CN101862637B - Method absorbing lead ions in sewage with tremolite amianthine - Google Patents
Method absorbing lead ions in sewage with tremolite amianthine Download PDFInfo
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- CN101862637B CN101862637B CN201010203551XA CN201010203551A CN101862637B CN 101862637 B CN101862637 B CN 101862637B CN 201010203551X A CN201010203551X A CN 201010203551XA CN 201010203551 A CN201010203551 A CN 201010203551A CN 101862637 B CN101862637 B CN 101862637B
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- suede
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Abstract
The invention relates to a method absorbing lead ions in sewage with tremolite amianthine. The tremolite amianthine mineral containing calcium magnesium alkaline earth metal silicate is calcinated, smashed and sieved and then reacts with ferric chloride to generate tremolite amianthine sorbent which is used to remove the lead ions in the sewage with 50-150mg/L lead compound. The tremolite amianthine sorbent is oscillated for 30 to 60'in water bath with the ph value of 6 to 8 and the constant temperature of 20 to 25 degrees centigrade and the removing rate of the lead ions in the sewage is 99.7 to 100 percent. When the lead compound concentration of the sewage is 50 to 200 mg/L, the tremolite amianthine sorbent has linear correlation with the sewage. After absorbing the metal sewage, the tremolite amianthine sorbent prepared through the invention can be regenerated and reused. The tremolite amianthine sorbent has the advantages of simple preparation technology, low cost and convenient popularization and application and accords with the requirement of environmental protection, saving energy and low carbon economy.
Description
Technical field
The present invention relates to sewage disposal, remove the method for lead ion in the trade effluent especially with tremolite down material.
Background technology
Along with developing rapidly of China's industry, serious environmental is polluted many rivers, lake and phreatic water quality is worsened day by day, electroplates, makes a large amount of heavy metal ion-containing waste waters of the annual discharging of industries such as grass, chemical industry; It is maximum to biotic environment and human survival harm to contain heavy metal such as Pb, Cd, Hg; Particularly China's electric motor car industry fast development, the lead-acid battery of scrapping has increased the weight of the lead contamination of the surface water, causes lead ion to China's ecological environment severe contamination; Produce the human body lead poisoning; Lead ion can combine with plurality of enzymes in the human body, thereby disturbs human body normal biochemical physiological function, especially disturbs nerve, blood and digestive system; Particularly children ' s lead poisoning influences normal development and dysnoesia.Environmental pollution conventional method for lead is that lead waste water is adopted neutralization precipitation, ion-exchange, electrolysis and liquid film infiltration etc., and these method costs of material are high, and expense is big, is difficult to apply.
China environmental protection research department and environmental science universities and colleges have carried out Pb in the waste water in the face of serious lead contamination diffusion problem
+The processing of ion is studied, and reports for work like " Chinese Mining Industry " 2007. the 2nd phases and handles lead waste water research, Pb in the waste water with Acidic Bentonite
+Clearance reach 99.6%, " University Of Nanhua's journal " 2005.19 (1) handled the research of heavy metal wastewater thereby with hydroxyapatite bioactive material, makes the Pb in the heavy metal wastewater thereby
+Ion concentration reaches 0.012-0.033mg/L.
Summary of the invention
The technical problem that the present invention will solve is to utilize abundant, the low-cost advantage of tremolite suede ore reserves, and lead ion in the sewage is adsorbed research, seeks feasible process, reduces the cost of processing lead contamination, realizes applying, and improves living environment.
Tremolite suede preparation of adsorbent method, its characteristic may further comprise the steps:
A, tremolite suede is put in the electric drying oven with forced convection 100～110 ℃ of roasting temperatures 3～4 hours, is cooled to room temperature, grind after 80～100 orders sieve tremolite suede powder;
B, with the ferric chloride solution of above-mentioned tremolite suede powder and 0.05～0.10mol/L by tremolite suede powder: ferric chloride solution=2～3: 100 weight ratios are mixed, and 300 times/minute constant-temperature shaking suction filtration after 20～24 hours is with distilled water washing leaching cake 2～3 times;
C, above-mentioned washing and filtering cake is placed in 140～150 ℃ of air dry ovens of temperature dried 1～2 hour;
D, the above-mentioned filter cake that will pass through oven dry are pulverized and are ground, and 80～100 orders sieve and promptly get tremolite suede adsorbent.
The method of lead ion in the tremolite suede sorbent treatment sewage; Its characteristic may further comprise the steps: getting leadedization thing is the sewage 100ml of 50～150mg/L, adds tremolite suede powder 0.2～0.5g, regulates pH value to 6～8; 20～25 ℃ of constant temperature water bath vibrations 30～60 minutes; After the centrifugal filtration, get supernatant and carry out the atomic spectrophotometer measurement, the lead ion clearance is 99.7～100% in the sewage.
The renovation process of tremolite suede adsorbent is characterized in that following steps:
The tremolite suede adsorbent that adsorbed metal ion with clear water washing 2～3 times, is used the H of 0.1～0.5mol/L again
2SO
4Washing was soaked 12～24 hours, and whenever at a distance from vibration in 6 hours 1～5 minute, using pure water to be washed till the solution pH value then was 6～8, after the filtration filter residue is placed 110～120 ℃ of oven for drying 3～4 hours, ground back 80～100 orders and sieved, and promptly got the tremolite suede adsorbent of regenerating.
The beneficial effect of said method of the present invention is: tremolite suede is a kind of silicate mineral of calcic magnesium alkaline-earth metal, the epigeosphere aboundresources, and it is cheap to be used to handle leaded sewage; Easy to utilize; Be that tremolite suede adsorbent preparation technology is simple, easy to operate again, and adsorption rate is high; Also can repeatedly regenerate and use repeatedly, meet energy-conservation low charcoal economic requirement.
Description of drawings
Fig. 1 is a tremolite suede adsorbent sem photograph.
Fig. 2 is the absorption figure of tremolite suede adsorbent under different temperatures.
Fig. 3 is the absorption figure of tremolite suede adsorbent under different PH.
Fig. 4 is the adsorbance of tremolite suede adsorbent to different lead concentrations.
The specific embodiment
The silicate mineral of tremolite suede series containing calcium magnesium alkaline-earth metal is rich in SiO2, CaO, and MgO is a kind of silicate mineral of double-stranded shape structure.Its theoretical (w%): CaO 13.8 that forms, MgO 24.6, SiO
258.8, H
2O 2.8; Be complete isomorphism between Mg, the Fe; If Mg/ (Mg+Fe)>=0.90 is the tremolite; Also have a spot of Al to replace Mg, Na, K, Mn replaced C a, M9, F in the tremolite
-Replace OH
-
Chemical composition: Ca
2(Mg, Fe
2+)
5[Si
4O
11]
2(OH)
2
Chemical property: a spot of Mg in the composition, can be by Fe
+ 2Replace.
Main material specification and source
The specification of table 1 main material and source
Tester and method
Tianjin, island AA-6200 atomic spectrophotometer: adopt calibration curve method.
Constant temperature water bath oscillator, all experiments are 300 rev/mins.
Preparation of adsorbent
Get adsorbents such as a certain amount of different tremolite suede, natural zeolite, sepiolite cashmere, bentonite, kaolin, use DHG-9070A type electric drying oven with forced convection respectively 100～110 ℃ of roasting temperatures 3～4 hours; After grinding respectively, under 80～100 mesh standard sieves, sieve, can make different adsorption agent powder.
The preparation of tremolite suede adsorbent
The ferric chloride solution 100ml of preparation 0.05～0.10mol/L, the tremolite suede of getting above-mentioned 2～3g mixes with the ferric chloride solution of each concentration of 100ml, and normal temperature time shakes suction filtration after 20～24 hours with 300 times/minute oscillators.With distilled water washing leaching cake 2～3 times, filter cake is put in the air dry oven 140～150 ℃ of bakings 1～2 hour, filter cake is pulverized ground, sieve now 80～100, make tremolite suede adsorbent.
Embodiment 1: the screening of different adsorbents
Get adsorbents such as the different tremolite suede of 0.2g, natural zeolite, sepiolite cashmere, bentonite, kaolin respectively; With 100ml concentration is that the lead nitrate solution (plumbum ion concentration in the simulated wastewater) of 50mg/L is mixed; Vibration is 1 hour in the constant temperature water bath oscillator under 20 ℃ of temperature; Solution is got supernatant and is put into small test tube after centrifugal, and the AA-6200 atomic spectrophotometer carries out analyzing and testing in Tianjin, island.
The screening of table 2 optimum absorbent
Adsorbent clearance (%) adsorption capacity (mg/g)
Natural zeolite 96.62 24.13
Sepiolite cashmere 95.17 23.77
Bentonite 96.44 24.09
Kaolin 96.07 24.00
Tremolite suede 99.77 25.00
Experimental result: tremolite suede adsorbent is used for adsorbing heavy metal in water Pb, and the water after the processing can reach discharge standard, and clearance reaches more than 99%.
Embodiment 2: the confirming of adsorbent optimum amount
Get 0.1g, 0.2g, 0.5g, 1.0,1.5g, 2.0g tremolite suede adsorbent; With 100ml concentration is that the lead nitrate solution (plumbum ion concentration in the simulated wastewater) of 50mg/L is mixed; Vibration is 1 hour in the constant temperature water bath oscillator under 20 ℃ of temperature; Reaction back solution is got supernatant and is put into small test tube through centrifugal, and the AA-6200 atomic spectrophotometer carries out analyzing and testing in Tianjin, island.
The screening of table 3 optimum absorbent consumption
Adsorbent consumption (g) clearance (%)
0.1 99.32
0.2 99.77
0.5 100.00
1.0 100.00
1.5 100.00
2.0 100.00
Experimental result: tremolite suede adsorbent is used for adsorption treatment low concentration wastewater heavy metal Pb, and the optimum amount of treating capacity 100ml is 0.2g～0.5g.
Embodiment 3: the mensuration of optimal adsorption temperature and pH value
Getting 0.1g tremolite suede adsorbent and 100ml concentration and be the lead nitrate solution (plumbum ion concentration in the simulated wastewater) of 50mg/L mixes; Vibration 1 hour in the constant temperature water bath oscillator under the temperature of 20 ℃, 30 ℃, 40 ℃ and 50 ℃ respectively; Reaction back solution is got supernatant and is put into small test tube through centrifugal, and the AA-6200 atomic spectrophotometer carries out analyzing and testing in Tianjin, island; The result sees Fig. 2, and drawing the optimal adsorption temperature is 20 ℃.Under ten different PH, be that the lead nitrate solution of 50mg/L is carried out adsorption experiment with the concentration of 100ml lead nitrate solution respectively again, the optimal adsorption pH value that draws optimum absorbent is 6～8, and the result sees Fig. 3.
Experimental result shows, 20 ℃ of optimum temperatures for the absorption of tremolite suede; Under neutrallty condition, it is the most suitable to adsorb.
Embodiment 4: the mensuration of optimal adsorption concentration
Get 0.1g tremolite suede adsorbent and the concentration of 100ml lead nitrate solution and be 30,50,100,150,200,300, the lead nitrate solution (plumbum ion concentration in the simulated wastewater) of 500mg/L mixes; Vibration is 1 hour in the constant temperature water bath oscillator under 20 ℃ of temperature; Reaction back solution is through centrifugal; Get supernatant and put into small test tube, the AA-6200 atomic spectrophotometer carries out analyzing and testing in Tianjin, island.The result is as shown in Figure 4; Fig. 4 shows that tremolite suede adsorbent is 400～500mg/L to the highest adsorption concentration that contains lead solution; Maximal absorptive capacity is 250～260mg/g, and every gram tremolite suede adsorbent is linear correlation to the adsorbance of lead thing when solution concentration is 50～200mg/L.
Embodiment 5: tremolite suede sorbent treatment copper plating wastewater
Get 0.5g tremolite suede adsorbent and mix with the 20ml copper plating wastewater, it is neutral regulating pH value, and vibration is 1 hour in the constant temperature water bath oscillator under 20 ℃ of temperature; Reaction back solution is through centrifugal; Get supernatant and put into small test tube, the AA-6200 atomic spectrophotometer carries out analyzing and testing in Tianjin, island, and the result lists in table four; Recording lead ion content is 0.06mg/L, can directly discharge according to national standard.
Table four
| Pb | Cr | Ni | Cu | Zn | |
| Copper plating wastewater (mg/L) | 0.30 | 1.24 | 0.74 | 24.9 | 0.18 |
| Handle back (mg/L) | 0.06 | 0.37 | 0.17 | 6.27 | 0 |
Embodiment 6: the zinc-plated waste water of tremolite suede sorbent treatment
Getting 0.5g tremolite suede adsorbent mixes with the zinc-plated waste water of 20ml; It is neutral regulating pH value, and vibration is 1 hour in the constant temperature water bath oscillator under 20 ℃ of temperature, and reaction back solution is through centrifugal; Get supernatant and put into small test tube, the AA-6200 atomic spectrophotometer carries out analyzing and testing in Tianjin, island; Collect this clear liquid, add 0.5g tremolite suede adsorbent (regulating suspension pH for neutral) again, recording lead ion content is 0.57mg/L, and the result sees table five, can directly discharge according to national standard.
Table five
| Pb | Cr | Ni | Cu | Zn | |
| Zinc-plated waste water (mg/L) | 183 | 67.5 | 7.8 | 24 | 172 |
| After the single treatment (mg/L) | 25.5 | 27.5 | 6.5 | 20.5 | 147.5 |
| Handle back (mg/L) 2 times | 0.57 | 10.0 | 4.3 | 16.5 | 121.0 |
Embodiment 7: tremolite suede adsorbent adsorbs Pb2+, Co2+, Cd2+, Ni2+, Cu2+ simultaneously
Plumbi nitras, nickel nitrate, the nitric acid of getting 0.5g tremolite suede adsorbent and 100ml concentration and be 50mg/L is separated, the mixed solution of copper nitrate, cobalt nitrate; It is neutral regulating pH value; Vibrate half an hour in the constant temperature water bath oscillator under 20 ℃ of temperature; Reaction back solution is got supernatant and is put into small test tube through centrifugal, and the AA-6200 atomic spectrophotometer carries out analyzing and testing in Tianjin, island.The result sees that table six shows, tremolite suede adsorbent is all very high to the adsorption capacity of lead, copper and cadmium.
Table six
| Pb | Co | Ni | Cd | Cu | |
| Before handling (mg/L) | 50 | 50 | 50 | 50 | 50 |
| Handle back (mg/L) | 1.32 | 35.59 | 16.42 | 6.63 | 12.24 |
| Clearance (%) | 97.36 | 28.82 | 67.16 | 86.74 | 75.52 |
Embodiment 8: tremolite suede adsorbent adsorbs Pb2+, Co2+, Cd2+, Ni2+, Cu2+ simultaneously
Plumbi nitras, nickel nitrate, the nitric acid of getting 0.5g tremolite suede adsorbent and 100ml concentration and be 50mg/L is separated, the mixed solution of copper nitrate, cobalt nitrate; It is neutral regulating pH value; Vibrated 30～60 minutes in the constant temperature water bath oscillator under 20～25 ℃ of temperature; Solution is got supernatant and is put into small test tube through centrifugal after the adsorption reaction, and the AA-6200 atomic spectrophotometer carries out analyzing and testing in Tianjin, island.The result sees table seven, and tremolite suede adsorbent all increases than the absorption of natural tremolite suede to plumbous and cadmium to the adsorption capacity of plumbous and cadmium.
Table seven
| Pb | Co | Ni | Cd | Cu | |
| Before handling (mg/L) | 50 | 50 | 50 | 50 | 50 |
| Handle back (mg/L) | 0.15 | 25.90 | 11.19 | 4.88 | 7.14 |
| Clearance (%) | 99.70 | 48.20 | 77.62 | 90.25 | 85.73 |
Embodiment 9: the regeneration of tremolite suede adsorbent
With clear water washing 2～3 times, with H2SO4 washing, the immersion 12～24h of 0.1～0.5mol/L, every separated 6h vibration 1～5 minute is washed till solution pH value 6～8 with pure water then, filters with the tremolite suede that adsorbed Pb2+, Co2+, Cd2+, Ni2+, Cu2+; With 110～120 ℃ of oven dry of filter cake, 3～4h, grind 80～100 orders and sieve, promptly get the tremolite suede adsorbent of regenerating.
Get the mixed solution of tremolite suede and 100ml plumbi nitras after the 0.5g regeneration, nickel nitrate, cadmium nitrate, copper nitrate, cobalt nitrate; It is neutral regulating pH value; Vibrated 30～60 minutes in the constant temperature water bath oscillator under 20～25 ℃ of temperature; Absorption back solution separates through filtering, and gets supernatant and puts into small test tube, and the AA-6200 atomic spectrophotometer carries out analyzing and testing in Tianjin, island.The result sees table eight, can know that by table the tremolite suede that adsorbed Pb2+, Co2+, Cd2+, Ni2+, Cu2+ is after Regeneration Treatment, and plumbum ion concentration reaches discharging standards, can repeat to do adsorbent and use.
Table eight
| Pb | Co | Ni | Cd | Cu | |
| Before handling (mg/L) | 50 | 50 | 50 | 50 | 50 |
| Handle back (mg/L) | 0.75 | 23.80 | 10.55 | 3.56 | 6.20 |
| Regeneration back clearance (%) | 98.50 | 52.40 | 78.90 | 92.88 | 87.60 |
Claims (3)
1. tremolite suede preparation of adsorbent method, the silicate mineral of said tremolite suede series containing calcium magnesium alkaline-earth metal is rich in SiO
2, CaO and MgO, be a kind of silicate mineral of double-stranded shape structure, its tremolite suede preparation of adsorbent method may further comprise the steps:
A, tremolite suede is put in the electric drying oven with forced convection 100～110 ℃ of roasting temperatures 3～4 hours, is cooled to room temperature, grind after 80～100 orders sieve tremolite suede powder;
B, with the ferric chloride solution of above-mentioned tremolite suede powder and 0.05～0.10mol/L by tremolite suede powder: ferric chloride solution=2～3: 100 weight ratios are mixed, and 300 times/minute constant-temperature shaking suction filtration after 20～24 hours is with distilled water washing leaching cake 2～3 times;
C, the filter cake after distilled water washing among the step b is placed in 140～150 ℃ of air dry ovens of temperature dried 1～2 hour;
D, will be in step c dried filter cake pulverize and grind, 80～100 orders sieve and promptly get tremolite suede adsorbent.
2. the method for lead ion in the tremolite suede sorbent treatment sewage of method preparation according to claim 1; Its characteristic may further comprise the steps: getting leadedization thing is the sewage 100ml of 50～150mg/L, adds tremolite suede adsorbent 0.2～0.5g, regulates pH value to 6～8; 20～25 ℃ of constant temperature water bath vibrations 30～60 minutes; After the centrifugal filtration, get supernatant and carry out the atomic spectrophotometer measurement, the lead ion clearance is 99.7～100% in the sewage.
3. method as claimed in claim 2 is characterized in that the renovation process of tremolite suede adsorbent may further comprise the steps: the tremolite suede adsorbent that will adsorb metal ion is used the H of 0.1～0.5mol/L again with clear water washing 2～3 times
2SO
4Washing was soaked 12～24 hours, and whenever at a distance from vibration in 6 hours 1～5 minute, using pure water to be washed till the pH value of solution value then was 6～8, after the filtration filter residue is placed 110～120 ℃ of oven for drying 3～4 hours, ground back 80～100 orders and sieved, and promptly got the tremolite suede adsorbent of regenerating.
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| CN103949202B (en) * | 2014-05-16 | 2016-08-24 | 宁波工程学院 | A kind of PTA process for treating industrial waste water |
| CN105797713B (en) * | 2015-12-28 | 2018-09-25 | 河北科技大学 | A kind of preparation method of metal-modified amphibole catalyst |
| CN115448357B (en) * | 2022-10-31 | 2023-10-27 | 中国地质大学（武汉） | Method for synthesizing lead halide perovskite by recycling lead ions in aqueous solution |
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Non-Patent Citations (2)
| Title |
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| 李梦耀等.膨润土的改性研究及其应用.《长安大学学报（地球科学版）》.2003,第25卷(第2期),第76页第1.2节. * |
| 罗道成等.改性膨润土的制备及其对电镀废水中Pb2+、Cr3+、Ni2+的吸附性能研究.《中国矿业》.2003,第12卷(第11期),第54页右栏第1段、第55页左栏第2段及表1、表2及表5. * |
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