CN105170091A - Preparation method of iron-modified reed biological carbon, and application of iron-modified reed biological carbon in treatment of phosphorus wastewater - Google Patents
Preparation method of iron-modified reed biological carbon, and application of iron-modified reed biological carbon in treatment of phosphorus wastewater Download PDFInfo
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Abstract
The invention provides a preparation method of iron-modified reed biological carbon, and application of the iron-modified reed biological carbon in treatment of phosphorus wastewater, and belongs to the field of water pollution control. The preparation method comprises the following steps: pre-treating reed straws; performing pyrolysis carbonization on the pre-treated reed straws to obtain biological carbon; cooling the biological carbon obtained from the pyrolysis carbonization to room temperature, grinding the biological carbon to enable the ground biological carbon to pass through a 10-50-mesh sieve, washing with clean water for a plurality of times, removing ash on the surface, and drying for later use; dissolving FeCl3 in water, adding the dried biological carbon, and stirring uniformly, wherein the mass ratio of iron to carbon is (0.56-1) to 1; evaporating moisture to dryness in a drying box at 85-105 DEG C, and performing heat treatment for 2h; washing the taken carbon with water until washing liquor is neutral, and drying for 6-12h so as to obtain the iron-modified reed biological carbon. A method is simple in process and is suitable for industrial process. The prepared iron-modified reed biological carbon is easy and liable when used in a dephosphorization technology, is good in adsorbing effect, and has a good application prospect in the low-concentration phosphorus wastewater and deep dephosphorization in sewage.
Description
technical field:
The present invention relates to a kind of preparation of iron modification reed charcoal, and be applied to process low-concentration phosphorus-containing wastewater and sewage deep dephosphorization, belong to field of water pollution control.
background technology:
Water resource occupancy volume per person is few in China, and distribution is uneven, and along with economic development and social total growth in the living standard, the demand of water resource is growing, and water pollution is serious.Wherein the water pollution of the surface water such as lake is more than half is to be exceeded standard the body eutrophication caused by nitrogen, phosphorus.According to Li Beige minimum of a value law: the growth of plant depends on that the external world is supplied to that minimum one of quantity in its required nutriment.The empirical formula of algae is C
106h
236o
110n
16p, can find, what in algae molecular formula, shared percentage by weight was minimum is nitrogen and phosphorus, especially phosphorus.So the eutrophication of phosphorus to control surface water controlled in sanitary sewage is vital.Be 0.5mg/L and 1mg/L according to one-level A standard in " urban wastewater treatment firm pollutant emission standard " (GB18918-2002) and B standard regulation phosphorus concentration limit value.And general town sewage after necessarily process in phosphorus concentration generally at 1-4mg/L, so, except will controlling pollution source, also need to find a kind of cost-effective method and remove Phosphorus From Wastewater, make it meet associated emission standard.
Conventional Sewage Biological Treatment is not high to low-concentration phosphorus-containing wastewater removal efficiency, and common secondary biochemical treatment method can only remove nitrogen and the phosphorus of 30%-50%, and be difficult to up to standard and complicated mechanism, process is wayward.Although chemical precipitation method dephosphorization clearance is very high, application is also very extensive, needs to add flocculant in waste water, so add processing cost, and can produce a large amount of chemical sludges.Absorption method dephosphorization due to efficient fast, non-secondary pollution, easy to operate, recoverable, metal oxide active point abundant and it is with low cost, become the study hotspot of domestic and international dephosphorization.
Charcoal is widely used in the research and practice of the aspects such as carbon fixation and emission reduction, soil remediation improvement, polluted water purification in recent years, has that cost is low, advantages of environment protection.Existing relevant scholar's research shows that the charcoal of the preparations such as paddy rice, wheat, corn has good suction-operated to pollutant in water body, Liu Jinge etc.
[1]the adsorption effect that have studied fresh kidney beans straw biological charcoal centering water chromium is remarkable, Zhang Hui etc.
[2]have studied charing rice straw to the absorption of ammonia nitrogen in water body and phosphorus, result shows that removal effect is greater than flyash and slag, RenJing etc.
[3]use the phosphorus in cotton stalk charcoal load iron removal water body, increase the clearance of phosphorus, the potentiality of this technology extensive application of charcoal purifying water body.Following several large advantage is had: 1. reed is fast as a kind of reproduction speed with reed straw charcoal load iron modification dephosphorization, the water plant that biomass is large, give free rein to rot to decompose if removed not in time, can pollute, this invention utilizes reed to prepare charcoal for raw material, rubbish is turned waste into wealth, improves the level of resources utilization, decreasing pollution; 2. charcoal has the characteristic of solid carbon, serve large gas carbon storehouse and increase the reduction of discharging effect that converges, and its loose structure adds the load factor of iron; 3. modifier iron chloride low price, nontoxic, phosphate radical and the iron ion of load in carbon surface and hole react has an effect, and can reach good phosphor-removing effect, and operating procedure is simple, and non-secondary pollution; 4. the adsorbent after absorption contains more rich phosphorus, can be used as plant growth fertilizer reuse.
summary of the invention:
The present invention is directed to the weak point of traditional dephosphorization technique, a kind of preparation method of iron modification reed charcoal is provided, the method limit oxygen and relative low temperature (<700 DEG C) condition under, the rich carbon, fine grained, the porous material that are produced by biomass material pyrolysis.
The object of the invention is to provide the iron modification reed charcoal that above-mentioned preparation method obtains.
The present invention also provides the application utilizing iron modification reed charcoal as adsorbent, the application mainly in process low-concentration phosphorus-containing wastewater.
Technical scheme corresponding claims book, undetermined.
A preparation method for iron modification reed charcoal, the preparation process of the method is as follows:
(1) first pretreatment is carried out to reed straw;
(2) reed pretreated for step (1) is carried out pyrolysis charring;
(3) charcoal that step (2) pyrolysis charring obtains is cooled to room temperature, ground 10-50 mesh sieve, with water cleaning several, removes surperficial ash content, dry for standby;
(4) FeCl is got
3soluble in water, add the charcoal of drying in step (3) and stir and evenly mix, keep iron charcoal mass ratio to be 0.56-1:1; Being placed in baking oven at the temperature of 85-105 DEG C keeps 6-12h, by moisture evaporate to dryness, then at 300-500 DEG C of heat treatment 2h; It is neutrality that taking-up washes with water to washing lotion, dries 6-12h, obtain iron modification reed charcoal finished product at the temperature of 85-105 DEG C.
Further design of the present invention is:
Pretreatment in step (1), washes the reed of harvesting with water surface dirt, is then put by clean reed and dries to constant weight in 85-105 DEG C in an oven, and the section that taking-up is broken into 0.5-1cm long is for subsequent use.
In step (2), pyrolysis temperature is 300-500 DEG C, and raising speed temperature is 15 DEG C/min, keeps 4-8h.
In step (3), oven dry is dry in 90-100 DEG C of baking oven.
In step (4), heat treatment temperature is 350-450 DEG C.
The iron modification reed charcoal that said method prepares.
The application of above-mentioned modification reed charcoal in process low-concentration phosphorus-containing wastewater.Be mainly used in low-concentration phosphorus-containing wastewater process that concentration range is 1-4mg/L and advanced treatment of wastewater.
Obtain load iron modification reed charcoal by said method, can be used as a kind of excellent adsorbent, and adopt absorption dephosphorization process, adsorption treatment phosphorus-containing wastewater, save adsorbent amount when and make water outlet water quality reaching standard.
beneficial effect of the present invention is as follows:
(1) the present invention adopts reed straw to be biological carbon feedstock, wide material sources, cheap, and the present invention is also for the handling problems solving reed sediment substrate provides new approach.Containing cellulose in reed straw, can be used to papermaking, weaving mat, curtain etc.; Root of phragmites communis also has medical value; Reed Leaves can be used for bag pyramid-shaped dumpling.Due to features such as reed vitality is strong, fast growths, be sight spot tourism, water surface greening, river management, purify water, protect native dyke strengthening, improve first choice of soil.But China's reed annual production is large, and according to statistics, China's area of Phragmites communis is about 1,300,000 hm
2, gross annual output amount is more than 2,200,000 tons
[4]really be used as papermaking, medicinal etc. reed amount is limited, most reed straw is still had to obtain Appropriate application, if do not processed in time, can rot to cause environmental pollution, so carry out the recycling of wetland plant reed, seek the new way turned waste into wealth, become hot issue urgently to be resolved hurrily.And the present invention is for which providing a kind of effective solution route, realize the object of recycling.
(2) the invention provides a kind of preparation technology of iron modification reed charcoal, by reed straw is mixed with ferrous solution dry after the method for calcine prepare modification reed charcoal, preparation is simple, applicable suitability for industrialized production.The oxide of modified reed charcoal surface meeting load iron or oxyhydroxide, had an effect by chemical reaction with the phosphate radical in water body, thus reach the effect removing phosphorus, so the iron of phosphor-removing effect and load has direct relation.
Iron modified technique provided by the invention is compared to other people iron modified technique, and as the zeolite-loaded iron such as Lu Yanqin, directly mixed with iron nitrate solution by zeolite and dry, its load capacity is maximum is only 8.325mg/g
[6], Luo Shujun have studied loaded modified bamboo charcoal and removes Phosphorus From Wastewater, and be carried on bamboo charcoal with cooking process repeatedly by iron chloride, maximum load iron is 41.53mg/g
[7], method of modifying load iron provided by the invention is 53.94mg/g, and the load effect of iron is better.
Modified reed charcoal processes initial concentration at temperature is 25 DEG C when being the phosphorus solution of 4mg/L, equilibrium adsorption capacity is 1.55mg/g, and unmodified reed charcoal equilibrium adsorption capacity is 0.019mg/g, modification reed charcoal adsorbance is 81.6 times of reed charcoal adsorbance, and modified phosphor-removing effect is remarkable.
(3) adsorbent of the present invention can be applicable to process phosphorous sanitary sewage, makes its qualified discharge.Charcoal after adsorption and dephosphorization includes abundant iron and P elements, can also recycle as fertilizer also field, and non-secondary pollution produces, economic benefits.This iron modification reed charcoal belongs to a kind of good adsorption performance, environmental protection shaped material.
Reed sediment substrate is recycled by the present invention, is prepared into charcoal, is sealed up for safekeeping by the carbon in organic matter, serves the effect increasing and converge and reduce discharging, decreases discharge and the atmosphere pollution of greenhouse gases.Due to the loose structure that reed charcoal is special, can interaction adsorbent, the polluter in adsorb atmospheric, soil and water, as phosphorus in Adsorption water body.Porosity characteristic is that Soil Microorganism provides migration place, and some nutrients that charcoal itself contains are also for soil provides fertility, can also be used as soil conditioner after absorption.Thus, method of the present invention has higher environment and economy benefit.Compare paddy rice and wheat, the phosphor-removing effect of three kinds of stalks has carried out comparison and analysis, as follows:
1) Wu Wenqing
[5]carry out etherification reaction with wheat stalk through alkali lye-ultrasonic wave process, introduce Fe
3+prepare adsorbent, adsorbent dosage is under the neutral environment of 0.1g, and process initial concentration is the phosphate solution 24h of 3mg/L, and rear residual concentration is 2.3mg/L, and the clearance of phosphorus is only 23.3%, and adsorbance is 0.23mg/g.And modification reed charcoal prepared by the present invention processes the phosphate solution 6h of 3mg/L under the same conditions, residual concentration is 0.467mg/L, the clearance of phosphorus reaches 84.4%, and adsorbance is now 1.267mg/g, and phosphor-removing effect is obviously better than wheat stalk adsorbent.
2) current, utilize the research of rice straw charcoal dephosphorization very few, main cause should be that colourity contained by rice straw charcoal is comparatively large, and water liquid during cleaning is buff, and this may be relevant with the growth course of paddy rice.And the phosphorus content of rice straw charcoal own is large, the phosphorus in process water body especially low-concentration phosphorus-containing wastewater time, have the phenomenon of a large amount of P elements stripping.
In sum, in the recycling problem solving reed sediment substrate, according to its special structure and energy-saving and emission-reduction advantage, there is very large application prospect at present, therefore reed straw is prepared into charcoal, be the recycling of reed sediment substrate, provide effective solution route.And adsorbent prepared by the present invention, on phosphor-removing effect compared with other agricultural crop straws, has obvious advantage, be conducive to processing low-concentration phosphorus-containing wastewater.
(4) the present invention is in process low-concentration phosphorus-containing wastewater technique, have employed second adsorption technique, by the adsorbent reuse after use, carry out second time absorption again, compared to traditional absorbing process, when making water outlet water quality reaching standard, saving the use amount of adsorbent, is a kind of dephosphorization process of energy-saving and emission-reduction.
accompanying drawing illustrates:
Fig. 1 is the XRD collection of illustrative plates of iron modification reed charcoal prepared by example one.
detailed description of the invention:
Below in conjunction with the drawings and specific embodiments, in the phosphorus-containing wastewater of process low concentration, more detailed description is done to the Synthesis and applications of iron modification biological charcoal in the present invention.
prepare example:
example one:
The making concrete steps of iron modification reed charcoal of the present invention are as follows:
(1) reed straw picks up from Nanjing wetland, washes away surface dirt by deionized water, is then put by clean reed and dries to constant weight in 100 DEG C in an oven, takes out the fritter shredding into length and be about 0.5-1cm.
(2) reed being broken into fritter in (1) step is filled in crucible, is placed in Muffle furnace and carries out pyrolysis, pyrolysis temperature is 350 DEG C, and temperature raising speed is 15 DEG C/min, keeps 6h.
(3) after pyrolysis in (2) step being completed, taking-up crucible is cooled to room temperature, be the reed charcoal prepared, by its ground 10-50 mesh sieve, with washed with de-ionized water several, remove residual ash in pyrolytic process, be placed in baking oven and dry to constant weight for subsequent use at 100 DEG C.
(4) FeCl is taken
3be dissolved in deionized water, preparation iron concentration is the solution of 1mol/L, adds the charcoal of drying in (3) step and stirs and evenly mixs, and keeps iron and charcoal mass ratio to be 0.56:1.Be placed in baking oven by moisture evaporate to dryness at the temperature of 100 DEG C, then proceeded in Muffle furnace in 350 DEG C of continuation heat treatment 2h.It is neutral that rear taking-up deionized water is washed till filtrate, is placed in 100 DEG C, baking oven and dries 10h, obtain iron modification reed charcoal finished product.
The XRD collection of illustrative plates of the iron modification reed charcoal of preparation as shown in Figure 1.Fe is had in XR spectrogram
2o
3characteristic peak, illustrate that modified iron oxide mainly exists with bloodstone form, and in the oxide of iron, the adhesive strength of bloodstone and reed charcoal is the highest.So compared with the preparation technology of other dephosphorization modified adsorbents, the load of iron is more firm, and load capacity is also larger, thus phosphor-removing effect is better.
example two:the making concrete steps of iron modification reed charcoal of the present invention are as follows:
(1) reed straw picks up from Nanjing wetland, washes away surface dirt by deionized water, is then put by clean reed and dries to constant weight in 90 DEG C in an oven, takes out the fritter shredding into length and be about 0.5-1cm.
(2) reed being broken into fritter in (1) step is filled in crucible, is placed in Muffle furnace and carries out pyrolysis, pyrolysis temperature is 450 DEG C, and temperature raising speed is 15 DEG C/min, keeps 4h.
(3) after pyrolysis in (2) step being completed, taking-up crucible is cooled to room temperature, be the reed charcoal prepared, by its ground 10-50 mesh sieve, with washed with de-ionized water several, remove residual ash in pyrolytic process, be placed in baking oven and dry to constant weight for subsequent use at 90 DEG C.
(4) FeCl is taken
3be dissolved in deionized water, preparation iron concentration is the solution of 1mol/L, adds the charcoal of drying in (3) step and stirs and evenly mixs, and keeps iron and charcoal mass ratio to be 1:1.Be placed in baking oven by moisture evaporate to dryness at the temperature of 90 DEG C, then proceeded in Muffle furnace in 450 DEG C of continuation heat treatment 2h.It is neutral that rear taking-up deionized water is washed till filtrate, is placed in 90 DEG C, baking oven and dries 12h, obtain iron modification reed charcoal finished product.
application example: iron modification reed charcoal is used for adsorption treatment low-concentration phosphorus-containing wastewater
The iron modification reed charcoal prepared using example one of following test is as the adsorbent of dephosphorization, verify that it has good adsorption effect to phosphorus in water body, in the process of adsorption and dephosphorization, be the phosphorus-containing wastewater of 1-4mg/L according to 0.5-4g/L dosage concentration for the treatment of, pH value of waste water is in 6-8 scope, temperature, between 20-30 DEG C, keeps the rotating speed absorption 5-8h of 80-120r/min.Compare phosphor-removing effect by three kinds of different treatment process, and by the actual phosphorus-containing wastewater of process, have more the substantial effect demonstrating the dephosphorization of iron modification biological charcoal, embody rule embodiment is as follows:
test case 1
Take 0.05 respectively, 0.05,0.1,0.1g modification biological charcoal be added to 50ml concentration be 1,2,3, in the solution containing phosphate of 4mg/L, pH value of solution is regulated to be 7 with HCl and NaOH that concentration is all 1M, under 25 DEG C of temperature, rotating speed are 120r/min condition, constant temperature oscillation 6h, extracts whole water sample A with vacuum filtration pump
1(A
11~ A
14), then by each A
1water sample adds 0.05 successively again, 0.05,0.1,0.1g modification biological charcoal, adsorption process same above carrying out, suction filtration after 6h, the charcoal after Separation of Solid and Liquid is designated as B
1(B
11~ B
14), and the phosphorus concentration C in measurement and calculation filtrate
1(C
11~ C
14) be respectively 0.084,0.462,0.342,0.470mg/L, can find out, a certain amount of adsorbent is after twice Batch absorption process, and aqueous concentration is all less than 0.5mg/L, meets the one-level emission standard A in " urban wastewater treatment firm pollutant emission standard " (GB18918-2002).
test case 2
Process initial concentration is the phosphorus-containing wastewater of 1mg/L, first by the charcoal B in test case 1
11recycle, being added to 50mL concentration is in the phosphorus-containing wastewater of 1mg/L, and regulate pH value of solution to be 7 with HCl and NaOH that concentration is all 1M, under 25 DEG C of temperature, rotating speed are 120r/min condition, constant temperature oscillation 6h, extracts whole water sample A with vacuum filtration pump
21, water sample A
21add again fresh Modified Activated Carbon 0.05g carry out above same adsorption process, suction filtration after 6h, and the phosphorus concentration C in measurement and calculation filtrate
21for 0.112mg/L.Can find out, after adsorption treatment, although aqueous concentration is a bit larger tham C
11value, but still be less than the one-level A standard value 0.5mg/L in " urban wastewater treatment firm pollutant emission standard " (GB18918-2002), and C
21value at below 0.2mg/L, reach III class water total phosphorus concentration limit value in " water environment quality standard " (GB3838-2002).
test case 3
Process initial concentration is the phosphorus-containing wastewater of 2mg/L, first by the adsorbent B of the later stage absorption 2mg/L phosphorus-containing wastewater in test case 1
12reclaim, being again added to 50mL concentration is in the phosphorus-containing wastewater of 2mg/L, and regulate pH value of solution to be 7 with HCl and NaOH that concentration is all 1M, under 25 DEG C of temperature, rotating speed are 120r/min condition, constant temperature oscillation 6h, extracts whole water sample A with vacuum filtration pump
22, at water sample A
22in add again fresh Modified Activated Carbon 0.05g carry out above same adsorption process, suction filtration after 6h, and the phosphorus concentration C in measurement and calculation filtrate
22for 0.498mg/L.After adsorption treatment, aqueous concentration is greater than C
120.462mg/L, but still be less than the one-level A standard value 0.5mg/L in " urban wastewater treatment firm pollutant emission standard " (GB18918-2002).
test case 4
Process initial concentration is the phosphorus-containing wastewater of 3mg/L, first by the adsorbent B of the later stage absorption 3mg/L phosphorus-containing wastewater in test case 1
13reclaim, being again added to 50mL concentration is in the phosphorus-containing wastewater of 3mg/L, and regulate pH value of solution to be 7 with HCl and NaOH that concentration is all 1M, under 25 DEG C of temperature, rotating speed are 120r/min condition, constant temperature oscillation 6h, extracts whole water sample A with vacuum filtration pump
23, at water sample A
23in add again fresh Modified Activated Carbon 0.1g carry out above same adsorption process, suction filtration after 6h, and the phosphorus concentration C in measurement and calculation filtrate
23for 0.467mg/L.After adsorption treatment, aqueous concentration is a bit larger tham C
130.342mg/L, but still be less than the one-level A standard value 0.5mg/L in " urban wastewater treatment firm pollutant emission standard " (GB18918-2002).
test case 5
Process 5m
3phosphorus concentration is the phosphorus-containing wastewater of 1mg/L, every for modification biological charcoal 0.5kg is put in a pore string bag, be suspended in pond, hang five altogether, 2.5kg, pond pH are 7.3 altogether to add iron modification biological charcoal, water temperature is 23 DEG C, speed of agitator is 100r/min, ensures that waste water fully contacts with adsorbent, after adsorption treatment 7h.Taken out by Modified Activated Carbon, continue to add 2.5kg Modified Activated Carbon in the same manner, take out after then continuing adsorption reaction 7h, the Modified Activated Carbon this time taken out is designated as B
21, and water sampling measure and calculation phosphoric residue concentration is 0.345mg/L.
By B
21after recovery, be again added to 5m
3phosphorus concentration is in the phosphorus-containing wastewater of 1mg/L, and wastewater pH is 7.1, and water temperature is 22 DEG C, by B
21every 0.5kg puts in a pore string bag, is suspended in pond, and hang five altogether, speed of agitator is 100r/min, ensures that waste water fully contacts with adsorbent, after adsorption treatment 7h.Modified Activated Carbon is taken out, continue to add the fresh Modified Activated Carbon of 2.5kg in the same manner, then take out after continuing adsorption reaction 7h, after adsorption treatment, aqueous concentration is 0.407mg/L, still be less than the one-level A standard value 0.5mg/L in " urban wastewater treatment firm pollutant emission standard ", can qualified discharge.
test case 6
Process 5m
3phosphorus concentration is the phosphorus-containing wastewater of 1.5mg/L, every for modification biological charcoal 1kg is put in a pore string bag, be suspended in pond, hang four altogether, 4kg, pond pH are 6.8 altogether to add iron modification biological charcoal, water temperature is 23 DEG C, speed of agitator is 100r/min, ensures that waste water fully contacts with adsorbent, after adsorption treatment 7h.Taken out by Modified Activated Carbon, continue to add 4kg Modified Activated Carbon in the same manner, take out after then continuing adsorption reaction 7h, the Modified Activated Carbon this time taken out is designated as B
22, and water sampling measure and calculation phosphoric residue concentration is 0.444mg/L.
By Modified Activated Carbon B
22after recovery, be again added to 5m
3phosphorus concentration is in the phosphorus-containing wastewater of 1.5mg/L, and wastewater pH is 7.1, and water temperature is 23 DEG C, by Modified Activated Carbon B
22every 1kg puts in a pore string bag, is suspended in pond, and hang four altogether, speed of agitator is 100r/min, ensures that waste water fully contacts with adsorbent, after adsorption treatment 7h.By Modified Activated Carbon B
22take out, continue to add the fresh Modified Activated Carbon of 4kg in the same manner, take out, after adsorption treatment after then continuing adsorption reaction 7h, aqueous concentration is 0.479mg/L, is still less than the one-level A standard value 0.5mg/L in " urban wastewater treatment firm pollutant emission standard " (GB18918-2002).
test case 7
Process 5m
3phosphorus concentration is the phosphorus-containing wastewater of 2.8mg/L, every for modification biological charcoal 1kg is put in a pore string bag, be suspended in pond, hang ten altogether, 10kg, pond pH are 6.5 altogether to add iron modification biological charcoal, water temperature is 23 DEG C, speed of agitator is 100r/min, ensures that waste water fully contacts with adsorbent, after adsorption treatment 7h.Taken out by Modified Activated Carbon, continue to add 10kg Modified Activated Carbon in the same manner, take out after then continuing adsorption reaction 7h, the Modified Activated Carbon this time taken out is designated as B
23, and water sampling measure and calculation phosphoric residue concentration is 0.322g/L.
Continue Modified Activated Carbon to reclaim to be labeled as B
23after recovery, be again added to 5m
3phosphorus concentration is in the phosphorus-containing wastewater of 2.8mg/L, and wastewater pH is 6.7, and water temperature is 23 DEG C, by B during input
23every 1kg puts in a pore string bag, is suspended in pond, and hang ten altogether, speed of agitator is 100r/min, ensures that waste water fully contacts with adsorbent, after adsorption treatment 7h.By Modified Activated Carbon B
23take out, continue to add the fresh Modified Activated Carbon of 10kg in the same manner, then take out after continuing adsorption reaction 7h, after adsorption treatment, aqueous concentration is 0.467mg/L, is still less than the one-level A standard value 0.5mg/L in " urban wastewater treatment firm pollutant emission standard " (GB18918-2002).
As seen from the above:
In application testing example 1 of the present invention, be divided into adding for twice by a certain amount of adsorbent and carry out adsorption and dephosphorization, the adsorbent that second time adds can be used further to subsequent adsorbtion.The adsorbent that second time in test case 1 is added use by the method in test case 2 to 4 reclaims, and carrying out second adsorption, ensureing that effluent quality is up to standard when reducing adsorbent use amount.Test case 5 in 7 with modification biological charcoal process actual phosphorus-containing wastewater, result shows, adsorbent can carry out secondary and utilize and process waste water, and aqueous concentration is all less than 0.5mg/L.
The present invention is compared with existing dephosphorization technique, not only prepare and a kind ofly there is good phosphor-removing effect and environmentally friendly modification biological charcoal makees adsorbent, also have found the adsorption and dephosphorization technique of corresponding optimization, have the double dominant of energy-saving and emission-reduction and resource circulation utilization, and have a good application prospect.
comparative analysis:
The advantage that reed charcoal is compared with other sorbent materials is as follows:
In prior art, the charcoal that relevant scholar utilizes zeolite or bamboo charcoal, wheat stalk etc. to be prepared into carries out the research of dephosphorization to its load iron, according to iron generation chemical reaction and the ion-exchange of the phosphorus in the modified adsorbent for phosphate removal mechanism of load iron mainly water body and load, thus reach the effect removed from water, and the removal effect of phosphorus and sorbent-loaded iron have very large relation.
The zeolite-loaded iron such as Lu Yanqin, directly mixed with iron nitrate solution by zeolite and dry, its load capacity is maximum is only 8.325mg/g
[6]the research that current zeolite does the pollutants such as adsorbent removal Heavy Metals in Waters organic matter is more, regeneration can be carried out after absorption, and with zeolite adsorption process nitrogen phosphorus etc., nitrogen phosphorus itself is that nutrient also can be used as fertilizer in field, as the zeolite after absorption is carried out regeneration process, processing cost can be added, so be unfavorable for promoting, so Comparatively speaking, be a kind of method turning waste into wealth, recycle with the dephosphorization of charcoal load iron, avoid secondary pollution.
Luo Shujun have studied loaded modified bamboo charcoal and removes Phosphorus From Wastewater, and be carried on bamboo charcoal with cooking process repeatedly by iron chloride, maximum load iron is 41.53mg/g
[7].Cooking process is cumbersome repeatedly, is not suitable for promoting.Li Jihui iron chloride modified wheat straw biological charcoal, has inquired into the effect of its phosphate adsorption, by Fe
3+mix with 6 kinds of different quality ratios with wheat straw biologic charcoal, modification is carried out to it.Determine Fe
3+when being 0.7 with the best mixing quality ratio of charcoal, adsorption effect is best, but the method modification makes the load effect of iron poor
[8], thus affect its phosphor-removing effect.
The reed selected in the present invention is prepared into charcoal as charcoal raw material, and carries out the modification of load iron chloride, and its load iron can reach 53.94mg/g, the bamboo charcoal that load effect is more above-mentioned and wheat stalk effective.And the present invention is in research process, the charcoal be prepared into rice straw, reed straw, raw material that these three kinds of annual productions of rice husk are all larger has carried out adsorption and dephosphorization and has compared, the three kinds of charcoals not carrying out load iron modification prepared under the same terms, when processing low-concentration phosphorus-containing wastewater, paddy rice and rice husk charcoal all have more phosphorus stripping phenomenon, and the phosphorus stripping that the present invention adopts reed straw only little, this may with plant in growth course, relevant with the elemental composition of itself to the absorption of soil Middle nutrition material.So reed is prepared into charcoal, be prepared into adsorbent, compare with load iron effect with the source of other sorbent materials, preprocessing process, there is certain advantage.
The present invention by wetland plant reed straw under the environment of low temperature (350 DEG C) hypoxemia after pyrolysis, be prepared into reed charcoal, form abundant pore structure, again charcoal is mixed with ferric chloride solution and dry after-baking, iron is immobilized on charcoal with the form of bloodstone, the preparation technology of whole dephosphorization adsorbent is simple, and condition is easy to control, is applicable to industrial production.And reed wide material sources, abundant raw materials, iron chloride reagent belongs to general chemical product, cheap.The preparation process technique of whole iron modification absorption is simple, cost is low, without the need at substantial manpower financial capacity.
Further, after adsorption treatment, Separation of Solid and Liquid is carried out, salvage out from phosphorus-containing wastewater by adsorbent, adsorbent is now rich in abundant phosphorus and ferro element, can be applied in soil, increase fertility to soil, the special structure of charcoal itself is also a kind of excellent soil conditioner.The utilization that the present invention is not only reed sediment substrate provides new approach, the process additionally using simple low cost prepares efficient dephosphorization adsorbent, and use secondary cycle absorption method secondary to utilize adsorbent, finally, using the adsorbent after use as soil conditioner, reed sediment substrate is turned waste into wealth, realizes recycling, dephosphorization adsorbent of the present invention and dephosphorization process be a kind of simply, at a low price, efficiently, the invention of environmental protection.
the bibliography inventory quoted as proof:
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Claims (8)
1. a preparation method for iron modification reed charcoal, the preparation process of the method is as follows:
(1) first pretreatment is carried out to reed straw;
(2) reed pretreated for step (1) is carried out pyrolysis charring;
(3) charcoal that step (2) pyrolysis charring obtains is cooled to room temperature, ground 10-50 mesh sieve, with water cleaning several, removes surperficial ash content, dry for standby;
(4) FeCl is got
3soluble in water, add the charcoal of drying in step (3) and stir and evenly mix, keep iron charcoal mass ratio to be 0.56-1:1; Being placed in baking oven at the temperature of 85-105 DEG C keeps 6-12h, by moisture evaporate to dryness, then at 300-500 DEG C of heat treatment 2h; It is neutrality that taking-up washes with water to washing lotion, dries 6-12h, obtain iron modification reed charcoal finished product at the temperature of 85-105 DEG C.
2. the preparation method of iron modification reed charcoal according to claim 1, wherein, pretreatment in step (1), wash the reed of harvesting with water surface dirt, then put by clean reed and dry to constant weight in 85-105 DEG C in an oven, the section that taking-up is broken into 0.5-1cm long is for subsequent use.
3. the preparation method of iron modification reed charcoal according to claim 1, wherein, in step (2), pyrolysis temperature is 300-500 DEG C, and raising speed temperature is 15 DEG C/min, keeps 4-8h.
4. the preparation method of iron modification reed charcoal according to claim 1, wherein, in step (3), oven dry is dry in 90-100 DEG C of baking oven.
5. the preparation method of iron modification reed charcoal according to claim 1, wherein, in step (4), heat treatment temperature is 350-450 DEG C.
6. the iron modification reed charcoal for preparing of the arbitrary described method of claim 1-5.
7. the application of the modification reed charcoal described in claim 6 in process low-concentration phosphorus-containing wastewater.
8. apply according to claim 7, be mainly used in low-concentration phosphorus-containing wastewater process that concentration range is 1-4mg/L and advanced treatment of wastewater.
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