CN106000277B - A kind of preparation and its application method of converted in-situ type phosphorus salvage material - Google Patents
A kind of preparation and its application method of converted in-situ type phosphorus salvage material Download PDFInfo
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- CN106000277B CN106000277B CN201610364137.4A CN201610364137A CN106000277B CN 106000277 B CN106000277 B CN 106000277B CN 201610364137 A CN201610364137 A CN 201610364137A CN 106000277 B CN106000277 B CN 106000277B
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- phosphorus
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- magnesium
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- salvage material
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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
- B01J20/04—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
-
- 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
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
Abstract
The invention discloses the preparations and its application method of a kind of in-situ chemical transformant phosphorus salvage material; by under 25~35 DEG C of stirring conditions; prepared carbonate solution is added in the magnesium salt solution of gas shield with fixed speed, stirs 10~30min, 30 DEG C of 1~4h of ageing; isolate solid phase; the flower-shaped magnesium carbonate phosphorus recycling material of drying to obtain, this method is simple and easy, consumes energy low, time-consuming short; it is low in cost, it is environmentally protective.Gained phosphorus recycling material parses the magnesium phosphate that magnesium ion generates indissoluble in conjunction with the phosphate radical in solution based on in-situ chemical conversion, dephosphorization can be carried out at room temperature, have many advantages, such as the pH and use safe that adsorption rate is fast, adapts to most of natural water source, it is a kind of dephosphorization adsorbent with a relatively high cost performance, new means are provided for P pollution control, there is good development prospect.
Description
Technical field
The invention belongs to sewage treatment fields, and in particular to the preparation of a kind of converted in-situ type phosphorus salvage material and its in dirt
The application of phosphorus recycling field in water process.
Background technique
With the development and the improvement of people's living standards of social economy, more and more phosphorus-containing wastewaters, which are discharged into water body, to be caused
Water eutrophication is got worse.China lake and basin water eutrophication are constantly aggravated, and phosphorus is that water eutrophication is formed
One of principal element, it is crucial for preventing water eutrophication dephosphorization, it is therefore desirable to actively seek sewage dephosphorization technology.Water at present
The minimizing technology of phosphorus mainly has chemical precipitation method, bioanalysis, absorption method in body.Chemical precipitation method phosphor-removing effect is good, but cost compared with
Height is also easy to produce secondary pollution；Bioanalysis sludge output is big, fluctuation of service；Absorption method because its with highly selective, low energy consumption by
Concern.Currently used adsorbent is natural material and waste residue, activated alumina and its modifier and artificial synthesized adsorbent etc.
Three categories.Natural material and activated alumina are at high cost because its adsorption capacity is small, and the application such as generation secondary pollution is limited
System, present artificial synthesized adsorbent are increasingly taken seriously.Existing research shows to develop, selectivity strong to phosphorus adsorption capacity
Good, the efficient dephosphorization material with some strength and chemical stability, small flow resistance, and it is applied to the adsorption and dephosphorization of each sewage
In technology, the phosphorus in sewage is enriched with and is separated, is the important means for guaranteeing sewage dephosphorization effect.
Dalian University of Technology's period-luminosity red (several solid waste adsorption and dephosphorization performances of the red of period-luminosity and its Exploration of Mechanism [D]
Dalian University of Technology's master thesis, 2010.) processing of phosphorus-containing wastewater, phosphorus will be used for after oyster shell washing, drying, grinding
Removal rate is 98.3%.The adsorbent is raw material using waste, and raw material sources are wide, realize waste resource recovery；And preparation work
Skill is simple, and low energy consumption, but the temperature required during dephosphorization is 35 DEG C, and practical application needs to heat, and when reaching adsorption equilibrium
Between it is long, adsorption capacity is lower, and limitation is high.
CN1803274A relates to the use of powdered zeolite, aluminium oxide or the silica gel soil that granularity is 60~100, presses after washing and drying
Certain proportion is added in rare earth hydroxide solution, and filter cake is obtained by filtration, through 300 in 0.75~1h of stirring, 15~20h of dipping
Screening obtains dephosphorization adsorbent after~600 DEG C of 0.5~2h of roasting.The adsorbent can remove zwitterion simultaneously, and adsorption capacity is big,
To the adsorption capacity of phosphorus up to 22~25mg/g, adsorption effect is preferable, and adsorbent can parse regeneration；But preparation process is complicated,
Energy consumption is high, and the prices of raw materials are high, and rare earth element is easily enriched in food chain, there is harm to ecological safety and human health.
Summary of the invention
The object of the present invention is to provide the preparations and its application method of a kind of converted in-situ type phosphorus salvage material, existing to overcome
Having technology to prepare, dephosphorization material energy consumption height, complex process, time-consuming, at high cost, safety is poor and existing dephosphorization material dephosphorization
It needs to heat, adsorption capacity is small and the defect long up to adsorption equilibrium required time.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of in-situ chemical transformant phosphorus salvage material, including following specific steps:
(1) carbonate and magnesium salt solution for preparing same 0.5~1.0mol/L of concentration respectively, according to CO3 2-And Mg2+Molar ratio
Under 25~35 DEG C of stirring conditions, the magnesium salts of gas shield is added in prepared carbonate solution by the ratio of 1:1 with fixed speed
In solution；
(2) after above-mentioned solution being stirred to react 10~30min, 30 DEG C of 1~4h of ageing isolate solid phase, at 40~80 DEG C
Material is used in the recycling of drying to obtain phosphorus.
Preferably, in step (1), the carbonate is selected from Li2CO3、Na2CO3、K2CO3In any one, magnesium salts is selected from
MgSO4、MgCl2Or Mg (NO3)2In any one.
Preferably, in step (1), the gas is at least one of nitrogen, argon gas, hydrogen or helium.
Preferably, in step (1), speed control is added in 2.0~5.0mL/min in the carbonate.
Preferably, in step (1), the gas shield is carried out at 25~35 DEG C.
The present invention also provides a kind of users of in-situ chemical transformant phosphorus salvage material using above method preparation
Method, the application method parse the phosphoric acid root knot in magnesium ion and solution based on the in-situ chemical transformant phosphorus salvage material
Symphysis dephosphorization at the magnesium phosphate of indissoluble.
Preferably, the in-situ chemical transformant phosphorus salvage material Yu phosphorus-containing wastewater of the application method press solid-to-liquid ratio 1:
1000-1:5000 mixing, adjusts pH to 3~10, reaches adsorption equilibrium after shaking 2~5h.
The present invention achieve compared with prior art it is following the utility model has the advantages that
(1) converted in-situ type phosphorus salvage material preparation required temperature is low, and preparation is simple, time-consuming short, at low cost
It is honest and clean, it is environmentally protective, safety is good.
(2) by situ conversion process, i.e. magnesium carbonate parses magnesium ion and generates indissoluble in conjunction with the phosphate radical in solution
Magnesium phosphate removes the phosphorus in sewage, and dephosphorization can carry out at room temperature, and absorption is short the time required to reaching balance, and adsorption capacity is big,
It can achieve 58.63~153.27mg/g.
(3) converted in-situ type phosphorus salvage material also has the advantage for the pH that adsorption rate is fast, adapts to most of natural water source,
A kind of higher dephosphorization adsorbent of cost performance, can it is both economical it is reasonable solve the problems, such as phosphorus-containing wastewater, be P pollution control
New means are provided, there is good development prospect.
Detailed description of the invention
Fig. 1 is the SEM figure of 1 gained in-situ chemical transformant phosphorus salvage material phosphorus of embodiment absorption front and back.
Fig. 2 is the XRD diagram of 1 gained in-situ chemical transformant phosphorus salvage material phosphorus of embodiment absorption front and back.
Fig. 3 is the FTIR figure of 1 gained in-situ chemical transformant phosphorus salvage material phosphorus of embodiment absorption front and back.
Fig. 4 is in-situ chemical transformant phosphorus salvage material phosphorus adsorption curve obtained by embodiment 1.
Fig. 5 is change of the in-situ chemical transformant phosphorus salvage material tp removal rate obtained by embodiment 1 with phosphorus initial concentration
Change curve.
Specific embodiment
Embodiment 1
(1) preparation of in-situ chemical transformant phosphorus salvage material
1) proper amount of sodium carbonate and Magnesium dichloride hexahydrate are weighed respectively, is respectively made into the solution of 0.5mol/L, are protected in 35 DEG C of nitrogen
Shield is stirred continuously down, is slowly added drop-wise to sodium carbonate liquor in magnesium chloride solution with 3.0mL/min；2) continue to stir for 35 DEG C
10min, 30 DEG C of ageing 1h, solution after reaction is filtered and is washed for several times into filtrate without chloride ion, and dehydrated alcohol washed once,
Vacuum drying obtains adsorbent material at 40 DEG C.
(2) the dephosphorization experiment of in-situ chemical transformant phosphorus salvage material
Weighing the phosphorus salvage material that 50mg is prepared and being placed in 50mL containing phosphorus concentration is to make it in 0.5mg/L phosphorus-containing wastewater sufficiently
Mixing adjusts pH between 3~10, and concussion absorption 2h reaches adsorption equilibrium.With in molybdenum-antimony anti-spectrophotometric method measurement filtrate
Phosphorus concentration, phosphorus salvage material are 62.34mg/g to the adsorbance of phosphorus, and the tp removal rate in solution is 95.68%.By embodiment 1
In-situ chemical transformant phosphorus salvage material phosphorus absorption obtained front and back carries out test characterization, as a result such as Fig. 1~5.
Fig. 1 is the scanning electron microscope (SEM) photograph of in-situ chemical transformant phosphorus salvage material phosphorus absorption front and back.Fig. 1 a is material before Phosphate Sorption
The scanning electron microscope (SEM) photograph of material, Fig. 1 b are the scanning electron microscope (SEM) photograph of material after Phosphate Sorption.It as seen from the figure, is flower-shaped knot before material Phosphate Sorption
Structure, significant changes occur for its surface topography after Phosphate Sorption, become club shaped structure.
Fig. 2 is the X-ray powder diffraction figure of in-situ chemical transformant phosphorus salvage material phosphorus absorption front and back, as seen from the figure, material
All diffraction maximums are monoclinic phase MgCO before expecting Phosphate Sorption3·3H2The diffraction maximum (JCPDS card number: 20-0669) (see Fig. 2 a) of O,
Without other magnesium carbonate hydrates, product is more pure.All diffraction maximums are Mg after Phosphate Sorption3(PO4)2·22H2O
Diffraction maximum (JCPDS card number: 44-0775) (see Fig. 2 b), illustrate that magnesium ion and the phosphate radical in solution are anti-in adsorption process
It answers, generates magnesium phosphate precipitation.
Fig. 3 is the infrared spectrogram of in-situ chemical transformant phosphorus salvage material phosphorus absorption front and back.As seen from the figure, it is inhaled with material
It is compared before attached phosphorus, in 1100cm after material Phosphate Sorption-1Nearby there is the stretching vibration peak of phosphate radical, illustrates that magnesium carbonate is converted into
Magnesium phosphate, this is consistent with the result that X-ray powder diffraction figure obtains.
Fig. 4 is the curve of adsorption kinetics of in-situ chemical transformant phosphorus salvage material, as seen from the figure, absorption of the material to phosphorus
It can reach balance in 100 minutes.
Fig. 5 is change of the in-situ chemical transformant phosphorus salvage material tp removal rate obtained by embodiment 1 with phosphorus initial concentration
Change curve, as seen from the figure, when phosphorus initial concentration is less than 200mg/L, removal rate of the in-situ chemical transformant phosphorus salvage material to phosphorus
Greater than 93.5%, and phosphorus initial concentration be 20mg/L when, material reaches 99.85% to the removal rate of phosphorus unexpectedly.
Embodiment 2
(1) preparation of in-situ chemical transformant phosphorus salvage material
1) appropriate lithium carbonate and magnesium nitrate are weighed respectively, are respectively made into the solution of 1.0mol/L, it is continuous in 25 DEG C of nitrogen protections
Under stirring, Lithium carbonate solution is slowly added drop-wise in magnesium nitrate solution with 2.5mL/min；2) 30 DEG C continue stir 20min, 30 DEG C
It is aged 1.5h, solution after reaction is filtered and is washed for several times, dehydrated alcohol is dried in vacuo at 50 DEG C after washed once to be inhaled
Enclosure material.
(2) the dephosphorization experiment of in-situ chemical transformant phosphorus salvage material
Weighing the dephosphorization adsorbent that 50mg is prepared and being placed in 100mL containing phosphorus concentration is to fill it in 2.0mg/LL phosphorus-containing wastewater
Divide mixing, adjust pH between 3~10, concussion absorption 3h reaches adsorption equilibrium.With in molybdenum-antimony anti-spectrophotometric method measurement filtrate
Phosphorus concentration, in-situ chemical transformant phosphorus salvage material is 86.32mg/g to the adsorbance of phosphorus, is to the tp removal rate in solution
96.35%.
Embodiment 3
(1) preparation of in-situ chemical transformant phosphorus salvage material
1) appropriate potassium carbonate and magnesium sulfate are weighed respectively, are respectively made into the solution of 0.75mol/L, it is continuous in 32 DEG C of helium protections
Under stirring, solution of potassium carbonate is slowly added drop-wise in Adlerika with 5.0mL/min；2) 25 DEG C continue stir 30min, 30 DEG C
It is aged 2.5h, is filtered, water washing is distilled, absolute alcohol washs one time, and vacuum drying obtains adsorbent material at 80 DEG C.
(2) the dephosphorization experiment of in-situ chemical transformant phosphorus salvage material
Weighing the dephosphorization adsorbent that 50mg is prepared and being placed in 150mL containing phosphorus concentration is to fill it in 100mg/L phosphorus-containing wastewater
Divide mixing, adjust pH between 3~10, concussion absorption 3.5h reaches adsorption equilibrium.Filtrate is measured with molybdenum-antimony anti-spectrophotometric method
In phosphorus concentration, in-situ chemical transformant phosphorus salvage material is 153.27mg/g to the adsorbance of phosphorus, to the phosphorus ligands in solution
Rate is 98.90%.
Embodiment 4
(1) preparation of in-situ chemical transformant phosphorus salvage material
1) proper amount of sodium carbonate and magnesium nitrate are weighed respectively, are respectively made into the solution of 0.6mol/L, it is continuous in 30 DEG C of argon gas protections
Under stirring, sodium carbonate liquor is slowly added drop-wise in magnesium nitrate solution with 4.0mL/min；2) continue to stir 25min for 30 DEG C, it will be anti-
Solution is filtered and is washed for several times into filtrate without chloride ion after answering, and is washed one time with absolute alcohol, is dried in vacuo at 60 DEG C
Obtain adsorbent material.
(2) the dephosphorization experiment of in-situ chemical transformant phosphorus salvage material
Weighing the dephosphorization adsorbent that 50mg is prepared and being placed in 250mL containing phosphorus concentration is to make it in 50mg/L phosphorus-containing wastewater sufficiently
Mixing adjusts pH between 3~10, and concussion absorption 5h reaches adsorption equilibrium.With in molybdenum-antimony anti-spectrophotometric method measurement filtrate
Phosphorus concentration, in-situ chemical transformant phosphorus salvage material are 142.35mg/g to the adsorbance of phosphorus, are to the tp removal rate in solution
99.68%.
The preparation cost that the above various embodiments prepares phosphorus salvage material is low, simple process, time-consuming short, material phosphorus adsorbance
Greatly, adsorption rate is fast, adaptable, safety is good, is a kind of higher dephosphorization adsorbent of cost performance, before having development well
Scape.
It should be noted last that the above specific embodiment is only used to illustrate the technical scheme of the present invention and not to limit it,
Although being described the invention in detail referring to preferred embodiment, it should be understood by one skilled in the art that can be to this
The technical solution of invention is modified or replaced equivalently, without departing from the spirit and scope of the technical solution of the present invention, should all
It is included within the scope of the claims of the present invention.
Claims (2)
1. a kind of preparation method of in-situ chemical transformant phosphorus salvage material, it is characterised in that: the in-situ chemical transformant phosphorus
Salvage material is flower-like structure, becomes club shaped structure after Phosphate Sorption；
The preparation method includes following specific steps:
(1) carbonate and magnesium salt solution for preparing same 0.5~1.0mol/L of concentration respectively, according to CO3 2-And Mg2+Molar ratio 1:1's
Under 25~35 DEG C of stirring conditions, the magnesium salt solution of gas shield is added in prepared carbonate solution by ratio with fixed speed
In；(2) after above-mentioned solution being stirred to react 10~30min, 30 DEG C of ageing 1h isolate solid phase, and dehydrated alcohol washed once,
40~80 DEG C of drying to obtain phosphorus recycling materials, wherein the carbonate is sodium carbonate, and magnesium salts is Magnesium dichloride hexahydrate；Institute
Stating gas is nitrogen；The addition speed of the carbonate solution is 3.0mL/min；The gas shield is carried out at 25~35 DEG C.
2. the application method of the in-situ chemical transformant phosphorus salvage material prepared method according to claim 1, feature exist
In: the application method parses magnesium ion and the phosphoric acid root knot in solution based on the in-situ chemical transformant phosphorus salvage material
Symphysis dephosphorization at the magnesium phosphate of indissoluble；The in-situ chemical transformant phosphorus salvage material and phosphorus-containing wastewater press solid-to-liquid ratio 1:
1000-1:5000 mixing, adjusting pH value of solution is 3~10, reaches adsorption equilibrium after shaking 2~5h.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190320A (en) * | 2010-03-05 | 2011-09-21 | 中国科学院过程工程研究所 | Method for preparing trihydrated magnesium carbonate by using continuous crystallization process |
| CN104086019A (en) * | 2014-06-17 | 2014-10-08 | 湖北富邦科技股份有限公司 | Industrial high-concentration phosphorus-containing wastewater treatment method |
| CN104973628A (en) * | 2015-06-30 | 2015-10-14 | 崇义章源钨业股份有限公司 | Method used for purifying sodium tungstate solution |
| CN105036161A (en) * | 2015-07-23 | 2015-11-11 | 韦海棉 | Preparation method of magnesium carbonate crystal |
| CN105347368A (en) * | 2015-12-14 | 2016-02-24 | 苏州市泽镁新材料科技有限公司 | Preparing method of high purity magnesium carbonate |
-
2016
- 2016-05-23 CN CN201610364137.4A patent/CN106000277B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190320A (en) * | 2010-03-05 | 2011-09-21 | 中国科学院过程工程研究所 | Method for preparing trihydrated magnesium carbonate by using continuous crystallization process |
| CN104086019A (en) * | 2014-06-17 | 2014-10-08 | 湖北富邦科技股份有限公司 | Industrial high-concentration phosphorus-containing wastewater treatment method |
| CN104973628A (en) * | 2015-06-30 | 2015-10-14 | 崇义章源钨业股份有限公司 | Method used for purifying sodium tungstate solution |
| CN105036161A (en) * | 2015-07-23 | 2015-11-11 | 韦海棉 | Preparation method of magnesium carbonate crystal |
| CN105347368A (en) * | 2015-12-14 | 2016-02-24 | 苏州市泽镁新材料科技有限公司 | Preparing method of high purity magnesium carbonate |
Non-Patent Citations (1)
| Title |
|---|
| "Removal of Phosphate from Eutrophic Lakes through Adsorption by in Situ Formation of Magnesium Hydroxide from Diatomite";Fazhi Xie et al.;《Environmental Science & Technology》;20131216;第48卷;第582-590页 * |
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Effective date of registration: 20210220 Address after: 230000 5th floor, building 3, 1688 Xiyou Road, high tech Zone, Hefei City, Anhui Province Patentee after: Anhui Chengxiang analysis and Test Technology Co.,Ltd. Address before: 230601 Ziyun Road, Hefei economic and Technological Development Zone, Anhui 292 Patentee before: ANHUI JIANZHU University |