CN104628073A - Method for preparing nano-iron used in wastewater treatment - Google Patents
Method for preparing nano-iron used in wastewater treatment Download PDFInfo
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- CN104628073A CN104628073A CN201510044175.7A CN201510044175A CN104628073A CN 104628073 A CN104628073 A CN 104628073A CN 201510044175 A CN201510044175 A CN 201510044175A CN 104628073 A CN104628073 A CN 104628073A
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Abstract
The invention discloses a method for preparing nano-iron used in wastewater treatment. The method comprises the following steps of firstly pulverizing aqueous anaerobically digested dried sludge, grinding, placing the ground sludge in deionized water, heating in a water bath and repeating for three times, mixing the filtrates and adjusting the pH to 8.5 to obtain an organic substance solution; adding diluted sulfuric acid according to a capacity ratio of (0.1-0.5): 1, heating in a water bath and adjusting the pH to 9 to obtain a reduced organic substance solution; preparing a ferric salt acid leaching filtrate from steel pickling wastewater sludge; mixing the reduced organic substance solution and the ferric salt acid leaching filtrate according to a capacity ratio of (1.3-15): 1, stirring, carrying out suction filtration, washing, and transferring a precipitate into a vacuumed container to obtain nano-iron. The method is used for removing dyes and multiple heavy metals in water, the removal rate of the heavy metals is 86-92%, the removal rate of COD is 85% and the removal rate of chromaticity in the wastewater is 97.65%.
Description
Technical field
The invention relates to wastewater treatment and city and industrial sludge process, particularly relate to a kind of method adopting sewage anaerobic digestion mud and steel pickling waste liquor mud to prepare the Nanoscale Iron of use in waste water treatment, this Nanoscale Iron can remove dyestuff and various heavy in water simultaneously.
Background technology
The solid waste that municipal sludge is city domestic sewage, produce in During Industrial Wastewater Treatment Process is the regular product of municipal sewage plant.In municipal sludge, water ratio is high, has parasitic ovum and pathogenic micro-organism etc., if do not dealt carefully with, discharging arbitrarily, producing serious secondary pollution by environment.
Process and the disposal options of city sewage and sludge routine mainly contain: sludge composting, sludge digestion, Sludge landfill, sludge incineration and mud fill out sea etc.
The developed countries such as America and Europe are in the construction of sewage work, and the investment of municipal sludge process, disposal accounts for the 50-70% of gross investment, and China only has 20-50%.Quickening along with Urbanization in China and the pay attention to day by day to environment protection, the quantity of municipal sewage plant increases sharply, and there is a sharp increase in output to cause sewage sludge.It is estimated, the sludge quantity (dry weight) that municipal sewage plant of current China discharges every year is approximately 1,300,000 tons, and annual growth is greater than 10%, particularly in the higher several city of Chinese Urbanization level and area, sewage sludge problem of outlet is very outstanding.
Pickling iron and steel in iron and steel and iron and steel products plant and produce a large amount of pickling waste waterss.In order to protection of the environment, save and make rational use of resources, Chinese scholars has carried out some researchs to pickling waste waters process, mainly adopts one-step calcinations, hydrochlorate partition method and oxidation neutralisation etc. to reclaim iron resources in pickling waste waters.
At present, some iron and steel enterprises still adopt traditional treatment process, namely lime, carbide slag or calcium hydroxide is generally adopted to carry out neutralizing treatment to it, produce a large amount of mud simultaneously, and the mud reprocessing produced is more difficult, take a large amount of soils, and cause the waste of secondary pollution and resource.Along with the raising of China's iron and steel output and quality, the quantity of pickling waste waters increases sharply, and the problem of outlet of pickling waste water sludge is very outstanding.
The Nanoscale Iron particle diameter of chemosynthesis is little, specific surface area is large, adsorbable pollutent is also reduced, be widely used in the in-situ immobilization of underground water and soil pollution, its repairing performance is superior, but due to the specific surface area of Nanoscale Iron large, very easily reunite, and the Zero-valent Iron wherein playing reductive action is easily oxidized in the environment, affects it and repair the stability polluted.In addition, chemosynthesis Nanoscale Iron will use a large amount of chemical reagent, and cost is very high.Therefore, research and development have the new direction that anti-agglomeration and oxidation resistant low cost Nanoscale Iron become development nano-iron material.
Because anaerobic digestion in municipal sludge is also containing the organism such as rich in protein, oligose, organic concentration is generally 60-70%, and the present inventor finds the molysite that can be extracted by chemical method in steel pickling waste liquor mud in the research in early stage.Therefore; the organism such as the protein in anaerobically digested sludge, oligose are converted into reducing sugar; in order to the molysite reduced in steel pickling waste liquor mud; the Nanoscale Iron containing Zero-valent Iron can be prepared; this Nanoscale Iron can be combined with Nanoscale Iron due to groups such as the hydroxyls on reducing sugar, makes nano iron particles mutually exclusive and not easily reunites, can reduce again the probability that the oxygen in Nanoscale Iron and environment reacts; play good shield effectiveness, improve the anti-agglomeration of Nanoscale Iron and anti-oxidant.And be raw material with solid waste sewage sludge and steel pickling waste liquor mud, the manufacturing cost of Nanoscale Iron can be reduced, and use it for and remove Wastewater Dyes and various heavy simultaneously, reach the object of the treatment of wastes with processes of wastes against one another.
Summary of the invention
The object of the invention is for existing Nanoscale Iron, easy gathering, the deficiency that oxidation-resistance is poor and manufacturing cost is high, the present invention extracts organism in anaerobically digested sludge first, it can be used as reductive agent to reduce the molysite extracted from steel pickling waste liquor mud and prepare Nanoscale Iron, to realize the removal to Wastewater Dyes and various heavy.
The present invention is achieved by following technical proposals.
For a preparation method for the Nanoscale Iron of wastewater treatment, there are following steps:
1. organism in anaerobically digested sludge is extracted
By water ratio be 40% anaerobic digestion dewatered sludge pulverize, be ground to the particle of particle diameter 1mm, be placed in deionized water, the mass ratio of dewatered sludge and deionized water is 1:25, then at 60 ~ 100 DEG C heating in water bath 3 ~ 6h, filter, reservation filtrate;
Residue after filter is repeated above-mentioned heating in water bath 2 times, and all filtrate mixed, add the sodium hydroxide solution of 3mol/L, adjust ph is 8.5, obtains organic solution, cools in vacuum drier, for subsequent use;
2. reduce extract organism
The dilute sulphuric acid of 2mol/L will be added in the step 1. middle organic solution extracted, the volume ratio of the dilute sulphuric acid of organic solution and 2mol/L is 0.1 ~ 0.5:1, heating in water bath 30min ~ 2h at 50 DEG C, be 9 by the sodium hydroxide solution adjust ph of 3mol/L again, obtain the organic solution reduced, be placed in Vacuum refrigerator 4 DEG C preservation;
3. the molysite in steel pickling waste liquor mud is extracted
Steel pickling waste liquor mud is dried 12h in 105 DEG C, obtains the steel pickling waste liquor mud of mummification, grinding, cross 100 mesh sieves; Again by mummification, sieve after steel pickling waste liquor mud immerse concentration be in the hydrochloric acid of 3mol/L, the steel pickling waste liquor mud of mummification and the mass ratio of hydrochloric acid are 0.5 ~ 5:1, normal temperature dipping 60min, and filtering separation obtains the acidleach filtrate of molysite;
4. Nanoscale Iron is prepared
In encloses container by step 2. in the acidleach filtrate of organic solution and step 3. middle molysite of reduction mix, the volume ratio of the acidleach filtrate of organic solution and molysite is 1.3 ~ 15:1, stir 15min, obtain black precipitate and be Nanoscale Iron, suction filtration, use the rapid washing precipitation of 90% ethanol 3 times again, precipitation is proceeded in vacuum-pumping container, obtain Nanoscale Iron.
Described step bath temperature is 1. 80 DEG C, heating in water bath 4h.
The volume ratio of the dilute sulphuric acid of described step organic solution 2. and 2mol/L is 0.2:1, heating in water bath 1h.
The described step 3. steel pickling waste liquor mud of mummification and the mass ratio of 3mol/L hydrochloric acid is 2.5:1.
Described by step 2. in reduction organic solution and step 3. middle acidleach filtrate mix, the volume ratio of the acidleach filtrate of organic solution and molysite is 5:1.
Beneficial effect of the present invention: adopt sewage anaerobic digestion mud and steel pickling waste liquor mud to prepare Nanoscale Iron first, and use it for the removal of dyestuff and various heavy in water.The clearance that the clearance of heavy metal in waste water of the present invention reaches 86 ~ 92%, COD is 85%, and in waste water, the clearance of colourity is 97.65%.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Raw material of the present invention sewage sludge used is from sewage work.
Embodiment 1
1. organism in anaerobically digested sludge is extracted
By water ratio be 40% anaerobic digestion dewatered sludge pulverize, be ground to the particle of particle diameter 1mm, be placed in deionized water, the mass ratio of dewatered sludge and deionized water is 1:25, then at 60 DEG C heating in water bath 6h, filter, reservation filtrate;
Residue after filter is repeated above-mentioned heating in water bath 2 times, and all filtrate mixed, add the sodium hydroxide solution of 3mol/L, adjust ph is 8.5, obtains organic solution, cools in vacuum drier, for subsequent use;
2. reduce extract organism
The dilute sulphuric acid of 2mol/L will be added in the step 1. middle organic solution extracted, the volume ratio of the dilute sulphuric acid of organic solution and 2mol/L is 0.1:1, heating in water bath 2h at 50 DEG C, be 9 by the sodium hydroxide solution adjust ph of 3mol/L again, obtain the organic solution reduced, be placed in Vacuum refrigerator 4 DEG C preservation;
3. the molysite in steel pickling waste liquor mud is extracted
Steel pickling waste liquor mud is dried 12h in 105 DEG C, obtains the steel pickling waste liquor mud of mummification, grinding, cross 100 mesh sieves; Again by mummification, sieve after steel pickling waste liquor mud immerse concentration be in the hydrochloric acid of 3mol/L, the steel pickling waste liquor mud of mummification and the mass ratio of hydrochloric acid are 0.5:1, normal temperature dipping 60min, and filtering separation obtains the acidleach filtrate of molysite;
4. Nanoscale Iron is prepared
In encloses container by step 2. in the acidleach filtrate of organic solution and step 3. middle molysite of reduction mix, the volume ratio of the acidleach filtrate of organic solution and molysite is 1.3:1, stir 15min, obtain black precipitate and be Nanoscale Iron, suction filtration, use the rapid washing precipitation of 90% ethanol 3 times again, precipitation is proceeded in vacuum-pumping container, obtain Nanoscale Iron.
The Wastewater Dyes of embodiment 1 and the detection of heavy metals removal effect:
Preparing methylene blue concentration is respectively (20mg/L) and several heavy metal Cu
2+(concentration is 15mg/L), Zn
2+(concentration is 40mg/L), Pb
2+(concentration is 40mg/L) and Cd
2+the simulation composite waste of (concentration is 40mg/L), regulate its pH value for neutral, respectively add 0.5g Nanoscale Iron wherein again, vibrate under room temperature 1h, filter, by the concentration of atomic absorption spectrometry heavy metal ions in wastewater, adopt the COD of potassium dichromate process wastewater measurement, by colourity in chromascope test waste water.
Wherein α
0-remove front heavy metal in waste water concentration mg/L, COD value and colourity
α
i-remove rear heavy metal in waste water concentration mg/L mg/L, COD value and colourity
The removal effect calculating heavy metal in waste water and methylene blue refers to table 1.(removal effect of table Methylene Blue expresses with the clearance of COD and colourity)
Table 1
| Heavy metal | Zn(II) | Cu(II) | Pb(II) | Cr(VI) | COD | Colourity |
| Clearance/% | 71.26 | 75.23 | 81.62 | 85.76 | 76.83 | 75.29 |
Embodiment 2
1. organism in anaerobically digested sludge is extracted
By water ratio be 40% anaerobic digestion dewatered sludge pulverize, be ground to the particle of particle diameter 1mm, be placed in deionized water, the mass ratio of dewatered sludge and deionized water is 1:25, then at 80 DEG C heating in water bath 4h, filter, reservation filtrate;
Residue after filter is repeated above-mentioned heating in water bath 2 times, and all filtrate mixed, add the sodium hydroxide solution of 3mol/L, adjust ph is 8.5, obtains organic solution, cools in vacuum drier, for subsequent use;
2. reduce extract organism
The dilute sulphuric acid of 2mol/L will be added in the step 1. middle organic solution extracted, the volume ratio of the dilute sulphuric acid of organic solution and 2mol/L is 0.2:1, heating in water bath 1h at 50 DEG C, be 9 by the sodium hydroxide solution adjust ph of 3mol/L again, obtain the organic solution reduced, be placed in Vacuum refrigerator 4 DEG C preservation;
3. the molysite in steel pickling waste liquor mud is extracted
Steel pickling waste liquor mud is dried 12h in 105 DEG C, obtains the steel pickling waste liquor mud of mummification, grinding, cross 100 mesh sieves; Again by mummification, sieve after steel pickling waste liquor mud immerse concentration be in the hydrochloric acid of 3mol/L, the steel pickling waste liquor mud of mummification and the mass ratio of hydrochloric acid are 2.5:1, normal temperature dipping 60min, and filtering separation obtains the acidleach filtrate of molysite;
4. Nanoscale Iron is prepared
In encloses container by step 2. in the acidleach filtrate of organic solution and step 3. middle molysite of reduction mix, the volume ratio of the acidleach filtrate of organic solution and molysite is 5:1, stir 15min, obtain black precipitate and be Nanoscale Iron, suction filtration, use the rapid washing precipitation of 90% ethanol 3 times again, precipitation is proceeded in vacuum-pumping container, obtain Nanoscale Iron.
The heavy metal in waste water of embodiment 2 and the detecting step of methylene blue removal effect are same as embodiment 1, and the removal effect being calculated heavy metal in waste water and methylene blue by detected result refers to table 2.
Table 2
| Heavy metal | Zn(II) | Cu(II) | Pb(II) | Cr(VI) | COD | Colourity |
| Clearance/% | 90.37 | 86.21 | 91.26 | 92.18 | 85.28 | 97.65 |
Embodiment 3
1. organism in anaerobically digested sludge is extracted
By water ratio be 40% anaerobic digestion dewatered sludge pulverize, be ground to the particle of particle diameter 1mm, be placed in deionized water, the mass ratio of dewatered sludge and deionized water is 1:25, then at 100 DEG C heating in water bath 3h, filter, reservation filtrate;
Residue after filter is repeated above-mentioned heating in water bath 2 times, and all filtrate mixed, add the sodium hydroxide solution of 3mol/L, adjust ph is 8.5, obtains organic solution, cools in vacuum drier, for subsequent use;
2. reduce extract organism
The dilute sulphuric acid of 2mol/L will be added in the step 1. middle organic solution extracted, the volume ratio of the dilute sulphuric acid of organic solution and 2mol/L is 0.5:1, heating in water bath 2h at 50 DEG C, be 9 by the sodium hydroxide solution adjust ph of 3mol/L again, obtain the organic solution reduced, be placed in Vacuum refrigerator 4 DEG C preservation;
3. the molysite in steel pickling waste liquor mud is extracted
Steel pickling waste liquor mud is dried 12h in 105 DEG C, obtains the steel pickling waste liquor mud of mummification, grinding, cross 100 mesh sieves; Again by mummification, sieve after steel pickling waste liquor mud immerse concentration be in the hydrochloric acid of 3mol/L, the steel pickling waste liquor mud of mummification and the mass ratio of hydrochloric acid are 5:1, normal temperature dipping 60min, and filtering separation obtains the acidleach filtrate of molysite;
4. Nanoscale Iron is prepared
In encloses container by step 2. in the acidleach filtrate of organic solution and step 3. middle molysite of reduction mix, the volume ratio of the acidleach filtrate of organic solution and molysite is 15:1, stir 15min, obtain black precipitate and be Nanoscale Iron, suction filtration, use the rapid washing precipitation of 90% ethanol 3 times again, precipitation is proceeded in vacuum-pumping container, obtain Nanoscale Iron.
The heavy metal in waste water of embodiment 2 and the detecting step of methylene blue removal effect are same as embodiment 1, and the removal effect being calculated heavy metal in waste water and methylene blue by detected result refers to table 3.
Table 3
| Heavy metal | Zn(II) | Cu(II) | Pb(II) | Cr(VI) | COD | Colourity |
| Clearance/% | 83.67 | 75.43 | 87.92 | 89.56 | 82.14 | 93.46 |
Claims (5)
1., for a preparation method for the Nanoscale Iron of wastewater treatment, there are following steps:
1. organism in anaerobically digested sludge is extracted
By water ratio be 40% anaerobic digestion dewatered sludge pulverize, be ground to the particle of particle diameter 1mm, be placed in deionized water, the mass ratio of dewatered sludge and deionized water is 1:25, then at 60 ~ 100 DEG C heating in water bath 3 ~ 6h, filter, reservation filtrate;
Residue after filter is repeated above-mentioned heating in water bath 2 times, and all filtrate mixed, add the sodium hydroxide solution of 3mol/L, adjust ph is 8.5, obtains organic solution, cools in vacuum drier, for subsequent use;
2. reduce extract organism
The dilute sulphuric acid of 2mol/L will be added in the step 1. middle organic solution extracted, the volume ratio of the dilute sulphuric acid of organic solution and 2mol/L is 0.1 ~ 0.5:1, heating in water bath 30min ~ 2h at 50 DEG C, be 9 by the sodium hydroxide solution adjust ph of 3mol/L again, obtain the organic solution reduced, be placed in Vacuum refrigerator 4 DEG C preservation;
3. the molysite in steel pickling waste liquor mud is extracted
Steel pickling waste liquor mud is dried 12h in 105 DEG C, obtains the steel pickling waste liquor mud of mummification, grinding, cross 100 mesh sieves; Again by mummification, sieve after steel pickling waste liquor mud immerse concentration be in the hydrochloric acid of 3mol/L, the steel pickling waste liquor mud of mummification and the mass ratio of hydrochloric acid are 0.5 ~ 5:1, normal temperature dipping 60min, and filtering separation obtains the acidleach filtrate of molysite.
4. Nanoscale Iron is prepared
In encloses container by step 2. in the acidleach filtrate of organic solution and step 3. middle molysite of reduction mix, the volume ratio of the acidleach filtrate of organic solution and molysite is 1.3 ~ 15:1, stir 15min, obtain black precipitate and be Nanoscale Iron, suction filtration, use the rapid washing precipitation of 90% ethanol 3 times again, precipitation is proceeded in vacuum-pumping container, obtain Nanoscale Iron.
2. the preparation method of a kind of Nanoscale Iron for wastewater treatment according to claim 1, is characterized in that, described step bath temperature is 1. 80 DEG C, heating in water bath 4h.
3. the preparation method of a kind of Nanoscale Iron for wastewater treatment according to claim 1, is characterized in that, the volume ratio of the dilute sulphuric acid of described step organic solution 2. and 2mol/L is 0.2:1, heating in water bath 1h.
4. the preparation method of a kind of Nanoscale Iron for wastewater treatment according to claim 1, is characterized in that, the described step 3. steel pickling waste liquor mud of mummification and the mass ratio of 3mol/L hydrochloric acid is 2.5:1.
5. the preparation method of a kind of Nanoscale Iron for wastewater treatment according to claim 1, it is characterized in that, described by step 2. in reduction organic solution and step 3. middle acidleach filtrate mix, the volume ratio of the acidleach filtrate of organic solution and molysite is 5:1.
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| CN105458294A (en) * | 2016-01-18 | 2016-04-06 | 中国科学院南海海洋研究所 | Nanometer zero-valent iron prepared from iron in acid mine wastewater and preparing method and application thereof |
| CN106392098A (en) * | 2016-10-10 | 2017-02-15 | 苏州经贸职业技术学院 | Preparation method of nanometer silver hydrosol and treatment method for dye wastewater |
| CN111663044A (en) * | 2020-05-14 | 2020-09-15 | 中冶南方工程技术有限公司 | Acid sludge and waste acid resource recovery device and process |
| CN111732085A (en) * | 2020-05-14 | 2020-10-02 | 中冶南方工程技术有限公司 | Acid sludge and waste acid integrated recovery device and process |
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