CN100460058C - Modified natural and self-making floating carrier and mesopore molecular sieve denitrogen dephosphorus material, its preparation and application - Google Patents
Modified natural and self-making floating carrier and mesopore molecular sieve denitrogen dephosphorus material, its preparation and application Download PDFInfo
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Abstract
A modified floating denitrifying-dephosphorizing material for treating the water in river and lake or the sewage is proportionally prepared from La, Ce, Al and Ca ions, light aggregate with large specific surface area, powdered coal ash, surfactant, cement, etc through mixing, impregnating in water, filtering and calcining.
Description
Affiliated technical field
The present invention relates to denitrogenation dephosphorizing material, preparation and the application of rivers and lakes water or waste water.
Background technology
Total phosphorus concentration is higher than the water body that 0.2mg/L or total nitrogen concentration be higher than 0.2mg/L and promptly is regarded as eutrophication water.Body eutrophication causes algalbloom, water quality deterioration, lake degeneration.Over past ten years, China's eutrophication water proportion rises to about 75% from 5.0%, and the water body ratio of oligotrophication reduces to 0.33% by 3.2%.
In the lake eutrophication restriction factor, the control of phosphorus accounts for 67%, and the control of nitrogen accounts for 30%.Therefore, dephosphorization is the key factor that prevents body eutrophication.Studies show that, phosphorus in the waste water exists with orthophosphates, metaphosphate, organophosphor form, under acid condition and the effect of bacterium living beings enzyme, be converted into orthophosphates, orthophosphates is restricted by the ionization equilibrium of phosphoric acid, ionization in water body, generating the phosphorus-containing groups principal mode is hydrogen phosphate and dihydrogen phosphate.The absorption method dephosphorization is to utilize porous or show the method that phosphate anion in the solid matter adsorbed water of specific surface realizes removing sewage phosphorus greatly.Adopt the natural materials adsorption and dephosphorization to carry out extensive studies and experiment, but natural materials phosphorus adsorption capacity is not high, the cycle of operation is short, is not suitable for commercial Application.S.A.Wassay soaks research (the Adsorption of fluoride that silica gel adsorbs fluorine phosphorus arsenic with lanthanum chloride solution, phosphate and arsenate iron onlanthanum impregnated silica gel.Wat.Env.Res.1996,68 (3): 295-300); Patent of invention 99119721.7,1999 iron-rare earth element compound water treatment adsorbent and preparation method thereof, to being stock with the molysite, the phosphorus sorbing material that adds the rare earth element formation has carried out synthesizing formula, synthesis condition, absorption property evaluation and desorb and compound adsorbent research; The experimental study of aqua oxidation lanthanum adsorption and dephosphorization (flat environmental science the 24th volume of the yellow rosy clouds tension force of fourth civilization the 5th phase 110-113) is for the equilibrium adsorption capacity of aqua oxidation lanthanum in orthophosphates, aspects such as pH accommodation and active oxidation compare, and prove that the aqua oxidation lanthanum has remarkable advantages.Flowing water dephosphorization experiment is not carried out in this experiment, and phosphor-removing effect generally needs 2 hours (Niu Limin Deng Chun tinkling of pieces of jade Ning Ping Yunnan environmental sciences 2,004 23 (3): 51-53) and will obtain preferably in impounded body.In current waters such as river, river course, remove phosphorus nitrogen, need the efficient height, denitrification functions is arranged and can keep the denitrogenation dephosphorizing material of the floatability of efficient in a long time, but the material that satisfies these requirements does not still have report at present.
Summary of the invention
The purpose of this invention is to provide can float on current water and the impounded body, recyclable regeneration, with denitrogenation dephosphorizing material, preparation and the application process of lanthanum ion, cerium ion, aluminium ion, calcium ion modification natural weight aggregate or mesopore molecular sieve.
The present invention is made up of following components in part by weight, wherein:
(1) modified natural materials by lanthanum ion and/or cerium ion and inessential metallic aluminium ion or calcium ion be combined as 5～33%, surplus is that the Large ratio surface lightweight aggregate forms,
(2) self-control floating carrier material is combined as 3～20% by lanthanum ion and/or cerium ion and inessential metallic aluminium ion or calcium ion, the combination 50～85% of Large ratio surface lightweight aggregate, flyash 5～10%, surfactant 0.5～1%, cement 1～5%, surplus is that double-ash powder is formed
(3) the silicon-based mesoporous molecular sieve material by lanthanum ion and/or cerium ion and inessential metallic aluminium ion or calcium ion be combined as 10～50%, surplus is that silicon-based mesoporous molecular sieve is formed,
The Large ratio surface lightweight aggregate refers to one of volcano float stone, diatomite, expanded perlite, expanded vermiculite, haydite, self-igniting coal gangue or bentonite.
The Large ratio surface lightweight aggregate refers to the unformed material of Large ratio surface that nature exists, i.e. one of volcano float stone, diatomite, expanded perlite, expanded vermiculite, haydite, self-igniting coal gangue or bentonite.
Lanthanum ion in the above component, cerium ion are meant that oxidation state is lanthanum, cerium ion and the water-soluble trivalent iron compound thereof of trivalent in the rare earth element, as aqua oxidation lanthanum, hydration lanthanum chloride, lanthanum nitrate, cerous nitrate, hydrous ceria.
Metallic aluminium ion, calcium ion are water-soluble aluminum sulfate, the inorganic salts of calcium sulfate.
Surfactant is 16-alkyl-3-methyl ammonium bromide.
The denitrogenation dephosphorizing preparation methods of modified natural, self-control floating carrier or silicon-based mesoporous molecular sieve:
(1) in the component and the ratio of leading portion described (1), the combination of lanthanum ion and/or cerium ion and inessential metallic aluminium ion or calcium ion is mixed the back water retting with the Large ratio surface lightweight aggregate, evenly stirring the back soaked 2～4 hours, filtering moisture, place 90～230 ℃ to dry, obtain modified natural denitrogenation dephosphorizing material;
(2) in the component and the ratio of leading portion described (2), is that double-ash powder mixes the back water retting with the combination of lanthanum ion and/or cerium ion and inessential metallic aluminium ion or calcium ion with combination, flyash, surfactant, the surplus of cement, Large ratio surface lightweight aggregate, evenly stirring the back soaked 12～24 hours, filtering moisture, place 90～230 ℃ to dry, obtain self-control floating carrier denitrogenation dephosphorizing material;
(3) in the component and the ratio of leading portion described (3), with the mixed precipitation of the combination of lanthanum ion and/or cerium ion and inessential metallic aluminium ion or calcium ion and softex kw, tetraethoxysilance, NaOH, water by weight 1～8%:2～6%:10～25%:0.3～1.5%:50～85%, the calcining moulding obtains silicon-based mesoporous molecular sieve denitrogenation dephosphorizing material.
The application of the denitrogenation dephosphorizing material of modified natural, self-control floating carrier or silicon-based mesoporous molecular sieve:
(1) modified natural denitrogenation dephosphorizing material is positioned over nature flows or impounded body in denitrogenation dephosphorizing;
(2) will make that floating carrier denitrogenation dephosphorizing material is positioned over that nature flows by oneself or impounded body in denitrogenation dephosphorizing;
(3) the denitrogenation dephosphorizing material of silicon-based mesoporous molecular sieve is positioned over nature flows or impounded body in denitrogenation dephosphorizing.
The effect of denitrogenation dephosphorizing material of the present invention is as follows:
When being used for impounded body, in that to contain phosphorus concentration be 1mg/L, contain NH
4 +Drop into 0.20～0.23g denitrogenation dephosphorizing particle in the-N concentration 10mg/L water, soaked 3～24 hours, when reaction after 3 hours the clearance of phosphorus generally reach more than 85%, reached molecular balance concentration in about 12 hours.
When being used for current water, will to contain phosphorus concentration be 1mg/L, contain NH
4 +The solution 10L of-N concentration 10mg/L, with flow velocity 4.0～6.5mm/s, flow 21.4L/h, by the filtrate that the denitrogenation dephosphorizing particle constitutes, clearance can reach more than 50%.
Denitrogenation dephosphorizing material of the present invention has the following advantages:
1, have bigger serface and than high-adsorption-capacity, phosphate and ammonia radical ion in can adsorbed water, denitrogenation dephosphorizing efficient height, time are fast in flowing water especially;
2, some natural weight aggregate itself has suction-operated preferably as vermiculite to ammonia radical ion, can reach the effect of denitrogenation;
3, the natural weight aggregate feed distribution is wide, and price is low, and material source is extensive;
4, density is all little than water, can float on the water surface, can salvage after recovery prepares again, recycles;
5, owing to the phosphorous acid group precipitation that is attached in the material hole, and lanthanum, cerium plasma can not cause secondary pollution to water body.
The specific embodiment
One, the experiment of modified natural carrier in impounded body.
Embodiment 1: mountain float stone 29.03g gets fire, lanthanum chloride 4.267g, pure water 139.0ml mixing stir about 4 hours, place mixture 90 ℃ of baking ovens to dry again, after taking out the denitrogenation dephosphorizing particle, in concentration is to put into 0.45g by every 2L in the 1ppm solution containing phosphate, reacts that to record tp removal rate in 24 hours be 93.27%, NH
4 +-N clearance 55.90%.
Embodiment 2: mountain float stone 20.10g gets fire, lanthanum chloride, cerous nitrate be 1.5g and 1.41g respectively, pure water 95.0ml mixing stir about 5 hours, place mixture 200 ℃ of baking ovens to dry again, after taking out the denitrogenation dephosphorizing particle, in concentration is to put into 0.45g by every 2L in the 1ppm solution containing phosphate, reacts that to record tp removal rate in 24 hours be 94.25%, NH
4 +-N clearance 52.18%.
Embodiment 3: get expanded perlite 5.0g, cerous nitrate is 0.675g altogether, pure water 47.4ml mixing stir about 4 hours, place mixture 90 ℃ of baking ovens to dry again, after taking out the denitrogenation dephosphorizing particle, in concentration is to put into 0.45g by every 2L in the 1ppm solution containing phosphate, reacts that to record tp removal rate in 24 hours be 91.05%.React and recorded NH in 12 hours
4 +-N clearance is 48.02%.
Embodiment 4: get expanded perlite 10.0g, lanthanum chloride 1.4g, pure water 95.0ml mixing stir about 4.5 hours, place mixture 180 ℃ of baking ovens to dry again, after taking out the denitrogenation dephosphorizing particle, in concentration is to put into 0.45g by every 2L in the 1ppm solution containing phosphate, reacts that to record tp removal rate in 24 hours be 92.36%.React and recorded NH in 12 hours
4 +-N clearance is 47.35%.
Embodiment 5: get expanded perlite 15.0g, lanthanum chloride 1.6g, cerous nitrate be 1.6g altogether, pure water 136.0ml mixes stirring 4.5 hours, place mixture 230 ℃ of baking ovens to dry again, after taking out the denitrogenation dephosphorizing particle, in concentration is to put into 0.45g by every 2L in the 1ppm solution containing phosphate, reacts that to record tp removal rate in 24 hours be 91.65%.React and recorded NH in 12 hours
4 +-N clearance is 52.01%.
Embodiment 6: get expanded vermiculite 10.0g, lanthanum chloride 1.0g, aluminum sulfate 0.4g, pure water 95.0ml mixing stir about 4.5 hours, place mixture 150 ℃ of baking ovens to dry again, after taking out the denitrogenation dephosphorizing particle, in concentration is to put into 0.45g by every 2L in the 1ppm solution containing phosphate, reacts that to record tp removal rate in 24 hours be 99.61%.React and recorded NH in 12 hours
4 +-N clearance is 54.2%.
Embodiment 7: get expanded vermiculite 15.0g, lanthanum chloride 1.0g, cerous nitrate 0.8g and calcium sulfate 0.2g, pure water 145.0ml mixing stir about 4.5 hours, place mixture 190 ℃ of baking ovens to dry again, after taking out the denitrogenation dephosphorizing particle, in concentration is to put into 0.45g by every 2L in the 1ppm solution containing phosphate, reacts that to record tp removal rate in 24 hours be 99.52%.React and recorded NH in 12 hours
4 +-N clearance is 49.6%.
Embodiment 8: get expanded vermiculite 5.0g, and lanthanum chloride 0.3g, cerous nitrate 0.38g, pure water 48.0ml mixing stir about 4.5 hours places mixture 230 ℃ of baking ovens to dry again, behind the taking-up denitrogenation dephosphorizing particle.At NH
4 +-N concentration is to put into 0.45g float type denitrogenation dephosphorizing particle by every 2L in the 10mg/L water, reacts that to record tp removal rate in 24 hours be 99.21%.React and recorded NH in 12 hours
4 +-N clearance is 51.3%.
Embodiment 9: get diatomite 10.12g, lanthanum chloride 1.47g, pure water 47.9ml mixing stir about 5 hours, place mixture 180 ℃ of baking ovens to dry again, after taking out the denitrogenation dephosphorizing particle, in concentration is to put into 0.45g by every 2L in the 1ppm solution containing phosphate, reacts that to record tp removal rate in 24 hours be 89.1%.Record NH
4 +-N clearance is 49.9%.
Embodiment 10: get diatomite 20.0g, lanthanum chloride, each 2.45g of cerous nitrate, pure water 100.0ml mixing stir about 4 hours, place mixture 200 ℃ of baking ovens to dry again, after taking out the denitrogenation dephosphorizing particle, in concentration is to put into 0.45g by every 2L in the 1ppm solution containing phosphate, reacts that to record tp removal rate in 24 hours be 85.6%.Record NH
4 +-N clearance is 46.5%.
Embodiment 11: get haydite 20.88g, lanthanum chloride 2.7g, pure water 100.0ml mixing stir about 5 hours, place mixture 230 ℃ of baking ovens to dry again, after taking out the denitrogenation dephosphorizing particle, in concentration is to put into 0.45g by every 200ml in the 1ppm solution containing phosphate, reacts that to record tp removal rate in 24 hours be 99.21%.Record NH
4 +-N clearance is 54.4%.
Embodiment 12: get haydite 15.0g, lanthanum chloride 1.0g, cerous nitrate 1.1g, pure water 80.0ml mixing stir about 4.5 hours, place mixture 180 ℃ of baking ovens to dry again, after taking out the denitrogenation dephosphorizing particle, in concentration is to put into 0.45g by every 200ml in the 1ppm solution containing phosphate, reacts that to record tp removal rate in 24 hours be 93.68%.Record NH
4 +-N clearance is 51.6%.
Embodiment 13: get haydite 10.0g, lanthanum chloride 0.77g, aluminum sulfate 0.7g, pure water 49.0ml mixing stir about 4 hours, place mixture 200 ℃ of baking ovens to dry again, after taking out the denitrogenation dephosphorizing particle, in concentration is to put into 0.45g by every 200ml in the 1ppm solution containing phosphate, reacts that to record tp removal rate in 24 hours be 97.61%.Record NH
4 +-N clearance is 56.6%.
Two, the experiment of modification worked materials in impounded body.
Embodiment 14: lanthanum chloride 2g, expanded perlite 4g, diatomite 4g, bentonite 6.5g, flyash 1.5g, surfactant 0.6g, double-ash powder 1g, about altogether 20.0g, mix back cement and water retting, evenly stirring the back soaked 24 hours, filtering moisture places 90 ℃ to dry, and makes diameter 0.8-1.5cm particle.Taking out 5g and carry out denitrogenation dephosphorizing, is to put into 0.45g by every 200ml in the 1ppm solution containing phosphate in concentration, reacts that to record tp removal rate in 24 hours be 100%.Record NH
4 +-N clearance is 54.21%.
Embodiment 15: get lanthanum chloride 1.0g, aluminum sulfate 0.4g, expanded perlite 2g, diatomite 2g, bentonite 3g, flyash 0.6g, surfactant 0.5g, double-ash powder 0.5g, be total to 10.0g, mix back cement and water retting, evenly stirring the back soaked 12 hours, filtering moisture places 180 ℃ to dry, and makes diameter 0.8-1.5cm particle.Taking out the denitrogenation dephosphorizing particle, is to put into 0.45g by every 200ml in the 1ppm solution containing phosphate in concentration, reacts that to record tp removal rate in 24 hours be 99.70%.Record NH
4 +-N clearance is 49.69%.
Embodiment 16: lanthanum chloride and cerous nitrate be 2g altogether, expanded perlite 4g, diatomite 4g, bentonite 6.5g, flyash 1.5g, surfactant 0.6g, double-ash powder 1g, about altogether 20.0g, mix back cement and water retting, evenly stirring the back soaked 16 hours, filtering moisture places 220 ℃ to dry, and makes diameter 0.8-1.5cm particle.Taking out 15g and carry out denitrogenation dephosphorizing, is to put into 0.45g by every 200ml in the 1ppm solution containing phosphate in concentration, reacts that to record tp removal rate in 24 hours be 96.56%.Record NH
4 +-N clearance is 51.23%.
Three, the experiment of modification meso-porous molecular sieve material in impounded body.
Embodiment 17: lanthanum chloride 0.06g, aluminum sulfate .0.04g, softex kw 0.08g, tetraethoxysilance 0.5g, NaOH 0.015g, add altogether 2g mixed precipitation of water, the calcining moulding is as modified mesoporous material.
Get 0.1g, 0.2g, 0.3g, 0.4g respectively, the 0.5g modified mesoporous material is in the sewage of 1mg/L in the 2L phosphorus content, stirs 10 minutes, and is static, surveys phosphorus content, phosphorus content and clearance result such as table 1 every sampling in 1 hour:
Table 1 different quality modified mesoporous material dephosphorization data
Embodiment 18: get 0.3g adding 2L phosphorus content and be respectively in the sewage of 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L in the modified mesoporous material of embodiment 17 preparations, stirred 10 minutes, static, survey phosphorus content, phosphorus content and clearance result such as table 2 every sampling in 1 hour:
Table 2. modified mesoporous material is to different phosphate content sewage dephosphorization data
Four, the experiment in current water.
Embodiment 19: take by weighing haydite 10g, lanthanum chloride, cerous nitrate be 1.4g altogether, water 100ml, stir 4h at a slow speed after, drainage, place dry in 190 ℃ of baking ovens stand-by.
Experimental facilities and method: with long 33cm, diameter is the vertical cylindrical glass tube of 4cm, and the porcelain granule light weight aggregate float type denitrogenation dephosphorizing particle 9g of interior dress is 4.5mm/s by flow velocity, flow be 21.4L/h feed concentration be 1mg/L contain P solution, the total feeding contains P solution 20L.Result such as following table 3:
Table 3. current water haydite denitrogenation dephosphorization data
Embodiment 20: self-control float type carrier material 30.0g, and lanthanum chloride, cerous nitrate be 6g altogether, and pure water 120.0ml mixing stir about 5 hours places baking oven to dry the back and takes out, and handles the water sample 200kg that fetches from Kunming Daqinghe River (inflow Dian Chi).
Experimental facilities and method: with the tank simulation river of long 4m, wide 15cm, high 4cm, placing 3g float type carrier denitrogenation dephosphorizing particle every 1m, is that 4.5mm/s experimentizes by flow velocity, is carrying out sampling and measuring except that the mouth of a river at regular intervals.The results are shown in Table 4:
Table 4. current water float type denitrogenation dephosphorization particle data
Claims (3)
1. the denitrogenation dephosphorizing material of modified natural, self-control floating carrier or silicon-based mesoporous molecular sieve is characterized in that being made up of following components in part by weight, wherein:
(1) modified natural materials by lanthanum ion and/or cerium ion and inessential metallic aluminium ion or calcium ion be combined as 5～33%, surplus is that the Large ratio surface lightweight aggregate forms,
(2) self-control floating carrier material is combined as 3～20% by lanthanum ion and/or cerium ion and inessential metallic aluminium ion or calcium ion, the combination 50～85% of Large ratio surface lightweight aggregate, flyash 5～10%, surfactant 0.5～1%, cement 1～5%, surplus is that double-ash powder is formed
(3) the silicon-based mesoporous molecular sieve material by lanthanum ion and/or cerium ion and inessential metallic aluminium ion or calcium ion be combined as 10～50%, surplus is that silicon-based mesoporous molecular sieve is formed,
The Large ratio surface lightweight aggregate refers to one of volcano float stone, diatomite, expanded perlite, expanded vermiculite, haydite, self-igniting coal gangue or bentonite.
2. the denitrogenation dephosphorizing preparation methods of modified natural, self-control floating carrier or silicon-based mesoporous molecular sieve is characterized in that:
(1) in the component and the ratio of claim 1 described (1), the combination of lanthanum ion and/or cerium ion and inessential metallic aluminium ion or calcium ion is mixed the back water retting with the Large ratio surface lightweight aggregate, evenly stirring the back soaked 2～4 hours, filtering moisture, place 90～230 ℃ to dry, obtain modified natural denitrogenation dephosphorizing material;
(2) in the component and the ratio of claim 1 described (2), is that double-ash powder mixes the back water retting with the combination of lanthanum ion and/or cerium ion and inessential metallic aluminium ion or calcium ion with combination, flyash, surfactant, the surplus of cement, Large ratio surface lightweight aggregate, evenly stirring the back soaked 12～24 hours, filtering moisture, place 90～230 ℃ to dry, obtain self-control floating carrier denitrogenation dephosphorizing material;
(3) in the component and the ratio of claim 1 described (3), with the mixed precipitation of the combination of lanthanum ion and/or cerium ion and inessential metallic aluminium ion or calcium ion and softex kw, tetraethoxysilance, NaOH, water by weight 1～8%:2～6%:10～25%:0.3～1.5%:50～85%, the calcining moulding obtains silicon-based mesoporous molecular sieve denitrogenation dephosphorizing material.
3. the application of the denitrogenation dephosphorizing material of modified natural, self-control floating carrier or silicon-based mesoporous molecular sieve is characterized in that:
(1) the modified natural denitrogenation dephosphorizing material that claim 2 described (1) is obtained be positioned over that nature flows or impounded body in denitrogenation dephosphorizing;
(2) the self-control floating carrier denitrogenation dephosphorizing material that claim 2 described (2) is obtained be positioned over that nature flows or impounded body in denitrogenation dephosphorizing;
(3) the denitrogenation dephosphorizing material of the silicon-based mesoporous molecular sieve that claim 2 described (3) is obtained be positioned over that nature flows or impounded body in denitrogenation dephosphorizing.
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