benefit And environmental benefit, it is possible to produced by scale of input metaplasia well, the sustainable development of social economy and environment can be promoted.
Accompanying drawing explanation
Fig. 1 is structure scanning electron microscope (SEM) photograph before growth sample adsorption.
Fig. 2 is structure scanning electron microscope (SEM) photograph after growth sample adsorption.
Detailed description of the invention
The weight proportion of composition of raw materials is: clay 35 ~ 50wt% egg shell 50 ~ 65wt%.
The structure utilizing clay and egg shell powder to prepare specifically walks from the preparation method of growth aqueous phase Phosphateadsorption material Suddenly it is:
(1) the egg shell powder after cleaning is put into high temperature box furnace and is carried out pre-sintering, and calcining heat 550 DEG C, during insulation Between: 1 h, ball milling sieves prepared egg shell powder.
(2) the egg shell powder pre-processed, clay are put into ball mill mixing, dry method ball in the ratio of recipe requirements Mill, crosses 60 mesh sieves after mixing, add appropriate deionized water and carry out granulation, after crossing 50 mesh sieves, and it is carried out the old of 24h Process.
(3) weigh 2g old after powder, under the pressure of 2MPa, carry out compression molding, be pressed into.By compressing sky Stem shape sample is placed in the batch-type furnace of 700 DEG C calcines 2 h.
(4) sample sintered is placed in hyperbaric heating processing equipment, boiling 3h.Sample is dried, i.e. obtains structure From growth aqueous phase Phosphateadsorption material, this sorbing material, when waste water dephosphorization, every other day measures a liquid waste concentration, with Time replace original waste liquid by new lead waste water, after circulate 60 times, dephosphorizing rate does not decline, Fig. 1 and Fig. 2 be respectively before absorption with The scanning electron microscope (SEM) photograph of sample after circulation absorption 60 times, as can be seen from Fig., before and after absorption, the microscopic appearance difference of sample is little, still So keep loose structure, illustrate that adsorbed product can continue to build loose structure on protocorm in adsorption process.
Embodiment 1
The weight proportion of composition of raw materials is: clay 50wt%, egg shell 50wt%.
Preparation method concretely comprises the following steps:
(1) the egg shell powder after cleaning is put into high temperature box furnace and is carried out pre-sintering, and calcining heat 550 DEG C, during insulation Between: 1 h, ball milling sieves prepared egg shell powder.
(2) the egg shell powder pre-processed, clay are put into ball mill mixing, dry method ball in the ratio of recipe requirements Mill, crosses 60 mesh sieves after mixing, add appropriate deionized water and carry out granulation, after crossing 50 mesh sieves, and it is carried out the old of 24h Process.
(3) weigh 2g old after powder, under the pressure of 2MPa, carry out compression molding, be pressed into.By compressing sky Stem shape sample is placed in the batch-type furnace of 700 DEG C calcines 2 h.
(4) sample sintered is placed in hyperbaric heating processing equipment, boiling 3h.Sample is dried, i.e. obtains structure From growth aqueous phase Phosphateadsorption material, this material is when the absorption of phosphorus, and after repeatedly adsorbing 60 times, dephosphorizing rate does not reduce, still Maintain initial dephosphorization efficiency.
This experiment mainly uses the phosphorus in phosphorus molybdenum antimony scandium water by Spectrophotometry, with the 80 initial phosphorus concentrations of mL as 5mg/L Simulated wastewater (KH2PO4The aqueous solution), add the material that 2g prepares, at room temperature stand 48h, take supernatant and be analyzed, The clearance calculating phosphorus is 94.68%.
Embodiment 2
The weight proportion of composition of raw materials is: clay 40wt%, egg shell 60wt%.
Preparation method concretely comprises the following steps:
(1) the egg shell powder after cleaning is put into high temperature box furnace and is carried out pre-sintering, and calcining heat 550 DEG C, during insulation Between: 1 h, ball milling sieves prepared egg shell powder.
(2) the egg shell powder pre-processed, clay are put into ball mill mixing, dry method ball in the ratio of recipe requirements Mill, crosses 60 mesh sieves after mixing, add appropriate deionized water and carry out granulation, after crossing 50 mesh sieves, and it is carried out the old of 24h Process.
(3) weigh 2g old after powder, under the pressure of 2MPa, carry out compression molding, be pressed into.By compressing sky Stem shape sample is placed in the batch-type furnace of 700 DEG C calcines 2 h.
(4) sample sintered is placed in hyperbaric heating processing equipment, boiling 3h.Sample is dried, i.e. obtains structure From growth aqueous phase Phosphateadsorption material.
After hydro-thermal, sample is dried, i.e. obtain structure from growth aqueous phase Phosphateadsorption material.
This experiment mainly uses the phosphorus in phosphorus molybdenum antimony scandium water by Spectrophotometry, with the 80 initial phosphorus concentrations of mL as 5mg/L Simulated wastewater (KH2PO4The aqueous solution), add the material that 2g prepares, at room temperature stand 48h, take supernatant and be analyzed, The clearance calculating phosphorus is 96.74%, and after sample Reusability 60 times, dephosphorizing rate does not reduce.
Embodiment 3
The weight proportion of composition of raw materials is: clay 35wt%, egg shell 65wt%.Preparation method concretely comprises the following steps:
(1) the egg shell powder after cleaning is put into high temperature box furnace and is carried out pre-sintering, and calcining heat 550 DEG C, during insulation Between: 1 h, ball milling sieves prepared egg shell powder.
(2) the egg shell powder pre-processed, clay are put into ball mill mixing, dry method ball in the ratio of recipe requirements Mill, crosses 60 mesh sieves after mixing, add appropriate deionized water and carry out granulation, after crossing 50 mesh sieves, and it is carried out the old of 24h Process.
(3) weigh 2g old after powder, under the pressure of 2MPa, carry out compression molding, be pressed into.By compressing sky Stem shape sample is placed in the batch-type furnace of 700 DEG C calcines 2 h.
(4) sample sintered is placed in hyperbaric heating processing equipment, boiling 3h.Sample is dried, i.e. obtains structure From growth aqueous phase Phosphateadsorption material.
This experiment mainly uses the phosphorus in phosphorus molybdenum antimony scandium water by Spectrophotometry, with the 80 initial phosphorus concentrations of mL as 5mg/L Simulated wastewater (KH2PO4The aqueous solution), add the material that 2g prepares, at room temperature stand 48h, take supernatant and be analyzed, The clearance calculating phosphorus is 98.65%, and sample recycles through 60 times, and dephosphorizing rate does not decline, and the microscopic appearance of sample is also Do not change.
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent with Modify, all should belong to the covering scope of the present invention.

Claims (1)

1. a structure is from the preparation method growing aqueous phase Phosphateadsorption material, it is characterised in that: described sorbing material former The weight proportion of material formula is: clay 35wt%, egg shell 65wt%, and preparation method concretely comprises the following steps:
(1) the egg shell powder after cleaning is put into high temperature box furnace and is carried out pre-sintering, calcining heat 550 DEG C, temperature retention time: 1 H, ball milling sieves prepared egg shell powder；
(2) the egg shell powder pre-processed, clay are put into ball mill mixing, dry ball milling in the ratio of recipe requirements, mix Cross 60 mesh sieves after even, add deionized water and carry out granulation, after crossing 50 mesh sieves, and it is carried out the old process of 24h；
(3) weigh 2 g old after powder, under the pressure of 2 MPa, carry out compression molding, be pressed into；By compressing hollow Column sample is placed in the batch-type furnace of 700 DEG C calcines 2 h；
(4) sample sintered is placed in hyperbaric heating processing equipment, boiling 3h；Sample is dried, i.e. obtains structure spontaneous Long aqueous phase Phosphateadsorption material.
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CN105126740B (en) * 2015-09-28 2018-06-15 福州大学 A kind of BIOLOGICAL CALCIUM type Phosphateadsorption porous material and preparation method thereof
CN105126760B (en) * 2015-09-28 2017-08-25 福州大学 Poly- hole sorbing material of one heavy metal species and preparation method thereof
CN107445216A (en) * 2016-06-01 2017-12-08 张会君 A kind of formula and preparation method for sewage disposal dephosphorization filler
CN110142032B (en) * 2019-06-11 2022-02-22 盐城工学院 Chitosan biochar composite material and preparation method and application thereof
CN112044395A (en) * 2020-07-13 2020-12-08 东莞理工学院 Phosphate adsorbent preparation system and method using excess sludge and biological shell wastes as raw materials
CN113244880A (en) * 2021-06-16 2021-08-13 南通大学 Sintered ceramsite capable of efficiently removing phosphorus, preparation method and regeneration method thereof
CN116726871A (en) * 2023-07-07 2023-09-12 上海尼普敦环境科技有限公司 Preparation method of dephosphorization material for water body treatment

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JP4827045B2 (en) * 2004-07-22 2011-11-30 長崎県 Water purification material and method for producing water purification material
CN102190343B (en) * 2010-03-03 2012-11-28 南京信息工程大学 Method for adsorbing phosphate in sewage by using eggshells
CN102380350B (en) * 2011-10-24 2013-06-05 上海海洋大学 Method for removing hydroxyapatite modified eggshell adsorbent material and recycling phosphate from wastewater
CN103288164B (en) * 2013-06-25 2015-07-01 南京信息工程大学 A method for synchronous nitrogen and phosphorus removal in sewage by combining modified zeolite and modified eggshell

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