CN102600817A - Preparation method of active carbon fiber phosphorous removal agent loaded with ferric oxide hydrate - Google Patents

Preparation method of active carbon fiber phosphorous removal agent loaded with ferric oxide hydrate Download PDF

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CN102600817A
CN102600817A CN2012100808372A CN201210080837A CN102600817A CN 102600817 A CN102600817 A CN 102600817A CN 2012100808372 A CN2012100808372 A CN 2012100808372A CN 201210080837 A CN201210080837 A CN 201210080837A CN 102600817 A CN102600817 A CN 102600817A
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preparation
nacf
dephosphorization
ferric oxide
solution
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CN102600817B (en
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张玲
刘建勇
周奇
万里华
刘凡清
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Abstract

The invention relates to a preparation method of an active carbon fiber phosphorous removal agent loaded with ferric oxide hydrate, belonging to the technical field of preparation process of phosphorous adsorption removal agents. The preparation method in the invention has the characteristics of being short in preparation time, simple in steps, simple and practicable in operation and the like; and the obtained composite adsorbent has the advantages of being uniform in fiber surface load, large in load capability, excellent in adsorption performance, low in preparation cost and the like.

Description

The preparation method of the NACF dephosphorization agent of load hydrated ferric oxide
Technical field
The present invention relates to a kind of preparation method of composite dephosphorizing agent, belong to adsorption and dephosphorization agent fabricating technology field.The collosol and gel impregnation preparation method of the NACF dephosphorization agent of the hydrated ferric oxide that is a kind of load.
Background technology
Current, water pollution problems is all over the world, and particularly near city and the industrial area, water pollution is particularly serious, even developed country also still fails to solve fully water pollution problems, it is shortage of water resources that the world faces another problem.To a certain extent, restricted the development of regional economy.Along with the develop rapidly of industry and improving constantly of urbanization of villages level, water supply gets and sewage purification will become China and even one of the main difficult problem that faces all over the world.Along with the day by day increase of the mankind to environmental resource development and use activity, nitrogenous in a large number, the sanitary sewage of phosphorus nutrition material, industrial wastewater are entered in the rivers and lakes, increased the load of water nutrition material, its direct result is the eutrophication that causes water body.For landlocked water body, phosphorus is the key constraints that makes body eutrophication.Therefore effectively the content that reduces phosphorus in the discharge water has become the important channel of control body eutrophication, pollution control of water, and that researches and develops novel dephosphorization agent becomes the very urgent task in environmental protection field.
Waste water dephosphorization method commonly used both at home and abroad at present mainly comprises chemical method dephosphorization, bioanalysis dephosphorization and absorption method dephosphorization.
Though the chemical dephosphorization method is very high to the clearance of phosphorus, operating cost is high; The metal remained ion not only makes effluent color dilution increase, and produces the mud that is difficult in a large number to handle, causes secondary pollution easily, and possibly also can produce chronic toxic action to biology; Bioanalysis dephosphorization treatment effect is difficult for stable; Processing procedure receives extraneous factors such as temperature, dissolved oxygen, pH value to influence bigger; " the town sewage processing pollutant emission standard " that the water outlet total phosphorus is difficult to reach country's promulgation (GB18918-2002) one-level B discharge standard (TP≤1mg/L) more need not carry one-level A discharge standard (TP≤0.5mg/L).
Comparatively speaking, absorption method has advantages such as technology is simple, treatment effect good, easy to operate and reliable, has remedied the deficiency of additive method to a certain extent.The absorption method dephosphorization is to carry out dephosphorization through a kind of affine absorption of carrying out between adsorption site on the adsorbent and the phosphate anion in the sewage.This method is compared with the chemical dephosphorization method, has the dephosphorization economical and efficient, and is recyclable, and the characteristics of non-secondary pollution are compared with the biological phosphate-eliminating method, adsorb more stable, easy to operate.
The key of absorption method dephosphorization is to seek a kind of appropriate adsorbent that is suitable for, and requires the absorption property of adsorbent outstanding, can regenerate, stable performance, and mechanical strength is high, and material is easy to get cheap.
The molysite material is easy to get, low price, and main application in the early time generally concentrates on the chemical dephosphorization, and consumption is big, and causes secondary pollution.The iron adsorbent absorption property is better, has adsorption and dephosphorization effect preferably, but because iron oxide generally is pulverous, is difficult in practical application, reclaim, and has only to load to it mechanical strength is higher, could realize column operation on the carrier that be prone to be shaped.
NACF is a kind of novel adsorption functional material, have unique pore structure, micropore prosperity, wide material sources, cheap, specific area big, the characterization of adsorption such as easy of regenerating.But NACF is low to the affinity interaction power of phosphorus in the environmental wastewater, adsorption site is few, clearance is not high, only uses NACF to handle waste water and is difficult to reach mark.
Through suitable preparation means hydrated ferric oxide is loaded to that to prepare novel adsorption and dephosphorization agent on the NACF matrix be a desirable way.
Summary of the invention
The present invention seeks to hydrated ferric oxide is loaded to the novel adsorption and dephosphorization agent for preparing a kind of not only economy on the NACF matrix but also good absorption property is arranged.
Two of the object of the invention is to provide a kind of new and effective preparation method of this adsorbent.
The present invention has adopted collosol and gel-infusion process, it is characterized in that having following preparation process and step:
A. dispose the iron nitrate solution that the 10mL molar concentration is 0.125~1.5 mol/L;
B. heat 40mL deionized water to 100 ℃, progressively splash into the iron nitrate solution in the above-mentioned a step, till solution becomes brown.Remove beaker, stop heating, obtain ferric hydroxide colloid solution after the cooling.
Its reaction equation is: Fe (NO 3) 3+ 3H 2O → Fe (OH) 3(colloid)+3HNO 3
C. NACF is cut into 0.4~0.6 cm square piece, after water washing for several times, dipping, filtration, drying in deionized water;
D. the NACF with step c gained takes by weighing 0.5 g, adds in the resulting sol solutions of step b, leaves standstill dipping;
E. with the solid drying of steps d gained, 105 ° of C of baking temperature, dry fully after, the room temperature that reaches to be cooled promptly gets dephosphorization adsorbent.
Adopted collosol and gel-infusion process among the present invention, compared with prior art, it is simple to have operating procedure, and method of operating is easy, effectively shortens preparation time, and resulting dephosphorization agent has advantages such as low-cost high absorption property.
The specific embodiment
Embodiment one:
The concrete steps of present embodiment are:
1. dispose the 0.125mol/L iron nitrate solution of 10mL;
2. heating 40mL deionized water to 100 ℃ progressively splashes into the iron nitrate solution among a, till solution becomes brown.Remove beaker, stop heating, obtain the ferric hydroxide colloid solution of 0.025mol/L after the cooling.
Reaction equation: Fe (NO 3) 3+ 3H 2O → Fe (OH) 3(colloid)+3HNO 3
3. NACF is cut into 0.4~0.6cm square piece, after water washing for several times, dipping, filtration, drying in deionized water;
4. the NACF with step c gained takes by weighing 0.5 g, adds in the resulting sol solutions of step b, leaves standstill dipping;
5. with the solid drying of steps d gained, 105 ° of C of baking temperature, dry fully after, the room temperature that reaches to be cooled promptly gets dephosphorization adsorbent.
Embodiment two:
The concrete steps of present embodiment are:
1. dispose the 0.25mol/L iron nitrate solution of 10mL;
2. heating 40mL deionized water to 100 ℃ progressively splashes into the iron nitrate solution among a, till solution becomes brown.Remove beaker, stop heating, obtain the ferric hydroxide colloid solution of 0.05mol/L after the cooling.
Reaction equation: Fe (NO 3) 3+ 3H 2O → Fe (OH) 3(colloid)+3HNO 3
3. NACF is cut into 0.4~0.6cm square piece, after water washing for several times, dipping, filtration, drying in deionized water;
4. the NACF with step c gained takes by weighing 0.5 g, adds in the resulting sol solutions of step b, leaves standstill dipping;
5. with the solid drying of steps d gained, 105 ° of C of baking temperature, dry fully after, the room temperature that reaches to be cooled promptly gets dephosphorization adsorbent.
Embodiment three:
The concrete steps of present embodiment are:
1. dispose the 0.5mol/L iron nitrate solution of 10mL;
2. heating 40mL deionized water to 100 ℃ progressively splashes into the iron nitrate solution among a, till solution becomes brown.Remove beaker, stop heating, obtain the ferric hydroxide colloid solution of 0.1mol/L after the cooling.
Reaction equation: Fe (NO 3) 3+ 3H 2O → Fe (OH) 3(colloid)+3HNO 3
3. NACF is cut into 0.4~0.6cm square piece, after water washing for several times, dipping, filtration, drying in deionized water;
4. the NACF with step c gained takes by weighing 0.5 g, adds in the resulting sol solutions of step b, leaves standstill dipping;
5. with the solid drying of steps d gained, 105 ° of C of baking temperature, dry fully after, the room temperature that reaches to be cooled promptly gets dephosphorization adsorbent.
Embodiment four:
The concrete steps of present embodiment are:
1. dispose the 1mol/L iron nitrate solution of 10mL;
2. heating 40mL deionized water to 100 ℃ progressively splashes into the iron nitrate solution among a, till solution becomes brown.Remove beaker, stop heating, obtain the ferric hydroxide colloid solution of 0.2mol/L after the cooling.
Reaction equation: Fe (NO 3) 3+ 3H 2O → Fe (OH) 3(colloid)+3HNO 3
3. NACF is cut into 0.4~0.6cm square piece, after water washing for several times, dipping, filtration, drying in deionized water;
4. the NACF with step c gained takes by weighing 0.5 g, adds in the resulting sol solutions of step b, leaves standstill dipping;
5. with the solid drying of steps d gained, 105 ° of C of baking temperature, dry fully after, the room temperature that reaches to be cooled promptly gets dephosphorization adsorbent.
Embodiment five:
The concrete steps of present embodiment are:
1. dispose the 1.5mol/L iron nitrate solution of 10mL;
2. heating 40mL deionized water to 100 ℃ progressively splashes into the iron nitrate solution among a, till solution becomes brown.Remove beaker, stop heating, obtain the ferric hydroxide colloid solution of 0.3mol/L after the cooling.
Reaction equation: Fe (NO 3) 3+ 3H 2O → Fe (OH) 3(colloid)+3HNO 3
3. NACF is cut into 0.4~0.6cm square piece, after water washing for several times, dipping, filtration, drying in deionized water;
4. the NACF with step c gained takes by weighing 0.5 g, adds in the resulting sol solutions of step b, leaves standstill dipping;
5. with the solid drying of steps d gained, 105 ° of C of baking temperature, dry fully after, the room temperature that reaches to be cooled promptly gets dephosphorization adsorbent.
Performance test methods: the adsorbent of getting mass M is put into conical flask, in this conical flask, adds concentration C then 0Be 10 mg P/L, measure the KH of volume V by adsorbent dosage 1.0g/L 2PO 4Solution adsorbs in constant temperature oscillator, and adsorption time is 24h, and adsorption temp is 20 ° of C, after absorption finishes, measures absorption back solution concentration C eMeasuring method GBT11893-1989, adsorbents adsorb capacity q (mg/g)=V* (C 0-C e)/M, the result sees table 1.
Table 1 new adsorbent phosphorus removal property
Adsorbent Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
Adsorption capacity (mg/g) 4.99 7.79 8.06 8.06 7.47
Can find out that from table 1 dephosphorization agent that hydrated ferric oxide of the present invention loads on the NACF matrix has good absorption property.

Claims (1)

1. the preparation method of the NACF dephosphorization agent of a load hydrated ferric oxide is characterized in that having following preparation process and step:
A. dispose the iron nitrate solution that the 10mL molar concentration is 0.125~1.5 mol/L;
B. heat 40mL deionized water to 100 ℃, progressively splash into the iron nitrate solution in the above-mentioned a step, till solution becomes brown;
Remove beaker, stop heating, obtain ferric hydroxide colloid solution after the cooling;
Its reaction equation is: Fe (NO 3) 3+ 3H 2O → Fe (OH) 3(colloid)+3HNO 3
C. NACF is cut into 0.4~0.6 cm square piece, after water washing for several times, dipping, filtration, drying in deionized water;
D. the NACF with step c gained takes by weighing 0.5 g, adds in the resulting sol solutions of step b, leaves standstill dipping;
E. with the solid drying of steps d gained, 105 ° of C of baking temperature, dry fully after, the room temperature that reaches to be cooled promptly gets dephosphorization adsorbent.
CN2012100808372A 2012-03-26 2012-03-26 Preparation method of active carbon fiber phosphorous removal agent loaded with ferric oxide hydrate Expired - Fee Related CN102600817B (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN103801261A (en) * 2013-11-14 2014-05-21 淮南矿业(集团)有限责任公司 Adsorbing material as well as preparation method and application thereof
CN103936206A (en) * 2014-05-14 2014-07-23 南京大学 Method for synchronously removing organic matter and phosphorus in sewage biochemical tail water
CN104230131A (en) * 2014-09-12 2014-12-24 哈尔滨工业大学深圳研究生院 Method for synchronously controlling release of nitrogen and phosphorus as well as smell-causing substances in polluted sediment
CN106238001A (en) * 2016-08-11 2016-12-21 四川大学 A kind of hydrated ferric oxide. modified nanometer cellulose and application thereof
CN106861605A (en) * 2017-03-31 2017-06-20 四川农业大学 Activated carbon supported nanometer Fe Al(Hydrogen)The preparation method and applications of oxide particle composites
CN116393112A (en) * 2023-03-10 2023-07-07 山东科技大学 Preparation method of iron-carbon particles and reinforced constructed wetland dephosphorization method based on iron-carbon particles

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CN101757892A (en) * 2010-01-02 2010-06-30 桂林理工大学 Preparation method of bagasse active carbon/ferric oxide
CN102247804A (en) * 2011-05-20 2011-11-23 上海大学 Preparation method of active carbon fiber phosphorous removing agent carrying lanthanum hydroxide

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CN101757892A (en) * 2010-01-02 2010-06-30 桂林理工大学 Preparation method of bagasse active carbon/ferric oxide
CN102247804A (en) * 2011-05-20 2011-11-23 上海大学 Preparation method of active carbon fiber phosphorous removing agent carrying lanthanum hydroxide

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103801261A (en) * 2013-11-14 2014-05-21 淮南矿业(集团)有限责任公司 Adsorbing material as well as preparation method and application thereof
CN103801261B (en) * 2013-11-14 2016-02-03 淮南矿业(集团)有限责任公司 Sorbing material and its preparation method and application
CN103936206A (en) * 2014-05-14 2014-07-23 南京大学 Method for synchronously removing organic matter and phosphorus in sewage biochemical tail water
CN103936206B (en) * 2014-05-14 2016-05-04 南京大学 A kind of method of organic matter and phosphorus in synchronous removal sewage biochemical tail water
CN104230131A (en) * 2014-09-12 2014-12-24 哈尔滨工业大学深圳研究生院 Method for synchronously controlling release of nitrogen and phosphorus as well as smell-causing substances in polluted sediment
CN106238001A (en) * 2016-08-11 2016-12-21 四川大学 A kind of hydrated ferric oxide. modified nanometer cellulose and application thereof
CN106238001B (en) * 2016-08-11 2019-12-10 四川大学 Ferric hydroxide modified nanocellulose and application thereof
CN106861605A (en) * 2017-03-31 2017-06-20 四川农业大学 Activated carbon supported nanometer Fe Al(Hydrogen)The preparation method and applications of oxide particle composites
CN116393112A (en) * 2023-03-10 2023-07-07 山东科技大学 Preparation method of iron-carbon particles and reinforced constructed wetland dephosphorization method based on iron-carbon particles

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