CN104474787B - A kind of filtrate for sewage disposal and preparation method thereof - Google Patents
A kind of filtrate for sewage disposal and preparation method thereof Download PDFInfo
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- CN104474787B CN104474787B CN201410745608.7A CN201410745608A CN104474787B CN 104474787 B CN104474787 B CN 104474787B CN 201410745608 A CN201410745608 A CN 201410745608A CN 104474787 B CN104474787 B CN 104474787B
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Abstract
The present invention is a kind of filtrate for sewage disposal, by humic acid, clay and deer natural pond soil mixed sintering form, NaOH can also be added as conditioning agent during sintering, the present invention is native for primary raw material with deer natural pond, the synchronous strengthening that can realize suspension and phosphorus is removed, this filtrate has large and strong to the Adsorption ability of the P elements feature of specific area, to the synchronous removal important in inhibiting of suspension in sewage and P elements, preparation method of the present invention is simple to operation, show through operation test, prepared filtrate is while guarantee is to the turbidity removal effect in Sewage Plant secondary treatment yielding water, there is good total phosphorus removal capacity, effluent quality meets the A standard-required of China GB18918-2002 " urban wastewater treatment firm pollutant emission standard " primary standard.
Description
Technical field
The invention belongs to advanced treatment of wastewater technical field, particularly a kind of filtrate for sewage disposal and preparation method thereof.
Background technology
Along with becoming increasingly conspicuous and the development of reuse of wastewater technology of shortage of water resources problem, the application of filtering in advanced treatment of wastewater and reuse is also increasingly extensive.Domestic conventional filtrate mainly contains quartz sand, gravel and anthracite etc.Quartz sand and gravel smooth surface, biomembrane poor adhesive force, the main suspension relied in mechanical retention effect removal sewage, function is relatively single.The biological activated carbon filter taking anthracite as representative, while guarantee turbidity removal effect, enhances filtering technique to organic biological degradation function, but still poor to the removal effect of nutrient.At present, China's water environment eutrophication problem is very serious.The excess load discharge of sanitary sewage and industrial wastewater Middle nutrition salt has become the main cause causing body eutrophication.Therefore, carrying out advanced treating to existing Sewage Plant secondary treatment yielding water makes nutrient concentrations wherein meet the even lower level of " urban wastewater treatment firm pollutant emission standard " (GB18918-2002) one-level A standard, to the quality of water environment important in inhibiting improving China's entirety.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of filtrate for sewage disposal and preparation method thereof, with deer natural pond soil for primary raw material, the synchronous strengthening that can realize suspension and phosphorus is removed, this filtrate has large and strong to the Adsorption ability of the P elements feature of specific area, to the synchronous removal important in inhibiting of suspension in sewage and P elements.
To achieve these goals, the technical solution used in the present invention is:
For a filtrate for sewage disposal, with quality than humic acid: clay: deer natural pond soil=(1-2): 5:10 gets raw material, and mixed sintering forms.
Further, can add with humic acid mass ratio when mixing is that the NaOH of 1:10 is as conditioning agent.
Present invention also offers a kind of method for the filtrate of sewage disposal described in preparation, comprise the steps:
1) deer natural pond soil is dried pulverize respectively with clay at 120 DEG C, mix to obtain mixture according to mass ratio 2:1 afterwards;
2) according to humic acid: clay: the mass ratio of deer natural pond soil=(1-2): 5:10, to step 1) add humic acid in gained mixture;
3) to step 2) add deionized water in gained mixed material and mix, control the moisture content of mixed material 70% ± 5%;
4) by step 3) gained material forms process, and average grain diameter controls between 5-10mm;
5) sintered under 700-800 DEG C of condition by the material after shaping, in Muffle furnace, Temperature fall, to (200 ± 10) DEG C, obtains the mixed material sintered afterwards;
6) by step 5) mixed material that sinters of gained carries out break process, obtains the finished product filtrate with irregular contour of equivalent grain size between 1-2mm.
Preferably, after described deer natural pond soil and clay dry rear pulverize, all remove average diameters in the part of more than 0.15mm by 100 mesh sieve subsets, mix again afterwards.
Preferably, described step 2) in, described humic acid is added according to the ratio of mass ratio 1:10 in the sodium hydroxide solution of mass concentration 1% and mixes to obtain mixed liquor, then this mixed liquor is added to step 1) in gained mixture.
Preferably, described step 4) by even for the material stirring prepared, put into forming machine extruded and cut, then in pan-type pelletizer, granulation obtains form of spherical particles raw material haydite, and control particle diameter is 5-10mm.
Preferably, described step 5) in sintering temperature condition be: in 10-20min, rise to design temperature 700-800 DEG C by room temperature, then continue sintering 120-160min at a set temperature.
Compared with prior art, the invention has the beneficial effects as follows:
(1) humic acid and conditioning agent NaOH is introduced in filtrate preparation process.Because the molecular weight of humic acid is large, carbon chain length, abundant pore passage structure can be formed in filtrate inside after sintering, increase the specific area of filtrate, but the connectedness in duct be poor; Add after NaOH through exploration discovery, contribute to humic acid strand and stretch, after sintering, can form a large amount of intercommunicating pores, the increase mass transfer rate of pollutant and the contact area effectively improved between filtrate and pollutant and the Adsorption ability to phosphorus thereof.
(2) contain the metallic elements such as a large amount of aluminium, calcium, magnesium, iron and manganese in the soil of deer natural pond, the P elements in sewage is efficiently removed by the formation by chemical bond.The present invention makes full use of the compositing characteristic of deer natural pond soil, is applied in the preparation of filtrate, to the recycling of deer natural pond soil and the synchronous removal important in inhibiting of phosphor in sewage element.
(3) except suspension, it is very limited to the phosphorus ligands performance in sewage that existing filtrate comprises quartz sand, gravel, anthracite and active carbon, the Novel filter material that the present invention proposes effectively has expanded the using function in filter tank, effectively can shorten waste water processes under the condition reaching identical removal effect.
(4) the biological phosphate-eliminating technology from traditional is different, the Novel filter material that the present invention proposes mainly relies on chemistry and physical adsorption process to carry out to the removal of phosphor in sewage element, and the stability of dephosphorization ability and phosphor-removing effect is all better than existing biological phosphate-eliminating technology.
To sum up, preparation method of the present invention is simple to operation, show through operation test, prepared filtrate is while guarantee is to the turbidity removal effect in Sewage Plant secondary treatment yielding water, have good total phosphorus removal capacity, effluent quality meets the A standard-required of China GB18918-2002 " urban wastewater treatment firm pollutant emission standard " primary standard.
Accompanying drawing explanation
Fig. 1 is finished product filtrate shape characteristic figure of the present invention.
Fig. 2 is the removal effect of filtrate of the present invention to variable concentrations pollutant.
Fig. 3 be under different adsorption time filtrate of the present invention to the Adsorption effect of TP.
Fig. 4 is filtrate of the present invention Adsorption effect to TP under different pH.
Fig. 5 for do not add humic acid (a) with add humic acid after (b) made filtrate to the Adsorption effect of TP.
Fig. 6 is the absorption property to phosphorus after media regeneration of the present invention.
Fig. 7 is the ruuning situation schematic diagram of the filter column system adopting filtrate of the present invention.
Detailed description of the invention
Embodiments of the present invention are described in detail below in conjunction with drawings and Examples.
In preparation method's research of filtrate of the present invention, inventors performed following process of the test, thus determine the more excellent controling parameters in filtrate preparation method.
(1) raw material is selected and preparation
Applicant finds after deliberation, and deer natural pond soil is a kind of rare material, originates in volcanic region, be generated by lower floor's volcanic soil, pH value is in acid, and general deer natural pond soil is in professional production and family's cultivation or soil improvement, all have good effect, it has very high permeability, retaining power and aeration.The size of deer natural pond soil is very not consistent, has many eyelets.Therefore, select deer natural pond soil as one of raw materials of filtrate.Appropriate clay is introduced to improve the mechanical strength of filtrate and relative proportion in sintering procedure.Meanwhile, add the humic acid of some and NaOH with the connectedness of the duct quantity and duct that increase filtrate inside, promote its Adsorption performance to pollutant.In addition, there is the volatilization of the organic mineralisings such as humic acid and steam in sintering procedure.All there is directly impact by the relative density of finished product filtrate and mechanical strength in mineralising gas and steam formation volume and rate of release etc.System optimization need be carried out to the humidity before pulp furnish, sintering time, sintering temperature, programming rate and mud ball sintering.
(2) pulp furnish optimization
Clay tool is a bit sticky, and is easy to be shaped after mixing with deer natural pond soil.But when clay ratios is too high, make filtrate too closely knit, duct is less, be unfavorable for increasing the alternate contact area of solid-liquid two.The clay controlling to be mixed in every kilogram of deer natural pond soil 0.3-0.5kg in preparation process is advisable.For increasing the duct quantity in filtrate, the more important thing is the quantity of intercommunicating pore, inventors performed lot of experiments.Select several frequently seen pore former, as starch, coal dust and lime stone etc., find that the connective duct that most of pore former is formed is less, have impact on pollutant migration in media as well and removal capacity.Humic acid is larger molecular organics matter, at high temperature carbonization can occur, and increases the duct quantity in filtrate.Therefore, final humic acid of selecting is as pore former.But when humic acid proportion is too high in preparation process, will mechanical strength and the relative density of filtrate be affected.When sintering time, sintering temperature and programming rate are all certain, adopt different humic acid quality than the intensity of the filtrate obtained under condition in table 1.As shown in Table 1, when the mass ratio of humic acid, clay and deer natural pond soil is 0-2:5:10, finished product ceramic grain filter has good intensity.The mass ratio determining humic acid, clay and deer natural pond soil is 0-2:5:10.
Table 1 different ratios of raw materials is on the impact of finished product filtrate intensity
Although the intensity of the less filtrate of the amount of humic acid is higher, the specific area of filtrate can be reduced, not reach the optimum efficiency removing pollutant., measure in test to the apparent density of filtrate and real density, the specific area in apparent density and real density larger explanation haydite is less for this reason.Result of the test shows, humic acid: clay: be optimum pulp furnish during the soil=1-2:5:10 of deer natural pond, this not only ensure that the intensity of filtrate also ensure that filtrate has huge specific area.
The real density of table 2 filtrate and apparent density
Wherein: TD: real density (TrueDensity) (kg/m
3)
AD: apparent density (ApparentDensity) (kg/m
3)
(3) sintering temperature
The intensity of sintering temperature on finished product filtrate has remarkable impact.Making temperature is too low, and filter structure is loose, and intensity is low; Temperature is too high, and ceramic grain filter easily occurs burning, and pore can be melted material blocking, the specific area of filtrate is declined, has an impact to filtrate adsorption fouling thing.
The finished product ceramic grain filter got under different temperatures carries out strength detection test.When pulp furnish, heating mode and sintering time are certain, the finished product that different sintering temperatures obtains spherical ceramic grain filter intensity results is as shown in table 2.As shown in Table 2, when sintering temperature is 700-800 DEG C, the intensity of each pollutant is optimum.
Impact on finished product filtrate intensity under the different sintering temperature of table 3
(4) calcination time
If sintering time is too short, obtained filtrate is loose, and intensity is not high.If sintering time is long, energy consumption is excessive.Get finished product filtrate and carry out strength detection test, under the condition that the condition such as pulp furnish and sintering temperature is certain, the intensity of the finished product filtrate that different sintering times obtains is as shown in table 4.When sintering time is 120-160min, filtrate intensity can meet the demands.
Impact on finished product filtrate intensity under the different sintering time of table 4
To sum up, by above-mentioned assay optimization controling parameters, obtain the preparation method of filtrate of the present invention, specifically comprise the steps:
Deer natural pond soil and clay are dried respectively at 120 DEG C; Require during oven dry that adjacent weighing for twice is not less than 3h interval time, weigh value difference and be less than minimum precision 0.01g.By the deer natural pond soil after oven dry and clay pulverize, and remove the component of average diameters at more than 0.15mm by 100 mesh sieve subsets; Mix to the deer natural pond soil after screening and clay powders according to mass ratio 2:1; Take appropriate humic acid powder, and it is mixed with 1% sodium hydroxide solution (conditioning agent).The mass ratio of humic acid and conditioning agent controls at about 1:10; According to humic acid: clay: the ratio of deer natural pond soil=(1-2): 5:10, in the mixture of clay and deer natural pond soil, add humic acid and conditioning agent mixed liquor, mix; In the mixture of humic acid, clay, conditioning agent and deer natural pond soil, add appropriate amount of deionized water, control the moisture content of mixed material about 70%, and mixing of materials is even; Adopt the mixed material handled well to form process, average grain diameter controls between 5-10mm; Mixed material after being shaped is sintered under 700-800 DEG C of condition, in sintering process, cavity temperature rises to design temperature (700-800 DEG C) by room temperature quick (10-20min), then continue sintering 120-160min at a set temperature, after completing, when Temperature fall is to about 200 DEG C in Muffle furnace, take out the mixed material sintered; Finally carried out break process and can obtain the finished product filtrate with irregular contour of equivalent grain size between 1-2mm, its shape characteristic as shown in Figure 1.
The filtrate made is carried out adsorption test, and step is as follows:
(1) total phosphorus solution of variable concentrations is joined in the colorimetric cylinder of 50mL, add 10g filtrate, leave standstill 24h at 25 DEG C after, get supernatant, cross 0.45 μm of filter membrane, measure the equilibrium concentration of total phosphorus, calculate clearance.As shown in Figure 2, the clearance first increases and then decreases of TP, the clearance of Novel filter material to TP is stabilized in about 95%, and when initial concentration is 2mg/L, clearance is maximum, can reach 98.64%.Initial concentration is that the resistance to mass tranfer overcome between liquid phase and solid phase provides important motive force, and therefore initial phosphorus concentration raises the adsorption capacity being conducive to improving filtrate, but the too high clearance that can reduce phosphorus of initial concentration.
(2) under the condition that TP concentration is certain, control different sorption reaction time, get supernatant and cross 0.45 μm of filter membrane, measure equilibrium concentration, calculate adsorption capacity.As shown in Figure 3, filtrate to TP in the starting stage rate of adsorption quickly, substantially reaches balance after 6h.
(3) TP concentration is certain, and regulate initial pH, other condition is described above.As shown in Figure 4, the minimum adsorption effect in neutral conditions of TP equilibrium concentration when pH=7 is better.Meanwhile, haydite has cushioning effect to pH in sewage, and the pH adsorbed in rear solution reaches unanimity.
From above-mentioned Adsorption experimental results, the present invention is according to humic acid: clay: the ratio of deer natural pond soil=(1-2): 5:10, and the Novel filter filtrate that introducing NaOH conditioning agent is developed simultaneously has good Adsorption performance to the phosphorus in water.The filtrate only adopting clay and deer natural pond soil to prepare for raw material under the same terms is compared, reach identical TP removal effect, introducing humic acid is only simple as pore former and NaOH as the use amount of filtrate after conditioning agent and uses clay and deer natural pond soil to be 1/4 during raw material (Fig. 5).Experiment condition is as follows: join in the colorimetric cylinder of 50mL by total phosphorus solution of different initial concentration, add filtrate, gets supernatant after leaving standstill 24h at 25 DEG C, crosses 0.45 μm of filter membrane, measures the equilibrium concentration of total phosphorus, calculates clearance.Fig. 5 a is for after adding humic acid, and 10g filtrate is to the removal effect of TP, and Fig. 5 b is not for add humic acid, and 40g filtrate is to the removal effect of TP.
Filtrate after absorption is carried out regeneration tests, and concrete steps are as follows:
Configuration concentration is 5mg/LTP solution, add 2g filtrate, carry out adsorption experiment, after having adsorbed, filtrate is dried, regenerate with the NaOH of 0.05%, after regeneration, again carry out adsorption experiment, 3 times so repeatedly, experimental result is as shown in Figure 6: therefrom can obtain after 3 adsorption-desorptions circulations, and filtrate can also with higher clearance absorption total phosphorus.
By finished product filtrate dress post, carry out filtration test, concrete steps are as follows:
The post height 1.5m of filtration system, diameter is 50mm.Filter post and collector pipe joining place filter screen separate, and filter opening aperture is 1.0mm.Filtrate depth of cracking closure is 1.0m, and current are lower to stream, and namely sewage enters by filtering post upper end, carries out sewage disposal via filter material layer, is finally catchmented by the collector pipe of end and is flowed out by outlet.Sewage in filter post adopts artificial distribution, paper examines turbidity and total phosphorus situation of change, simulation of water quality Sewage Plant secondary effluent, and influent turbidity and total phosphorus control to control about 7 at about 30mg/L and 1mg/L, pH respectively, and the water intake velocity of filter column system is 5.0m/h.As can be seen from Figure 7 the turbidity in water outlet is at about 1.0NTU, and water outlet total phosphorus mean concentration is 0.092mg/L, both operationally in all meet the A standard-required of GB18918-2002 " urban wastewater treatment firm pollutant emission standard " primary standard.
For contrast introduces NaOH conditioning agent to the impact of finished product filtrate pollutant removal.Adopt according to humic acid: clay: the ratio preparation of deer natural pond soil=(1-2): 5:10, but finished product filtrate obtained when not introducing conditioning agent is adopted to use the same method and carried out filtration test with condition, result as shown in figures 7 c and 7d.As seen from the figure, the residual quantity of filtering total phosphorus in water outlet when introducing conditioning agent is relatively stable, average out to 0.156mg/L; And filtrate does not adopt when preparing the residual quantity of filtering TP in water outlet during conditioning agent to have obvious ascendant trend along with the increase of filtration time.But, whether adopt conditioning agent on the impact of the removal effect of its suspension in filtrate preparation process and not obvious.
To sum up analyze known, the treatment effect of filtrate to secondary effluent prepared by method of the present invention is good, water outlet meets the A standard-required of GB18918-2002 " urban wastewater treatment firm pollutant emission standard " primary standard, and this filtrate dephosphorization ability is high, has good environmental benefit and social benefit.
Claims (6)
1. for a filtrate for sewage disposal, with quality than humic acid: clay: deer natural pond soil=(1-2): 5:10 gets raw material, and mixed sintering forms, and it is characterized in that, adding during mixing with humic acid mass ratio is that the NaOH of 1:10 is as conditioning agent.
2. prepare the method for the filtrate of sewage disposal described in claim 1, it is characterized in that, comprise the steps:
1) deer natural pond soil is dried pulverize respectively with clay at 120 DEG C, mix to obtain mixture according to mass ratio 2:1 afterwards;
2) according to humic acid: clay: the mass ratio of deer natural pond soil=(1-2): 5:10, to step 1) add humic acid in gained mixture;
3) to step 2) add deionized water in gained mixed material and mix, control the moisture content of mixed material 70% ± 5%;
4) by step 3) gained material forms process, and average grain diameter controls between 5-10mm;
5) sintered under 700-800 DEG C of condition by the material after shaping, in Muffle furnace, Temperature fall, to (200 ± 10) DEG C, obtains the mixed material sintered afterwards;
6) by step 5) mixed material that sinters of gained carries out break process, obtains the finished product filtrate with irregular contour of equivalent grain size between 1-2mm.
3. according to claim 2 for the preparation of the method for the filtrate of sewage disposal, it is characterized in that, after described deer natural pond soil and clay dry rear pulverize, all remove average diameters in the part of more than 0.15mm by 100 mesh sieve subsets, mix again afterwards.
4. according to claim 2 for the preparation of the method for the filtrate of sewage disposal, it is characterized in that, described step 2) in, described humic acid is added according to the ratio of mass ratio 1:10 in the sodium hydroxide solution of mass concentration 1% and mixes to obtain mixed liquor, then this mixed liquor is added to step 1) in gained mixture.
5. according to claim 2 for the preparation of the method for the filtrate of sewage disposal; it is characterized in that; described step 4) in forming processing step be: by even for the material stirring prepared; put into forming machine extruded and cut; then in pan-type pelletizer, granulation obtains form of spherical particles raw material haydite, and control particle diameter is 5-10mm.
6. according to claim 2 for the preparation of the method for the filtrate of sewage disposal, it is characterized in that, described step 5) in sintering temperature condition be: in 10-20min, rise to design temperature 700-800 DEG C by room temperature, then at a set temperature continue sintering 120-160min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2691696B2 (en) * | 1995-04-04 | 1997-12-17 | 科学技術庁無機材質研究所長 | Clay-humic acid composite porous body and method for producing the same |
| JP3794003B2 (en) * | 1998-01-12 | 2006-07-05 | 平井工業株式会社 | Phosphate ion-adsorbing filter medium and production method |
| JP2002001372A (en) * | 2000-06-28 | 2002-01-08 | Pekku:Kk | Sewage cleaning apparatus |
| CN1727290A (en) * | 2004-07-30 | 2006-02-01 | 峨眉山市大千实业有限公司 | Filter material of artificial pozzolana in use for aerating biological filter |
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