CN101186357A - Method for deep purifying heavy metal micro-polluted water by resin-base nano hydrated ferric oxide - Google Patents
Method for deep purifying heavy metal micro-polluted water by resin-base nano hydrated ferric oxide Download PDFInfo
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- CN101186357A CN101186357A CNA2007101913553A CN200710191355A CN101186357A CN 101186357 A CN101186357 A CN 101186357A CN A2007101913553 A CNA2007101913553 A CN A2007101913553A CN 200710191355 A CN200710191355 A CN 200710191355A CN 101186357 A CN101186357 A CN 101186357A
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- heavy metal
- resin
- ferric oxide
- hydrated ferric
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- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 96
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 85
- LDHBWEYLDHLIBQ-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide;hydrate Chemical compound O.[OH-].[O-2].[Fe+3] LDHBWEYLDHLIBQ-UHFFFAOYSA-M 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 18
- 229920005989 resin Polymers 0.000 claims abstract description 91
- 239000011347 resin Substances 0.000 claims abstract description 91
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000010521 absorption reaction Methods 0.000 claims abstract description 3
- 238000003795 desorption Methods 0.000 claims description 78
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 63
- 238000001179 sorption measurement Methods 0.000 claims description 33
- 239000002585 base Substances 0.000 claims description 23
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 21
- 150000002500 ions Chemical class 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- 229920001429 chelating resin Polymers 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 230000008929 regeneration Effects 0.000 claims description 2
- 238000011069 regeneration method Methods 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 abstract description 2
- 150000001768 cations Chemical class 0.000 abstract 2
- -1 Na<+> Chemical class 0.000 abstract 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract 1
- 239000003729 cation exchange resin Substances 0.000 abstract 1
- 230000002860 competitive effect Effects 0.000 abstract 1
- 239000008187 granular material Substances 0.000 abstract 1
- 229910017604 nitric acid Inorganic materials 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 24
- 239000011521 glass Substances 0.000 description 21
- 230000008676 import Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000011068 loading method Methods 0.000 description 2
- VAOCPAMSLUNLGC-UHFFFAOYSA-N metronidazole Chemical compound CC1=NC=C([N+]([O-])=O)N1CCO VAOCPAMSLUNLGC-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a method of deeply purifying heavy metal micro-polluted water body through resin-based nano hydrated ferric oxide, which pertains to the technical field of water environmental treatment. The steps are: nano hydrated ferric oxide granules are supported on cation exchange resin so as to generate the resin-based nano hydrated ferric oxide materials; the water micro-polluted by the heavy metal passes through an absorption column which is filled with the resin-based nano hydrated ferric oxide or the heavy metal micro-polluted water and the resin-based nano hydrated ferric oxide are mixed in a container and then are vibrated before being centrifugally dried; the absorbed resin-based nano hydrated ferric oxide can be desorbed by acid fluid such as HC1or HNO3 solution etc. or can be desorbed and regenerated by EDTA solution. When a great number of cations such as Na<+>, k<+>, Ca<2+>, Mg<2+>, etc. exist in the polluted water, the invention still can reduce and lead the effluent heavy metal concentration to meet safety control standard; when a great number of competitive cations coexist in the heavy metal micro-polluted water, the effluent heavy metal concentration can be reduced to meet the safety control standard with very large treatment capacity.
Description
Technical field
The present invention relates to utilize the method for resin-base nano hydrated ferric oxide deep purifying heavy metal micro-polluted water body, a kind of utilization of saying so more specifically has high-adsorption-capacity very and the resin-base nano hydrated ferric oxide technology of coming the deep purifying heavy metal micro-polluted water body optionally to heavy metals such as lead, copper, cadmiums.
Background technology
Because the high toxicity and the effect of potential biological accumulation of heavy metal contamination, guarantee has great importance for water quality safety to realize heavy metal micro-polluted water body deep purifying, accordingly, countries in the world just at the development of new treatment technology to adapt to more harsh heavy metal safety control standard, wherein adsorption separation technology has obtained extensive concern because of characteristics such as easy and simple to handle, that universality is strong in this field, and adsorption and separation material commonly used has gac, ion exchange resin, resin, molecular sieve etc.Yet, for the heavy metal micro-polluted water body, because characteristics such as its component complexity, Pollutant levels are low, competing ions concentration height, traditional adsorption and separation material all has been subjected to stern challenge at aspects such as treatment effect, loading capacity, adsorption selectivity, regenerabilities.
Hydrous iron oxide (Hydrous Ferric Oxides) has very high adsorption selectivity energy extensively to be paid close attention to because of it to many heavy metal ion.But hydrous iron oxide generally exists with ultra-fine grain (about particle diameter 0.02-10 micron), will produce huge pressure when directly using with the fluidised form system and fall, and makes it be difficult to directly realize industrial applications.(Modeling?Pb?sorption?to?microporous?amorphous?oxides?as?discrete?particles?andcoatings，Journal?of?Colloid?and?Interface?Science，2005，281，1；Adsorption?andcoprecipitation?of?copper?with?the?hydrous?oxides?of?iron?and?aluminum，Environ.Sci.Technol.1997，31，10)。
Summary of the invention
1, invents the technical problem that will solve
The method that the purpose of this invention is to provide resin-base nano hydrated ferric oxide deep purifying heavy metal micro-polluted water body, can prepare resin-base nano hydrated ferric oxide by this method, be applied to the advanced treatment that micro heavy pollutes in surface water and the underground water, can realize the safety control of water body.
2, technical scheme
The method of resin-base nano hydrated ferric oxide deep purifying heavy metal micro-polluted water body, it may further comprise the steps:
(A). the method by liquid deposition on Zeo-karb, makes the resin-base nano hydrated ferric oxide material with the nano hydrated ferric oxide particles supported;
(B). be controlled to be 3～7 at pH, temperature is controlled to be under 5～50 ℃, with the water body that is subjected to the little pollution of heavy metal with flow be 0.5～30BV/h by being filled with the adsorption column of resin-base nano hydrated ferric oxide, the heavy metal content of water outlet can reach the safety control standard; Be mixed in according to a certain volume in the container by heavy metal micro-polluted water body and resin base hydrous iron oxide, the centrifuge dripping after 1～10 hour that vibrates, the heavy metal content of centrifuge mother liquor can reach the safety control standard;
(C). for the resin base hydrous iron oxide after the absorption, available HCl or HNO
3Acid solutions such as solution are carried out desorption, and wherein resin matrix can return steps A and applies mechanically, and add alkali lye in the desorption liquid and make heavy metal precipitation, and filtering separation; Or adopt EDTA solution to carry out desorption and regeneration.
There is a large amount of Na in the little pollution deep treatment method of common heavy metal in water
+, K
+, Ca
2+, Mg
2+During Deng positively charged ion, its treatment effect will be had a greatly reduced quality.But present method is because hydrous iron oxide (HFO) particle to high adsorption selectivity, the high adsorption efficiency of nano particle HFO and the Donnan film effect of Zeo-karb of heavy metal ion such as lead, copper, cadmium, still shows excellent treatment effect.
Its Zeo-karb can be D001 (Zhengguang Resin Co., Ltd.'s production), 001 * 7 (Jiangsu Nanda Gede Environmental Protection Technology Co., Ltd's production), D113 (Jiangsu Nanda Gede Environmental Protection Technology Co., Ltd's production), Amberlite IR 252 (U.S. Rohm Haas Co. production) resins etc., the mass percent of the iron level of load (in iron) can be controlled at 0.5～40%.
Wherein the heavy metal concentration of polluted-water can be 0.01～300mg/L, can attach most importance to 0～200 times of metal molar concentration of the volumetric molar concentration of competing ions.Wherein the volume ratio with the resin base hydrous iron oxide of polluted-water is controlled is made as 500: 1～10: 1, and Controllable Temperature is made as 5～50 ℃, and the vibration controllable rotation speed is made as 100～300rpm, and duration of oscillation is controlled to be made as 1～10 hour.Middle HCl or HNO
3The weight percent of solution is controlled to be made as 0.5～5%, and perhaps the concentration of EDTA is 1-40%, the controlled 0.5～5BV/h that is made as of the flow of desorption liquid.
3, beneficial effect
The invention provides the method for resin-base nano hydrated ferric oxide deep purifying heavy metal micro-polluted water body, method by liquid deposition loads on hydrous iron oxide prepares the resin-base nano hydrated ferric oxide material on the Zeo-karb, the present invention had both solved the high fluid resistance problem when the particulate form hydrous iron oxide is used, utilize resin surface to solidify the Donnan film effect that positive charge produces simultaneously, but strengthening material is to the adsorption selectivity and the loading capacity of heavy metal ion.In polluted-water, there is a large amount of Na
+, K
+, Ca
2+, Mg
2+During Deng positively charged ion, the present invention still can make the heavy metal concentration of water outlet be reduced to the safety control standard when coexistence in the heavy metal micro-polluted water body has a large amount of competing ions, its water outlet heavy metal concentration still can be reduced to the safety control standard, and very large treatment capacity is arranged.
Embodiment
Further specify the present invention by the following examples.
Embodiment 1:
With 50ml (about 40 gram) is that the supported quantity (with Fe) of parent and Fe is that 10% HFO-D001 packs in the glass adsorption column of strap clamp cover that (Φ 32 * 360mm), under 25 ± 5 ℃, with heavy metal micro-polluted water body (Pb in D-001
2+Concentration be 1ppm, Ca
2+Concentration be 100ppm, K
+Concentration be 100ppm, Na
+Concentration be 100ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 6, by resin bed, treatment capacity is greater than 20000BV with the flow of 500ml/h, water outlet Pb
2+Concentration drop to below the 2ppb.
Be that HCl flow following current with 100ml/h under 50 ± 5 ℃ temperature of 2% is carried out desorption by resin bed with 200ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 2:
With 50ml (about 40 gram) is that the supported quantity (with Fe) of parent and Fe is that 12% HFO-D001 packs in the glass adsorption column of strap clamp cover that (Φ 32 * 360mm), under 35 ± 5 ℃, with heavy metal micro-polluted water body (Cu in D-001
2+Concentration be 1ppm, Ca
2+Concentration be 100ppm, Na
+Concentration be 100ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 6, by resin bed, treatment capacity is greater than 10000BV with the flow of 500ml/h, water outlet Cu
2+Concentration drop to below the 2ppb.
Be that HCl flow following current with 80ml/h under 50 ± 5 ℃ temperature of 2% is carried out desorption by resin bed with 200ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 3:
With 100ml (about 79 gram) is that the supported quantity (with Fe) of parent and Fe is that 8% HFO-D001 packs in the glass adsorption column of strap clamp cover that (Φ 32 * 360mm), under 15 ± 5 ℃, with heavy metal micro-polluted water body (Cd in D-001
2+Concentration be 1ppm, Ca
2+Concentration be 100ppm, Na
+Concentration be 100ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 7, by resin bed, treatment capacity is greater than 7000BV with the flow of 500ml/h, water outlet Cd
2+Concentration drop to below the 3ppb.
Be that HCl flow following current with 200ml/h under 40 ± 5 ℃ temperature of 3% is carried out desorption by resin bed with 300ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 4:
With 100ml (about 84 gram) is that the supported quantity (with Fe) of parent and Fe is that 15% HFO-D001 packs in the glass adsorption column of strap clamp cover that (Φ 32 * 360mm), under 15 ± 5 ℃, with heavy metal micro-polluted water body (Pb in D-001
2+Concentration be 1ppm, Cd
2+Concentration be 1ppm, Cu
2+Concentration be 1ppm, Ca
2+Concentration be 100ppm, Na
+Concentration be 100ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 5, by resin bed, treatment capacity is greater than 8000BV with the flow of 2000ml/h, water outlet Pb
2+, Cd
2+, Cu
2+Concentration all drop to below the 2ppb.
Be that HCl flow following current with 100ml/h under 50 ± 5 ℃ temperature of 2% is carried out desorption by resin bed with 200ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 5:
With 100ml (about 96 gram) is that the supported quantity (with Fe) of parent and Fe is that 32% HFO-D001 packs in the glass adsorption column of strap clamp cover that (Φ 32 * 360mm), under 15 ± 5 ℃, with heavy metal micro-polluted water body (Pb in D-001
2+Concentration be 3ppm, Cd
2+Concentration be 1ppm, Cu
2+Concentration be 1ppm, Ca
2+Concentration be 100ppm, Na
+Concentration be 100ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 6, by resin bed, treatment capacity is greater than 12000BV with the flow of 2000ml/h, water outlet Pb
2+, Cd
2+, Cu
2+Concentration all drop to below the 2ppb.
With 200ml concentration 2% HNO
3Flow following current with 150ml/h under 35 ± 5 ℃ temperature is carried out desorption by resin bed, the desorption rate of heavy metal＞99.9%, and the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 6:
With 80ml (about 63 gram) is that the supported quantity (with Fe) of parent and Fe is that 8% HFO-D001 packs in the glass adsorption column of strap clamp cover that (Φ 32 * 360mm), under 15 ± 5 ℃, with heavy metal micro-polluted water body (Pb in D-001
2+Concentration be 0.5ppm, Ca
2+Concentration be 100ppm, Na
+Concentration be 100ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 4, by resin bed, treatment capacity is greater than 15000BV with the flow of 2000ml/h, water outlet Pb
2+Concentration drop to below the 2ppb.
Be that EDTA flow following current with 100ml/h under 35 ± 5 ℃ temperature of 5% is carried out desorption by resin bed with 250ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 7:
With 80ml (about 70 gram) is that the supported quantity (with Fe) of parent and Fe is that 25% HFO-D001 packs in the glass adsorption column of strap clamp cover that (Φ 32 * 360mm), under 15 ± 5 ℃, with heavy metal micro-polluted water body (Pb in D-001
2+Concentration be 1.5ppm, Ca
2+Concentration be 100ppm, Na
+Concentration be 300ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 7, by resin bed, treatment capacity is greater than 13000BV with the flow of 3000ml/h, water outlet Pb
2+Concentration drop to below the 2ppb.
Be that HCl flow following current with 150ml/h under 25 ± 5 ℃ temperature of 3% is carried out desorption by resin bed with 300ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 8:
With 80ml (about 60 gram) is that the supported quantity (with Fe) of parent and Fe is that 2.5% HFO-D001 packs in the glass adsorption column of strap clamp cover that (Φ 32 * 360mm), under 35 ± 5 ℃, with heavy metal micro-polluted water body (Pb in D-001
2+Concentration be 0.5ppm, Ca
2+Concentration be 80ppm, Na
+Concentration be 100ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 3.5, by resin bed, treatment capacity is greater than 12000BV with the flow of 1500ml/h, water outlet Pb
2+Concentration drop to below the 2ppb.
Be that HCl flow following current with 150ml/h under 25 ± 5 ℃ temperature of 3% is carried out desorption by resin bed with 300ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 9:
With 5ml (about 4 gram) is that the supported quantity (with Fe) of parent and Fe is the beaker that 8% HFO-D001 puts into 2000ml in D-001, under 20 ± 5 ℃, with 1500ml heavy metal micro-polluted water body (Pb
2+Concentration be 1ppm, Ca
2+Concentration be 120ppm, Na
+Concentration be 100ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 6, import beaker then, with 150rpm vibration centrifuging after 4 hours.Filtrate Pb
2+Concentration drop to below the 2ppb.
Be that 1% HCl adds under 30 ± 5 ℃ temperature in the resin after centrifugal with 50ml concentration, soak centrifuge dripping after 1 hour, the desorption rate of heavy metal＞99%, the resin behind aforesaid operations can use as supporting parent repeatedly.
Embodiment 10:
With 5ml (about 4 gram) is that the supported quantity (with Fe) of parent and Fe is the beaker that 12% HFO-D001 puts into 2000ml in D-001, under 30 ± 5 ℃, with 1000ml heavy metal micro-polluted water body (Pb
2+Concentration be 2ppm, Cu
2+Concentration be 1ppm, concentration be 1ppm, Ca
2+Concentration be 50ppm, Na
+Concentration be 50ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 7, import beaker then, with 200rpm vibration centrifuging after 3 hours.Filtrate Pb
2+, Cu
2+, Cd
2+Concentration all drop to below the 2ppb.
Be that 2% HCl adds under 40 ± 5 ℃ temperature in the resin after centrifugal with 50ml concentration, soak centrifuge dripping after 2 hours, the desorption rate of heavy metal＞99%, the resin behind aforesaid operations can use as supporting parent repeatedly.
Embodiment 11:
Be that the supported quantity (with Fe) of parent and Fe is that 15% HFO-001 * 7 pack in the glass adsorption column that strap clamp overlaps that (Φ 32 * 360mm), under 25 ± 5 ℃, with heavy metal micro-polluted water body (Pb into 100ml (about 80 gram) in 001 * 7
2+Concentration be 2ppm, Ca
2+Concentration be 100ppm, Na
+Concentration be 100ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 6, by resin bed, treatment capacity is greater than 12000BV with the flow of 2000ml/h, water outlet Pb
2+Concentration drop to below the 2ppb.
Be that HCl flow following current with 100ml/h under 50 ± 5 ℃ temperature of 2% is carried out desorption by resin bed with 200ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 12:
Be that the supported quantity (with Fe) of parent and Fe is that 13% HFO-001 * 7 pack in the glass adsorption column that strap clamp overlaps that (Φ 32 * 360mm), under 15 ± 5 ℃, with heavy metal micro-polluted water body (Cu into 150ml (about 120 gram) in 001 * 7
2+Concentration be 0.5ppm, Ca
2+Concentration be 100ppm, Na
+Concentration be 100ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 4, by resin bed, treatment capacity is greater than 10000BV with the flow of 2000ml/h, water outlet Cu
2+Concentration drop to below the 2ppb.
Be that HCl flow following current with 150ml/h under 45 ± 5 ℃ temperature of 4% is carried out desorption by resin bed with 200ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 13:
Be that the supported quantity (with Fe) of parent and Fe is that 2% HFO-001 * 7 pack in the glass adsorption column that strap clamp overlaps that (Φ 32 * 360mm), under 35 ± 5 ℃, with heavy metal micro-polluted water body (Cd into 150ml (about 107 gram) in 001 * 7
2+Concentration be 0.5ppm, Ca
2+Concentration be 60ppm, Na
+Concentration be 150ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 4, by resin bed, treatment capacity is greater than 5000BV with the flow of 2000ml/h, water outlet Cd
2+Concentration drop to below the 2ppb.
Be that EDTA flow following current with 150ml/h under 25 ± 5 ℃ temperature of 8% is carried out desorption by resin bed with 350ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 14:
Be that the supported quantity (with Fe) of parent and Fe is that 12% HFO-001 * 7 pack in the glass adsorption column that strap clamp overlaps that (Φ 32 * 360mm), under 25 ± 5 ℃, with heavy metal micro-polluted water body (Cu into 120ml (about 95 gram) in 001 * 7
2+Concentration be 1ppm, Cd
2+Concentration be 0.5ppm, Ca
2+Concentration be 80ppm, Na
+Concentration be 150ppm, Mg
2+Concentration be 120ppm) the pH value transfer to 7, by resin bed, treatment capacity is greater than 9000BV with the flow of 1200ml/h, water outlet Cu
2+, Cd
2+Concentration all drop to below the 3ppb.
With 200ml concentration 1% HNO
3Flow following current with 200ml/h under 25 ± 5 ℃ temperature is carried out desorption by resin bed, the desorption rate of heavy metal＞99.9%, and the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 15:
Be that the supported quantity (with Fe) of parent and Fe is that 25% HFO-001 * 7 pack in the glass adsorption column that strap clamp overlaps that (Φ 32 * 360mm), under 45 ± 5 ℃, with heavy metal micro-polluted water body (Pb into 50ml (about 43 gram) in 001 * 7
2+Concentration be 2ppm, Cd
2+Concentration be 0.5ppm, Ca
2+Concentration be 120ppm, Na
+Concentration be 150ppm, Mg
2+Concentration be 120ppm) the pH value transfer to 6, by resin bed, treatment capacity is greater than 9000BV with the flow of 1500ml/h, water outlet Pb
2+, Cd
2+Concentration all drop to below the 2ppb.
With 150ml concentration 2% HNO
3Flow following current with 80ml/h under 45 ± 5 ℃ temperature is carried out desorption by resin bed, the desorption rate of heavy metal＞99.9%, and the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 16:
Be that the supported quantity (with Fe) of parent and Fe is that 15% HFO-001 * 7 pack in the glass adsorption column that strap clamp overlaps that (Φ 32 * 360mm), under 45 ± 5 ℃, with heavy metal micro-polluted water body (Pb into 80ml (about 65 gram) in 001 * 7
2+Concentration be 1ppm, Cu
2+Concentration be 0.5ppm, Ca
2+Concentration be 120ppm, Na
+Concentration be 150ppm, Mg
2+Concentration be 120ppm) the pH value transfer to 6, by resin bed, treatment capacity is greater than 15000BV with the flow of 1500ml/h, water outlet Pb
2+, Cu
2+Concentration all drop to below the 3ppb.
Be that HCl flow following current with 100ml/h under 65 ± 5 ℃ temperature of 1% is carried out desorption by resin bed with 150ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 17:
Is that the supported quantity (with Fe) of parent and Fe is the beaker that 2000ml is put in 8% HFO-001 * 7 with 5ml (about 4 gram) in 001 * 7, under 20 ± 5 ℃, with 1500ml heavy metal micro-polluted water body (Pb
2+Concentration be 1ppm, Ca
2+Concentration be 100ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 6, import beaker then, with 150rpm vibration centrifuging after 4 hours.Filtrate Pb
2+Concentration drop to below the 2ppb.
Be that 1% HCl adds under 30 ± 5 ℃ temperature in the resin after centrifugal with 50ml concentration, soak centrifuge dripping after 1 hour, the desorption rate of heavy metal＞99%, the resin behind aforesaid operations can use as supporting parent repeatedly.
Embodiment 18:
With 100ml (about 80 gram) is that the supported quantity (with Fe) of parent and Fe is that 10% HFO-D113 packs in the glass adsorption column of strap clamp cover that (Φ 32 * 360mm), under 25 ± 5 ℃, with heavy metal micro-polluted water body (Pb in D113
2+Concentration be 1ppm, Ca
2+Concentration be 80ppm, Na
+Concentration be 150ppm, Mg
2+Concentration be 120ppm) the pH value transfer to 6, by resin bed, treatment capacity is greater than 15000BV with the flow of 800ml/h, water outlet Pb
2+Concentration all drop to below the 2ppb.
Be that HCl flow following current with 100ml/h under 55 ± 5 ℃ temperature of 1% is carried out desorption by resin bed with 150ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 19:
With 100ml (about 88 gram) is that the supported quantity (with Fe) of parent and Fe is that 25% HFO-D113 packs in the glass adsorption column of strap clamp cover that (Φ 32 * 360mm), under 25 ± 5 ℃, with heavy metal micro-polluted water body (Pb in D113
2+Concentration be 1ppm, Ca
2+Concentration be 100ppm, Na
+Concentration be 150ppm, Mg
2+Concentration be 120ppm) the pH value transfer to 6, by resin bed, treatment capacity is greater than 20000BV with the flow of 1200ml/h, water outlet Pb
2+Concentration all drop to below the 2ppb.
Be that HCl flow following current with 100ml/h under 35 ± 5 ℃ temperature of 1% is carried out desorption by resin bed with 250ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 20:
With 100ml (about 76 gram) is that the supported quantity (with Fe) of parent and Fe is that 8% HFO-D113 packs in the glass adsorption column of strap clamp cover that (Φ 32 * 360mm), under 15 ± 5 ℃, with heavy metal micro-polluted water body (Cu in D113
2+Concentration be 1ppm, Ca
2+Concentration be 100ppm, Na
+Concentration be 150ppm, Mg
2+Concentration be 120ppm) the pH value transfer to 5, by resin bed, treatment capacity is greater than 9000BV with the flow of 1500ml/h, water outlet Cu
2+Concentration drop to below the 2ppb.
With 250ml concentration 1% HNO
3Flow following current with 100ml/h under 25 ± 5 ℃ temperature is carried out desorption by resin bed, the desorption rate of heavy metal＞99.9%, and the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 21:
With 120ml (about 95 gram) is that the supported quantity (with Fe) of parent and Fe is that 12% HFO-D113 packs in the glass adsorption column of strap clamp cover that (Φ 32 * 360mm), under 35 ± 5 ℃, with heavy metal micro-polluted water body (Cd in D113
2+Concentration be 1ppm, Ca
2+Concentration be 100ppm, Na
+Concentration be 150ppm, Mg
2+Concentration be 120ppm) the pH value transfer to 4, by resin bed, treatment capacity is greater than 9000BV with the flow of 1500ml/h, water outlet Cd
2+Concentration drop to below the 3ppb.
Be that EDTA flow following current with 100ml/h under 45 ± 5 ℃ temperature of 8% is carried out desorption by resin bed with 250ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 22:
With 5ml (about 4 gram) is that the supported quantity (with Fe) of parent and Fe is the beaker that 15% HFO-D113 puts into 2000ml in D113, under 25 ± 5 ℃, with 1500ml heavy metal micro-polluted water body (Pb
2+Concentration be 2ppm, Ca
2+Concentration be 100ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 6, import beaker then, with 200rpm vibration centrifuging after 3 hours.Filtrate Pb
2+Concentration drop to below the 2ppb.
With 50ml concentration 1% HNO
3Under 40 ± 5 ℃ temperature, add in the resin after centrifugal, soaks centrifuge dripping after 2 hours, the desorption rate of heavy metal＞99%, the resin behind aforesaid operations can be repeatedly as supporting the parent use.
Embodiment 23:
With 5ml (about 4 gram) is that the supported quantity (with Fe) of parent and Fe is the beaker that 8% HFO-D113 puts into 2000ml in D113, under 25 ± 5 ℃, with 1500ml heavy metal micro-polluted water body (Cu
2+Concentration be 1ppm, Ca
2+Concentration be 100ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 4, import beaker then, with 150rpm vibration centrifuging after 4 hours.Liquor C u
2+Concentration drop to below the 2ppb.
Be that 2% HCl adds under 50 ± 5 ℃ temperature in the resin after centrifugal with 50ml concentration, soak centrifuge dripping after 1 hour, the desorption rate of heavy metal＞99%, the resin behind aforesaid operations can use as supporting parent repeatedly.
Embodiment 24:
With 80ml (about 63 gram) is that the supported quantity (with Fe) of parent and Fe is that 12% HFO-252 packs in the glass adsorption column of strap clamp cover that (Φ 32 * 360mm), under 25 ± 5 ℃, with heavy metal micro-polluted water body (Pb in Amberlite252
2+Concentration be 1ppm, Ca
2+Concentration be 100ppm, Na
+Concentration be 150ppm, Mg
2+Concentration be 120ppm) the pH value transfer to 6, by resin bed, treatment capacity is greater than 15000BV with the flow of 1500ml/h, water outlet Pb
2+Concentration drop to below the 2ppb.
Be that HCl flow following current with 40ml/h under 45 ± 5 ℃ temperature of 2% is carried out desorption by resin bed with 200ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 25:
Be that the supported quantity (with Fe) of parent and Fe is that 10% HFO-252 packs in the glass adsorption column that strap clamp overlaps that (Φ 32 * 360mm), under 25 ± 5 ℃, with heavy metal micro-polluted water body (Cu into 100ml (about 75 gram) in Amberlite 252
2+Concentration be 1ppm, Ca
2+Concentration be 100ppm, Na
+Concentration be 150ppm, Mg
2+Concentration be 120ppm) the pH value transfer to 5, by resin bed, treatment capacity is greater than 12000BV with the flow of 1000ml/h, water outlet Cu
2+Concentration drop to below the 2ppb.
Be that HCl flow following current with 90ml/h under 35 ± 5 ℃ temperature of 1% is carried out desorption by resin bed with 300ml concentration, the desorption rate of heavy metal＞99.9%, the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 26:
Be that the supported quantity (with Fe) of parent and Fe is that 15% HFO-252 packs in the glass adsorption column that strap clamp overlaps that (Φ 32 * 360mm), under 25 ± 5 ℃, with heavy metal micro-polluted water body (Pb into 80ml (about 64 gram) in Amberlite 252
2+Concentration be 1ppm, Cu
2+Concentration be 1ppm, Ca
2+Concentration be 100ppm, Na
+Concentration be 150ppm, Mg
2+Concentration be 120ppm) the pH value transfer to 5, by resin bed, treatment capacity is greater than 9000BV with the flow of 1000ml/h, water outlet Pb
2+, Cu
2+Concentration all drop to below the 2ppb.
With 200ml concentration 1% HNO
3Flow following current with 90ml/h under 35 ± 5 ℃ temperature is carried out desorption by resin bed, the desorption rate of heavy metal＞99.9%, and the resin behind the desorption can use as supporting parent repeatedly.
Embodiment 27:
Is that the supported quantity (with Fe) of parent and Fe is the beaker that 15% HFO-252 puts into 2000ml with 5ml (about 4 gram) in Amberlite 252, under 30 ± 5 ℃, with 1500ml heavy metal micro-polluted water body (Pb
2+Concentration be 2ppm, Ca
2+Concentration be 150ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 6, import beaker then, with 200rpm vibration centrifuging after 3 hours.Filtrate Pb
2+Concentration drop to below the 2ppb.
With 40ml concentration 1% HNO
3Under 40 ± 5 ℃ temperature, add in the resin after centrifugal, soaks centrifuge dripping after 2 hours, the desorption rate of heavy metal＞99%, the resin behind aforesaid operations can be repeatedly as supporting the parent use.
Embodiment 28:
Is that the supported quantity (with Fe) of parent and Fe is the beaker that 12% HFO-252 puts into 2000ml with 5ml (about 4 gram) in Amberlite 252, under 30 ± 5 ℃, with 1500ml heavy metal micro-polluted water body (Pb
2+Concentration be 2ppm, Cd
2+Concentration be 1ppm, Ca
2+Concentration be 150ppm, Mg
2+Concentration be 100ppm) the pH value transfer to 5, import beaker then, with 250rpm vibration centrifuging after 5 hours.Filtrate Pb
2+, Cd
2+Concentration all drop to below the 2ppb.
With 50ml concentration 2% HNO
3Under 25 ± 5 ℃ temperature, add in the resin after centrifugal, soaks centrifuge dripping after 3 hours, the desorption rate of heavy metal＞99%, the resin behind aforesaid operations can be repeatedly as supporting the parent use.
Claims (5)
1. the method for a resin-base nano hydrated ferric oxide deep purifying heavy metal micro-polluted water body, its step comprises:
(A). the method by liquid deposition on Zeo-karb, makes the resin-base nano hydrated ferric oxide material with the nano hydrated ferric oxide particles supported;
(B). at pH is 3～7, and temperature is under 5～50 ℃, is that 0.5～30BV/h is by being filled with the adsorption column of resin-base nano hydrated ferric oxide with being subjected to the water body of the little pollution of heavy metal with flow; Perhaps will be subjected to heavy metal micro-polluted water body and resin base hydrous iron oxide is to be mixed in the container in 500: 1～10: 1 by volume, vibration back centrifuge dripping;
(C). for the resin-base nano hydrated ferric oxide after the absorption, with HCl or HNO
3Solution carries out desorption, and wherein resin-base nano hydrated ferric oxide returns step (A) and applies mechanically, and add alkali lye in the desorption liquid and make heavy metal precipitation, and filtering separation; Or adopt EDTA solution to carry out desorption and regeneration.
2. the method for a kind of resin-base nano hydrated ferric oxide deep purifying heavy metal micro-polluted water body according to claim 1, it is characterized in that Zeo-karb can be D001 in the step (A), 001 * 7, D113, Amberlite 252 resins, the hydrous iron oxide mass percent (in Fe) of load is 0.5～40%.
3. the method for resin-base nano hydrated ferric oxide deep purifying heavy metal micro-polluted water body according to claim 2, it is characterized in that the heavy metal concentration of polluted-water can be 0.01～300mg/L in the step (B), can attach most importance to 0～200 times of metal molar concentration of the volumetric molar concentration of competing ions.
4. according to the method for each described resin-base nano hydrated ferric oxide deep purifying heavy metal micro-polluted water body in the claim 1～3, it is characterized in that in the step (B) that the vibration controllable rotation speed is made as 100～300rpm, duration of oscillation is controlled to be made as 1～10 hour.
5. according to the method for each described resin-base nano hydrated ferric oxide deep purifying heavy metal micro-polluted water body in the claim 1～3, it is characterized in that HCl or HNO in the step (C)
3The weight percent of solution can be 0.5～5%, and perhaps the concentration of EDTA is 1-40%, the controlled 0.5～5BV/h that is made as of the flow of desorption liquid.
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