CN110252239A - A kind of efficient method for controlling Organic- arsenic pollution in water - Google Patents
A kind of efficient method for controlling Organic- arsenic pollution in water Download PDFInfo
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- CN110252239A CN110252239A CN201910401024.0A CN201910401024A CN110252239A CN 110252239 A CN110252239 A CN 110252239A CN 201910401024 A CN201910401024 A CN 201910401024A CN 110252239 A CN110252239 A CN 110252239A
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- ldhs
- mnfe
- arsenic
- water
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 42
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 41
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 8
- 238000000703 high-speed centrifugation Methods 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims description 35
- XKNKHVGWJDPIRJ-UHFFFAOYSA-N arsanilic acid Chemical compound NC1=CC=C([As](O)(O)=O)C=C1 XKNKHVGWJDPIRJ-UHFFFAOYSA-N 0.000 claims description 32
- 229950002705 arsanilic acid Drugs 0.000 claims description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 230000001376 precipitating effect Effects 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 7
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims description 7
- 238000005273 aeration Methods 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000001179 sorption measurement Methods 0.000 claims description 7
- 238000004064 recycling Methods 0.000 claims description 6
- 238000002242 deionisation method Methods 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(II) nitrate Inorganic materials [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 238000006555 catalytic reaction Methods 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 6
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract description 3
- 230000029087 digestion Effects 0.000 abstract description 2
- 150000001455 metallic ions Chemical class 0.000 abstract description 2
- 150000001495 arsenic compounds Chemical class 0.000 abstract 1
- 231100000086 high toxicity Toxicity 0.000 abstract 1
- 239000011949 solid catalyst Substances 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 description 14
- 238000007254 oxidation reaction Methods 0.000 description 14
- 238000010521 absorption reaction Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000011010 flushing procedure Methods 0.000 description 6
- 238000003760 magnetic stirring Methods 0.000 description 6
- 244000144972 livestock Species 0.000 description 5
- 244000144977 poultry Species 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
- VBUNOIXRZNJNAD-UHFFFAOYSA-N ponazuril Chemical compound CC1=CC(N2C(N(C)C(=O)NC2=O)=O)=CC=C1OC1=CC=C(S(=O)(=O)C(F)(F)F)C=C1 VBUNOIXRZNJNAD-UHFFFAOYSA-N 0.000 description 4
- 229960003508 ponazuril Drugs 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- -1 aromatic series arsenic compound Chemical class 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 210000003608 fece Anatomy 0.000 description 3
- 238000006385 ozonation reaction Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000005349 anion exchange Methods 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 238000007210 heterogeneous catalysis Methods 0.000 description 2
- 238000007172 homogeneous catalysis Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000002352 surface water Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 238000001927 high performance liquid chromatography-inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 239000002815 homogeneous catalyst Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000001394 metastastic effect Effects 0.000 description 1
- 206010061289 metastatic neoplasm Diseases 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- XMVJITFPVVRMHC-UHFFFAOYSA-N roxarsone Chemical compound OC1=CC=C([As](O)(O)=O)C=C1[N+]([O-])=O XMVJITFPVVRMHC-UHFFFAOYSA-N 0.000 description 1
- 229960003052 roxarsone Drugs 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0222—Compounds of Mn, Re
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Materials Engineering (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Catalysts (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention belongs to water-treatment technology fields, and in particular to a method of Organic- arsenic in water removal is removed using layered double hydroxide (LDHs) catalysis ozone, Organic- arsenic in water can be efficiently controlled and pollute.The present invention is directed to the removal problems for high toxicity Organic- arsenic in water, seek a kind of method efficiently, green, economic.The present invention is realized by following steps: one, preparing MnFe-LDHs；Two, the purification of raw water；Three, MnFe-LDHs is recycled using high speed centrifugation or filter method, the method for removing Organic- arsenic in water removal using LDHs catalysis ozone can be completed.Arsenic compound in water removal can have both been removed with efficient catalytic ozone using MnFe-LDHs of the invention (removal rate is more than 98%), simultaneously can inorganic arsenic (removal rate is more than 99.9%) to be discharged in efficiently concentrating degradation process, realize the security control that Organic- arsenic pollutes in water.Digestion of metallic ion rate is extremely low in use process, not will cause secondary pollution；The solid catalyst that the present invention uses can be isolated by filtration and be recycled, and reduce operating cost.
Description
Technical field
The invention belongs to water-treatment technology fields, and in particular to a kind of to be catalyzed using layered double hydroxide (LDHs)
The method that ozone removes Organic- arsenic in water removal can efficiently control Organic- arsenic in water and pollute.
Background technique
For a long time, the aromatic series arsenic compound for being widely used as feed addictive in livestock and poultry breeding industry and being used
(AOCs) enough attention and stringent management are not obtained.Metabolism is hardly happened after in AOCs intake livestock and poultry body, is more than
90% can be excreted in original form by excrement.Due to being rich in nutriment in feces of livestock and poultry, after generally going through accumulation
Farmland nearby is applied to as fertilizer.However, AOCs has quite high water solubility, with field irrigation and rain drop erosion, fertilizer
AOCs in material can be transferred in underground water and surface water by eluviation.It is reported that in feces of livestock and poultry about 57% arsenic
Natural water body can be entered by agricultural run-off.From being derived from the Ah detected in surface water water sample near Delta of the Pearl River pig farm
It dissipates acid (p-ASA) concentration and reaches 0.53~2.6 μ g/L.The roxarsone detected in the runoff for flowing through feces of livestock and poultry improvement soil
(ROX) at concentrations up to 1.07mg/L.Although the toxicity of AOCs is very low, it is safe from harm substantially under low dosage to human body, in water
They can be generated by biology and non-biological transformation approach in environment has hypertoxicity, high carcinogenic and strong metastatic inorganic
Arsenic.Therefore, it needs to find the pollution problem that effective treating method solves Organic- arsenic in environment.
Catalytic ozonation is the persistent organic pollutants oxidation removal hot spot technology with application prospect, i.e., logical
It crosses and some catalyst is added, promote the hydroxyl radical free radical (OH) for generating a large amount of high oxidation activities in reaction system, reach degradation
The purpose of organic pollutants.According to the difference of catalyst, which is divided into homogeneous catalysis ozone oxidation and heterogeneous catalysis
Ozone oxidation.The common catalyst of homogeneous catalysis ozone oxidation is generally transition metal ions, such as: Mn2+、Fe2+、Fe3+、Cu2+、
Zn2+、Co2+Deng.Homogeneous catalyst has many advantages, such as faster reaction speed, higher reactivity, but after the reaction, gold
Belong to ion-solubility Yu Shuizhong, catalyst is caused to be largely lost, causes the loss of economy and the pollution to environment.With homogeneously urge
Change ozone oxidation to compare, heterogeneous catalysis ozone oxidation can not only improve the removal efficiency of organic matter, while have operation letter
The features such as single, easy to maintain, without secondary pollution, therefore have broad application prospects in water treatment procedure and potentiality to be exploited.
Layered double hydroxide (LDHs) has unique layer structure, acid-base property, strong adsorptivity and interlayer anion exchange
Ability has broad application prospects in catalytic field.
Summary of the invention
Present invention seek to address that the Security Control Problem that Organic- arsenic pollutes in water, has been put forward for the first time a kind of utilization LDHs catalysis
The method that ozone removes Organic- arsenic in water removal.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of efficient method for controlling Organic- arsenic pollution in water, described method includes following steps:
Step 1: preparation MnFe-LDHs
S1, by Mn (NO3)2·4H2O and Fe (NO3)3·9H2O, which is added in deionized water, to be stirred to being completely dissolved；
S2, under stirring conditions, by NaOH and Na2CO3Mixed solution is added drop-wise in the mixed solution of step S1 dropwise and adjusts
Saving its pH is 9.8~10.1；
S3, by the mixed solution of step S2 in 60 DEG C of water-bath aging 4h, maintain mixed solution pH be 9.8~
10.1；
It is successively several with ethyl alcohol and deionized water flushing will to filter resulting precipitating for the mixed solution of S4, filtration step S3
Secondary, the precipitating after rinsing well, which is placed in 60 DEG C of baking oven, to be dried in vacuum overnight to get MnFe-LDHs；
Step 2: the purification of raw water
S5, the raw water containing arsanilic acid is placed in reactor, MnFe-LDHs made from step S4 is added thereto, and
20~40min is sufficiently stirred with magnetic stirring apparatus, to reach adsorption equilibrium, be then passed through into reactor ozone reaction 5~
30min can be realized the efficiently concentrating of the efficient inorganic arsenic for removing and discharging of arsanilic acid in raw water；
Step 3: the recycling of MnFe-LDHs
S6, MnFe-LDHs is recycled using high speed centrifugation or the method for filtering, and if successively being cleaned with ethyl alcohol and deionization
Dry time, the MnFe-LDHs cleaned up is placed in 60 DEG C of baking oven and is dried in vacuo.
Preferably, Mn (NO described in step S13)2·4H2O and Fe (NO3)3·9H2The molar ratio of O be 1~1.5:1~
1.5, more preferably 1:1.
Preferably, NaOH described in step S2 and Na2CO3Molar ratio be 3~4:1, more preferably 3.5:1.
Preferably, the ratio between the dosage mg and the volume L of raw water of MnFe-LDHs described in step S5 are 10~500:1.
Preferably, ozone described in step S5 is prepared with pure oxygen, the ozone passes through sand core aeration head from reaction
Device bottom is passed through, and keeping the temperature in reactor is 15~45 DEG C, and the pH of solution is 3~11 in reactor.
Preferably, the flow velocity of the ozone is 0.1~1.0L/min.
Preferably, the revolving speed of centrifuge is 13000~16000r/ when supercentrifugal process being used to recycle MnFe-LDHs
Min, more preferably 15000r/min.
The principle of the invention: currently, the method for removing Organic- arsenic in water body mainly has absorption method and some high-level oxidation technologies
Including UV/H2O2、UV/TiO2、UV/O3, Fenton oxidation method etc., but these technologies only realize Organic- arsenic to inorganic arsenic
Oxidation conversion, thoroughly arsenic pollution object is not removed from water body.LDHs be a major class it is important have supermolecular intercalation knot
The novel inorganic functional material of structure has unique space structure and higher ion exchange capacity.The interlayer of MnFe-LDHs
Anion exchange properties are conducive to ozone and inorganic arsenic and enter wherein interbed, accelerate ozone catalytic decomposition and release it is inorganic
The enrichment of arsenic；High-specific surface area is capable of providing a large amount of catalysis and active adsorption sites, is conducive to the catalysis and release of ozone
Inorganic arsenic absorption；Regular orderly open duct, size adjustable aperture then can be to be catalyzed and adsorption reaction provide object
Matter transmission path, the inorganic arsenic for being conducive to AOCs and release diffuse to active site.The MnFe-LDHs developed is a kind of green
Color, efficient, stable multifunctional solid material, can be realized the security control of AOCs in water.
The beneficial effects of the present invention are:
One, MnFe-LDHs of the invention has hydroxyl group contained on interlayer anion commutativity and its laminate,
Be conducive to the absorption of the inorganic arsenic of catalysis ozone decomposition and release；
Two, MnFe-LDHs of the invention can be recycled after using and recycle, and reduce operating cost；
Three, operation of the present invention is simple, it is easy to accomplish；
Four, the method applied in the present invention digestion of metallic ion concentration is extremely low, and secondary pollution is minimum；
Five, the present invention can be effectively removed arsanilic acid in water (atoxylic acid), and removal rate is up to 95% or more, simultaneously
Substantially it is detected without inorganic arsenic.
Detailed description of the invention
Fig. 1 is the removal effect figure of different process Ponazuril；
Fig. 2 is the effect picture of 70 reuse MnFe-LDHs Catalytic Ozonation arsanilic acids of the embodiment of the present invention.
Specific embodiment
Below by embodiment, in conjunction with attached drawing, explanation is further described to technical solution of the present invention.
Embodiment 1:
A kind of efficient method for controlling Organic- arsenic pollution in water, described method includes following steps:
Step 1: preparation MnFe-LDHs
S1, the Mn (NO for being 1:1 by molar ratio3)2·4H2O and Fe (NO3)3·9H2O be added in deionized water stir to
It is completely dissolved；
S2, under stirring conditions, by the NaOH and Na of molar ratio 3.5:12CO3Mixed solution is added drop-wise to step S1 dropwise
Mixed solution in adjust its pH be 9.8~10.1；
S3, by the mixed solution of step S2 in 60 DEG C of water-bath aging 4h, maintain mixed solution pH be 9.8~
10.1；
It is successively several with ethyl alcohol and deionized water flushing will to filter resulting precipitating for the mixed solution of S4, filtration step S3
Secondary, the precipitating after rinsing well, which is placed in 60 DEG C of baking oven, to be dried in vacuum overnight to get MnFe-LDHs；
Step 2: the purification of raw water
S5, raw water being placed in reactor, the volume of raw water is 500mL, and the concentration of arsanilic acid is 1.2mg/L in raw water,
MnFe-LDHs made from 10mg step S4 is added thereto, and 30min is sufficiently stirred with magnetic stirring apparatus, it is flat to reach absorption
Weighing apparatus, prepares ozone with pure oxygen, is passed through by sand core aeration head from reactor bottom, keeps 45 DEG C of reaction temperature and pH is 7
Under the conditions of react 30min, ozone flow velocity is 0.5L/min, can be realized the efficient of arsanilic acid in raw water and removes and the nothing of release
The efficiently concentrating of machine arsenic；
Step 3: the recycling of MnFe-LDHs
S6, MnFe-LDHs is recycled using supercentrifugal process, centrifuge speed 15000r/min, and successively uses ethyl alcohol
Several times with deionization cleaning, the MnFe-LDHs cleaned up is placed in 60 DEG C of baking oven and is dried in vacuo.
The removal rate of the present embodiment arsanilic acid is 96.2%, and inorganic arsenic is not detected.
Embodiment 2:
A kind of efficient method for controlling Organic- arsenic pollution in water, described method includes following steps:
Step 1: preparation MnFe-LDHs
S1, the Mn (NO for being 1:1 by molar ratio3)2·4H2O and Fe (NO3)3·9H2O be added in deionized water stir to
It is completely dissolved；
S2, under stirring conditions, by the NaOH and Na of molar ratio 3.5:12CO3Mixed solution is added drop-wise to step S1 dropwise
Mixed solution in adjust its pH be 9.8~10.1；
S3, by the mixed solution of step S2 in 60 DEG C of water-bath aging 4h, maintain mixed solution pH be 9.8~
10.1；
It is successively several with ethyl alcohol and deionized water flushing will to filter resulting precipitating for the mixed solution of S4, filtration step S3
Secondary, the precipitating after rinsing well, which is placed in 60 DEG C of baking oven, to be dried in vacuum overnight to get MnFe-LDHs；
Step 2: the purification of raw water
S5, raw water being placed in reactor, the volume of raw water is 500mL, and the concentration of arsanilic acid is 6mg/L in raw water, to
MnFe-LDHs made from 30mg step S4 is wherein added, and 20min is sufficiently stirred with magnetic stirring apparatus, to reach adsorption equilibrium,
Ozone is prepared with pure oxygen, is passed through by sand core aeration head from reactor bottom, keeping 15 DEG C of reaction temperature and pH is 9 condition
Lower reaction 20min, ozone flow velocity are 0.1L/min, can be realized the efficient inorganic arsenic removed and discharge of arsanilic acid in raw water
Efficiently concentrating；
Step 3: the recycling of MnFe-LDHs
S6, MnFe-LDHs is recycled using filtration method, and is successively cleaned several times with ethyl alcohol and deionization, cleaning is dry
Net MnFe-LDHs is placed in 60 DEG C of baking oven and is dried in vacuo.
The removal rate of the present embodiment arsanilic acid is 95.4%, and inorganic arsenic is not detected.
Embodiment 3:
The quality for the MnFe-LDHs that the present embodiment is added into raw water is 100mg, and other conditions are the same as embodiment 1.
The removal rate of the present embodiment arsanilic acid is 98.4%, and inorganic arsenic is not detected.
Embodiment 4:
The flow velocity of the present embodiment ozone is 1.0L/min, and other conditions are the same as embodiment 2.
The removal rate of the present embodiment arsanilic acid is 97.2%, and inorganic arsenic is not detected.
Embodiment 5:
A kind of efficient method for controlling Organic- arsenic pollution in water, described method includes following steps:
Step 1: preparation MnFe-LDHs
S1, the Mn (NO for being 1:1 by molar ratio3)2·4H2O and Fe (NO3)3·9H2O be added in deionized water stir to
It is completely dissolved；
S2, under stirring conditions, by the NaOH and Na of molar ratio 3.5:12CO3Mixed solution is added drop-wise to step S1 dropwise
Mixed solution in adjust its pH be 9.8~10.1；
S3, by the mixed solution of step S2 in 60 DEG C of water-bath aging 4h, maintain mixed solution pH be 9.8~
10.1；
It is successively several with ethyl alcohol and deionized water flushing will to filter resulting precipitating for the mixed solution of S4, filtration step S3
Secondary, the precipitating after rinsing well, which is placed in 60 DEG C of baking oven, to be dried in vacuum overnight to get MnFe-LDHs；
Step 2: the purification of raw water
S5, raw water being placed in reactor, the volume of raw water is 500mL, and the concentration of arsanilic acid is 3.2mg/L in raw water,
MnFe-LDHs made from 20mg step S4 is added thereto, and 20min is sufficiently stirred with magnetic stirring apparatus, it is flat to reach absorption
Weighing apparatus, prepares ozone with pure oxygen, is passed through by sand core aeration head from reactor bottom, keeps 15 DEG C of reaction temperature and pH is 3
Under the conditions of react 30min, ozone flow velocity is 0.5L/min, can be realized the efficient of arsanilic acid in raw water and removes and the nothing of release
The efficiently concentrating of machine arsenic；
Step 3: the recycling of MnFe-LDHs
S6, MnFe-LDHs is recycled using supercentrifugal process, the revolving speed of centrifuge is 15000r/min, and successively uses second
Pure and mild deionization cleaning several times, the MnFe-LDHs cleaned up is placed in 60 DEG C of baking oven and is dried in vacuo.
The removal rate of the present embodiment arsanilic acid is 98.3%, and inorganic arsenic is not detected.
Embodiment 6:
It is 45 DEG C that reaction temperature is kept in the step S5 of the present embodiment, and other conditions are the same as embodiment 5.
The removal rate of the present embodiment arsanilic acid is 98.5%, and inorganic arsenic is not detected.
Embodiment 7:
For other conditions with embodiment 5, MnFe-LDHs used is the MnFe-LDHs that embodiment 5 recycles, and repeats test 9
Secondary, MnFe-LDHs used is the MnFe-LDHs of last recycling, altogether reuse 10 times, ten reuse MnFe- every time
The effect of LDHs Catalytic Ozonation arsanilic acid is as shown in Fig. 2.
As shown in Fig. 2, MnFe-LDHs has good reuse, its catalysis ozone Ponazuril after reuse ten times
Removal rate is still higher than 96%, in addition, not detecting inorganic arsenic during ten reuses, illustrates that MnFe-LDHs is shown
Good reuse.In conclusion MnFe-LDHs can not only arsanilic acid in efficient catalytic ozone degradation water, and can be high
The inorganic arsenic discharged in effect enrichment arsanilic acid degradation process, has many advantages, such as efficient, green, economic, the Organic- arsenic suitable for water
The removal of compound.
Embodiment 8:
The present embodiment inquires into the absorption property of independent MnFe-LDHs Ponazuril:
Step 1: preparation MnFe-LDHs
S1, the Mn (NO for being 1:1 by molar ratio3)2·4H2O and Fe (NO3)3·9H2O be added in deionized water stir to
It is completely dissolved；
S2, under stirring conditions, by the NaOH and Na of molar ratio 3.5:12CO3Mixed solution is added drop-wise to step S1 dropwise
Mixed solution in adjust its pH be 9.8~10.1；
S3, by the mixed solution of step S2 in 60 DEG C of water-bath aging 4h, maintain mixed solution pH be 9.8~
10.1；
It is successively several with ethyl alcohol and deionized water flushing will to filter resulting precipitating for the mixed solution of S4, filtration step S3
Secondary, the precipitating after rinsing well, which is placed in 60 DEG C of baking oven, to be dried in vacuum overnight to get MnFe-LDHs；
Step 2: the purification of raw water
S5, raw water being placed in reactor, the volume of raw water is 500mL, and the concentration of arsanilic acid is 10mg/L in raw water, to
MnFe-LDHs made from 50mg step S4 is wherein added, and 20min is sufficiently stirred with magnetic stirring apparatus, to reach adsorption equilibrium.
Embodiment 9:
The present embodiment inquires into the performance of independent ozone oxidation arsanilic acid:
The volume of raw water is 500mL in reactor, and the concentration of arsanilic acid is 10mg/L in raw water；
It is passed through ozone into reactor, is reacted: ozone is prepared with pure oxygen, by sand core aeration head from reactor bottom
It is passed through with flow velocity 0.5L/min, reacts 30min under conditions of to keep 25 DEG C of reaction temperature and pH be 7, it can be achieved that Ah San in water
The part removal of acid.
Embodiment 10:
The performance test of the present embodiment discussion MnFe-LDHs O3 catalytic oxidation arsanilic acid:
Step 1: preparation MnFe-LDHs
S1, the Mn (NO for being 1:1 by molar ratio3)2·4H2O and Fe (NO3)3·9H2O be added in deionized water stir to
It is completely dissolved；
S2, under stirring conditions, by the NaOH and Na of molar ratio 3.5:12CO3Mixed solution is added drop-wise to step S1 dropwise
Mixed solution in adjust its pH be 9.8~10.1；
S3, by the mixed solution of step S2 in 60 DEG C of water-bath aging 4h, maintain mixed solution pH be 9.8~
10.1；
It is successively several with ethyl alcohol and deionized water flushing will to filter resulting precipitating for the mixed solution of S4, filtration step S3
Secondary, the precipitating after rinsing well, which is placed in 60 DEG C of baking oven, to be dried in vacuum overnight to get MnFe-LDHs；
Step 2: the purification of raw water
S5, raw water being placed in reactor, the volume of raw water is 500mL, and the concentration of arsanilic acid is 10mg/L in raw water, to
MnFe-LDHs made from 50mg step S4 is wherein added, and 20min is sufficiently stirred with magnetic stirring apparatus, to reach adsorption equilibrium,
Ozone is prepared with pure oxygen, is passed through by sand core aeration head from reactor bottom, keeping 25 DEG C of reaction temperature and pH is 7 condition
Lower reaction 30min, ozone flow velocity are 0.5L/min, can be realized the efficient inorganic arsenic removed and discharge of arsanilic acid in raw water
Efficiently concentrating.
Embodiment 8,9,10 inquires into the comparison of MnFe-LDHs, ozone and MnFe-LDHs O3 catalytic oxidation arsanilic acid respectively
Experiment, contrast effect figure are shown in attached drawing 1.
As shown in Fig. 1, in 30 minutes, MnFe-LDHs can realize the removal of small part arsanilic acid by suction-operated
(14.37%)；And individually ozone oxidation can remove 37.22% arsanilic acid for 30 minutes.And when MnFe-LDHs combines with ozone
In use, the removal effect of arsanilic acid is significant in water, removal rate reaches 98.04% in 30 minutes.Using independent ozone oxidation
In the process, detected that 0.752mg/L inorganic arsenic discharges by High performance liquid chromatography-inductively coupled plasma mass spectrometry instrument, and
In MnFe-LDHs/O3In technique, inorganic arsenic is not detected, illustrates to discharge in MnFe-LDHs Ponazuril degradation process
Inorganic arsenic has good concentration effect.
In conclusion MnFe-LDHs of the invention has hydrogen contained on interlayer anion commutativity and its laminate
Oxygen groups are conducive to the absorption of the inorganic arsenic of catalysis ozone decomposition and release；MnFe-LDHs of the invention can be returned after using
It receives and recycles, reduce operating cost；Operation of the present invention is simple, it is easy to accomplish；The method applied in the present invention metal ion is molten
Concentration is extremely low out, and secondary pollution is minimum；The present invention can be effectively removed arsanilic acid in water, and removal rate is up to 95% or more, simultaneously
Substantially it is detected without inorganic arsenic.
Embodiment described above is preferred version of the invention, is not intended to limit the present invention in any form,
There are also other variants and remodeling on the premise of not exceeding the technical scheme recorded in the claims.
Claims (7)
1. a kind of method of Organic- arsenic pollution in efficiently control water, which is characterized in that described method includes following steps:
Step 1: preparation MnFe-LDHs
S1, by Mn (NO3)2·4H2O and Fe (NO3)3·9H2O, which is added in deionized water, to be stirred to being completely dissolved；
S2, under stirring conditions, by NaOH and Na2CO3Mixed solution be added drop-wise in the mixed solution of step S1 and adjust dropwise
Its pH is 9.8~10.1；
S3, by the mixed solution of step S2 in 60 DEG C of water-bath aging 4h, maintain mixed solution pH be 9.8~10.1；
The mixed solution of S4, filtration step S3 will filter resulting precipitating and successively be rinsed several times with ethyl alcohol and deionized water, will
Precipitating after rinsing well, which is placed in 60 DEG C of baking oven, to be dried in vacuum overnight to get MnFe-LDHs；
Step 2: the purification of raw water
S5, the raw water containing arsanilic acid is placed in reactor, MnFe-LDHs made from step S4 is added thereto, and use magnetic force
20~40min is sufficiently stirred in blender, and to reach adsorption equilibrium, 5~30min of ozone reaction, energy are then passed through into reactor
Enough realize the efficiently concentrating of the efficient inorganic arsenic for removing and discharging of arsanilic acid in raw water；
Step 3: the recycling of MnFe-LDHs
S6, MnFe-LDHs is recycled using high speed centrifugation or the method for filtering, and is successively cleaned with ethyl alcohol and deionization several
It is secondary, the MnFe-LDHs cleaned up is placed in 60 DEG C of baking oven and is dried in vacuo.
2. the method for Organic- arsenic pollution in efficient control water according to claim 1, which is characterized in that described in step S1
Mn(NO3)2·4H2O and Fe (NO3)3·9H2The molar ratio of O is 1~1.5:1~1.5.
3. the method for Organic- arsenic pollution in efficient control water according to claim 1, which is characterized in that described in step S2
NaOH and Na2CO3Molar ratio be 3~4:1.
4. the method for Organic- arsenic pollution in efficient control water according to claim 1, which is characterized in that described in step S5
The ratio between dosage mg and the volume L of raw water of MnFe-LDHs are 10~500:1.
5. the method for Organic- arsenic pollution in efficient control water according to claim 4, which is characterized in that described in step S5
Ozone is prepared with pure oxygen, and the ozone is passed through by sand core aeration head from reactor bottom, keeps the temperature in reactor
It is 15~45 DEG C, the pH of solution is 3~11 in reactor.
6. the method for Organic- arsenic pollution in efficient control water according to claim 5, which is characterized in that the stream of the ozone
Speed is 0.1~1.0L/min.
7. the method for Organic- arsenic pollution in efficient control water according to claim 1, which is characterized in that use high speed centrifugation
The revolving speed of centrifuge is 13000~16000r/min when method recycles MnFe-LDHs.
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