CN101780985A - Hydrotalcite-like compound used for raw water treatment - Google Patents
Hydrotalcite-like compound used for raw water treatment Download PDFInfo
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Abstract
The invention discloses a hydrotalcite-like compound. The chemical formula of the hydrotalcite-like compound is shown as follows: [Zn2+1-xFe3+x(OH)2][Cl-]x.H2O, wherein x=0.5-0.6; the hydrotalcite-like compound can be used as an adsorbent to absorb humic acid in raw water; the hydrotalcite-like compound has good adsorption property on the humic acid in raw water; the maximum adsorption capacity on the humic acid in the raw water can reach higher than 12.2mg/g and is far higher than the maximum adsorption capacity 2.51mg/g of granular active carbon; the rate of adsorption of the hydrotalcite-like compound on the humic acid is shown as follows: the adsorption capacity reaches more than 90 percent of the maximum adsorption capacity in 5 minutes, and adsorption equilibrium is achieved in 45 minutes.
Description
Technical field
The invention belongs to inorganic lamellar material preparation field and sewage purification field, be specifically related to the houghite of the humic acids in a kind of adsorbable water.
Background technology
Humic acid material extensively is present in natural soil and the water body, mainly be decomposed to form through microorganism and various physical and chemical process by the animals and plants remains, be organic main component in the natural water body, account for 50%～90% (massfraction) of total organic matter in the water.Humic acid mainly comprises humic acid, fulvic acid and hydrophilic small molecules organism.Because humic acid produces color beastly and smell in water body, particularly can generation in the chlorine disinfectant process multiple by product haloform that human body is had carcinogenic, teratogenesis, mutagenesis etc.In recent years, the drinking water safety problem is subjected to attention more and more widely, and " drinking water sanitary standard " (GB 5749-2006) of promulgation in 2006 has haloform etc. three to cause the disinfection byproduct (DBP) (DBPs) of effect as controlled member to human body first.Therefore how simultaneously, humic acid has certain absorption complexing action to toxic organic compound in the water body and heavy metal ion, can form combined pollutant, and humic acid becomes the research focus of environment circle in the economical and efficient ground removal water body.
In the prior art, the method for removing humic acid in the water body mainly contains: membrane filtration, flocculence, oxidation style, biological process etc., wherein use more with membrane filtration, flocculence and oxidation style research.Though membrane filtration can be removed the macromolecular substance in the humic acid, but be difficult to remove the hydrophilic small molecules organism, often contain high volence metal ions such as calcium, magnesium in the natural water body in addition, can with the oxygen-containing functional group generation complex reaction in the humic acid molecule, very easily cause film to pollute; Flocculence can reach about 60% the clearance of humic acid, there are some researches show that still inorganic flocculating agent and organic floculant have certain harm to the health of human body, so the security of humic acid is under suspicion always in the flocculence removal water body; The difficult for biological degradation of humic acid has limited the application of biological process, and experiment shows that active sludge 48h only has 10% to the degradation rate of humic acid, and treatment effect is relatively poor; Though by can to a certain degree degrade humic acid in the water body of oxidation style such as ozone, photochemical catalysis, electrolysis, running cost is higher, device is complicated, treatment capacity is limited, therefore influences it in actual application in engineering.Absorption method relies on pore structure intensive on the sorbent material, huge specific surface area, or forms various chemical bonds by various active groups in surface and adsorbate, reaches the organic purpose of enrichment selectively.The advantage of absorption method is that the organism of reluctant metal ion of biological process and difficult degradation is had removal effect preferably.It more and more is subject to people's attention at present as a kind of solid phase extraction techniques of less energy-consumption.Use more about the research of carbonaceous adsorbent, polymeric adsorbent and inorganic mineral sorbent material both at home and abroad at present.Wherein the gac in the carbonaceous adsorbent exist the absorption back be difficult for regeneration, to problems such as hydrophilic small molecules organism adsorption effect differences; Polymeric adsorbent is not good to the hydrophilic small molecules organism adsorption effect in the humic acid; The absorption property of the zeolite in the inorganic mineral sorbent material is limited by the amount of the activator of zeolite surface modification; Though rankinite is cheap, fulvic acid and the hydrophilic small molecules organic removal rate little to molecular weight are not high; Pyrrhosiderite is not high to fulvic acid and hydrophilic small molecules organic removal rate, and adsorption effect also is subjected to the influence of solution ion concentration and pH; PERFORMANCE OF MODIFIED VERMICULITE can be by hydrogen bond and huge legendary turtle cooperation with the absorption fulvic acid, is that the clearance of the humic acid solution of 20mg/L can reach about 80% to mass concentration, and in adsorption process, the pH of solution and ionic concn can influence adsorption effect, and regeneration is not easy; Also there is the shortcoming of adsorbent reactivation difficulty in aluminium hydroxide/wilkinite.Houghite in the inorganic mineral sorbent material (hydrotalcite-like compounds is called for short HTlc) is the mixed metal hydroxides that a class has laminate structure.Its general formula is [M
2+ 1-xM
3+X (OH)
2] [A
N-]
X/nMH
2O, wherein M
2+Be divalent metal, M
3+Be trivalent metal cation, A
N-Be interlayer anion, x is the molar fraction of trivalent metal cation among every mole of HTLc, and m is the mole number of interlayer crystal water among every mole of HTLc.Owing to part divalent-metal ion in the lamella is had the residue positive charge by the trivalent metal ion isomorphous substitution, be called the structure positive charge.Houghite is the nano particle with laminate structure, has the interchangeability of interlayer anion, and specific surface area is bigger, the source is abundant, price economy all has stronger adsorptive power to various heavy metal ion, organic anion, inorganic anion etc., can be used to handle sewage of low concentration.
Present houghite is mainly Mg/Al, Mg/Fe type houghite has certain removal effect (referring to [1] Wang Jinnan to humic acid in the water, Li Aimin, Zhang Long, Zhou Youdong, Zhang Quanxing. absorption method is removed the progress of humic acid in the water body. Environmental Pollution and Control, 2008,30 (8): 73-77; [2] Zhang Xiaojin. magnesium iron houghite and composite oxides preparation and to the research [D] of humic acid removal effect in the water. Shandong University, 2006).
But do not see other types, for example the report of Zn/Fe type houghite.
Summary of the invention
The object of the invention provides a kind of houghite.
For achieving the above object, the concrete technical scheme of the present invention is, a kind of houghite, and the chemical formula of described houghite is: [Zn
2+ 1-xFe
3+ x(OH)
2] [Cl
-]
xH
2O, wherein, x=0.5～0.6.
The method for preparing above-mentioned houghite may further comprise the steps:
(1) in the whole process of preparation, be mete-wand with the amount of substance, with FeCl
24H
2The amount of substance of O is 1 part; Under 10～30 ℃, with 1～10 part of ZnCl
26H
2O and 1 part of FeCl
24H
2O dissolves in deionized water, obtains solution A;
(2) regulate pH with the NaOH solution adding solution A of 1～5mol/L and be about 7～8, stirred 1～4 hour, obtain solution B;
(3) get 1～2 part of hydrogen peroxide, being mixed with massfraction with deionized water is 6～10% hydrogen peroxide solution, adds solution B with Fe
2+Be oxidized to Fe
3+, 10～30 ℃ of down aging 3～6h, suction filtration is washed till pH6.5～8 with deionized water, prepares described houghite at 70～80 ℃ of drying 16～24h then.
The present invention also comprises the processing of above-mentioned houghite to former water, and described former water is the former water that contains humic acid, and the present invention protects described houghite as Application humic in the former water of adsorbents adsorb simultaneously; Houghite of the present invention has the good adsorption performance to the water humic acid, can reach more than the 12.2mg/g the saturated extent of adsorption of humic acid in the water.
Use the method for described houghite, may further comprise the steps as humic acids in the former water of adsorbents adsorb:
By agitation as appropriate houghite is suspended in the former water to adsorb the humic acids in the former water in fluidized-bed, the saturated back of houghite absorption humic acids is by method and former water sepn such as sedimentation or filtrations;
Wherein, the suitable consumption of houghite is 1～10g/L, in the adsorption process, temperature is 15～35 ℃, and the humic acids starting point concentration is 15～150mg/L, pH value of solution=3～7, adsorption time is 100～140min, and control ionogen (in NaCl) concentration is less than 0.025mol/L.
Ultimate principle of the present invention is: houghite is the nano particle with laminate structure, has the interchangeability of interlayer anion, and specific surface area is bigger, and various heavy metal ion, organic anion, inorganic anion etc. are all had stronger adsorptive power.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
1, houghite of the present invention is to the maximal absorptive capacity (12.2mg/g) of the humic acid maximal absorptive capacity (2.51mg/g far above granulated active carbon; referring to: Chen J P; Wu S.Simultaneousadsorption of copper ions and humic acid onto an activated carbon[J] .JColloid Interface Sci; 2004,280 (2): 334-342.)
2, houghite of the present invention is to the rate of adsorption of humic acid (5min adsorptive capacity more than 90% of adsorptive capacity that reaches capacity, 45min reaches adsorption equilibrium) (90% of the adsorptive capacity that reaches capacity needs 120min to be higher than modified clinoptilolite, referring to: square Jinpeng, Zhang Panyue, Ceng Guang is bright, Zou Sai, Yang Li, Wu Hao, Cao Qun. the research of humic acid in the modified clinoptilolite planar water. Chinese water supply and drainage, 2008,24 (23): 48-51).
Description of drawings
Catalyst preparation process schema in Fig. 1 present embodiment one to four;
The ultimate analysis figure of houghite among Fig. 2 embodiment one;
The XRD figure of houghite among Fig. 3 embodiment one;
The FTIR of houghite figure among Fig. 4 embodiment one;
The ultimate analysis figure of houghite among Fig. 5 embodiment two;
The ultimate analysis figure of houghite among Fig. 6 embodiment three;
The humic acid starting point concentration is to the influence of houghite absorption humic acid among Fig. 7 embodiment four;
PH is to the influence of houghite absorption humic acid among Fig. 8 embodiment four;
Temperature is to the influence of houghite absorption humic acid among Fig. 9 embodiment four;
Ionogen is to the influence of houghite absorption humic acid among Figure 10 embodiment four;
The kinetics of houghite absorption humic acid among Figure 11 embodiment four;
Gained hydrotalcite-like compound synoptic diagram among Figure 12 embodiment.
Embodiment
Below in conjunction with drawings and Examples the present invention is further described:
Embodiment one: shown in accompanying drawing 1:
The first step is a mete-wand with the amount of substance, with FeCl
24H
2The amount of substance of O is 1 part; Under 30 ℃, with 1 part of ZnCl
26H
2O and 1 part of FeCl
24H
2O dissolves in the 100ml deionized water, obtains solution A;
In second step, the NaOH solution of getting an amount of 1mol/L adds solution A adjusting pH and is about 7, stirs 2 hours, obtains solution B;
The 3rd step, get 1 part of hydrogen peroxide, being mixed with massfraction with deionized water is 6% hydrogen peroxide solution, adds solution B with Fe
2+Be oxidized to Fe
3+, 30 ℃ of down aging 3h, suction filtration is washed till pH with deionized water and is about 7, makes houghite at 70 ℃ of dry 16h then.
Fig. 2～Fig. 4 is for characterizing the collection of illustrative plates of houghite.
Embodiment two: shown in accompanying drawing 1:
The first step is a mete-wand with the amount of substance, with FeCl
24H
2The amount of substance of O is 1 part; Under 10 ℃, with 2 parts of ZnCl
26H
2O and 1 part of FeCl
24H
2O dissolves in deionized water, obtains solution A;
In second step, the NaOH solution of getting an amount of 1mol/L adds solution A adjusting pH and is about 8, stirs 2 hours, obtains solution B;
The 3rd step, get 1 part of hydrogen peroxide, being mixed with massfraction with deionized water is 6% hydrogen peroxide solution, adds solution B with Fe
2+Be oxidized to Fe
3+, 10 ℃ of down aging 6h, suction filtration is washed till pH with deionized water and is about 6.5, makes houghite at 80 ℃ of dry 24h then.
Fig. 5 is the ultimate analysis figure of houghite.
Embodiment three: shown in accompanying drawing 1:
The first step is a mete-wand with the amount of substance, with FeCl
24H
2The amount of substance of O is 1 part; Under 10 ℃, with 4 parts of ZnCl
26H
2O and 1 part of FeCl
24H
2O dissolves in deionized water, obtains solution A;
In second step, the NaOH solution of getting an amount of 1mol/L adds solution A adjusting pH and is about 7, stirs 2 hours, obtains solution B;
The 3rd step, get 1 part of hydrogen peroxide, being mixed with massfraction with deionized water is 6% hydrogen peroxide solution, adds solution B with Fe
2+Be oxidized to Fe
3+, 10 ℃ of down aging 6h, suction filtration is washed till pH with deionized water and is about 8, makes houghite at 80 ℃ of dry 24h then.
Fig. 6 is the ultimate analysis figure of houghite.
Embodiment four:
Adopt the Static Adsorption method to come humic acid in the treating water.With humic acid (BR) and 0.1mol/L NaOH hot solution (about 60 ℃) preparation HA mother liquor.In washing, the dry 250mL Erlenmeyer flask of crossing, add certain amount of H A mother liquor and one-level ultrapure water, mix, regulate pH to design load with sodium hydroxide and hydrochloric acid soln.A certain amount of houghite is added in the Erlenmeyer flask, mix and regulate once more the pH value.25 ℃ of vibrations of constant temperature certain hour (t) takes out with behind the 0.45 μ m membrane filtration in constant temperature oscillator, measures HA concentration in the filtrate, does blank (not adding HTlc) experiment simultaneously, according to the change calculations adsorptive capacity (qe) of HA concentration before and after the absorption.HA concentration adopts the UV254 method to measure.Instrument is the UV-7504 ultraviolet-visible spectrophotometer, and wavelength is 254nm, and the mensuration temperature is a room temperature.
Investigate different humic acid starting point concentrations, initial pH, temperature, electrolyte concentration to the influence that houghite adsorbs humic acids, see Fig. 7～Figure 11 respectively.
(1) the humic acid starting point concentration the results are shown in Figure 7 to the influence of houghite absorption humic acid;
(2) initial pH the results are shown in Figure 8 to the influence of houghite absorption humic acid;
(3) temperature the results are shown in Figure 9 to the influence of houghite absorption humic acid;
(4) ionogen the results are shown in Figure 10 to the influence of houghite absorption humic acid;
(5) kinetics of houghite absorption humic acid the results are shown in Figure 11.
By agitation as appropriate houghite is suspended in the former water to adsorb the humic acids in the former water in fluidized-bed, the saturated back of houghite absorption humic acids is by method and former water sepn such as sedimentation or filtrations.The suitable consumption of houghite is 1～10g/L, and temperature is 15～35 ℃, and the humic acids starting point concentration is 15～150mg/L, pH value of solution=3～7, and adsorption time is 100～140min, control ionogen (in NaCl) concentration is less than 0.025mol/L.
Claims (4)
1. a houghite is characterized in that, the chemical formula of described houghite is: [Zn
2+ 1-xFe
3+ x(OH)
2] [Cl
-]
xH
2O, wherein, x=0.5～0.6.
2. a method for preparing houghite is characterized in that, may further comprise the steps:
(1) in the whole process of preparation, be mete-wand with the amount of substance, with FeCl
24H
2The amount of substance of O is 1 part; Under 10～30 ℃, with 1～5 part of ZnCl
26H
2O and 1 part of FeCl
24H
2O dissolves in deionized water, obtains solution A;
(2) regulate pH with the NaOH solution adding solution A of 1～5mol/L and be about 7～8, stirred 1～4 hour, obtain solution B;
(3) get 1～2 part of hydrogen peroxide, being mixed with massfraction with deionized water is 6～10% hydrogen peroxide solution, adds solution B with Fe
2+Be oxidized to Fe
3+, 10～30 ℃ of down aging 3～6h, suction filtration is washed till pH6.5～8 with deionized water, prepares described houghite at 70～80 ℃ of drying 16～24h then.
3. the described houghite of claim 1 is as Application humic in the former water of adsorbents adsorb.
4. application rights requires the method for 1 described houghite as humic acids in the former water of adsorbents adsorb, may further comprise the steps:
In fluidized-bed, houghite is suspended in the former water to adsorb the humic acids in the former water, saturated back of houghite absorption humic acids and former water sepn by stirring;
Wherein, the consumption of houghite is 1～10g/L, in the adsorption process, temperature is 15～35 ℃, and the humic acids starting point concentration is 15～150mg/L, pH value of solution=3～7, adsorption time is 100～140min, and control ionogen (in NaCl) concentration is less than 0.025mol/L.
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| CN102150685A (en) * | 2011-01-31 | 2011-08-17 | 浙江工业大学 | Binary magnesium-aluminum hydrotalcite and use thereof as disinfectant |
| CN102976517A (en) * | 2012-11-28 | 2013-03-20 | 常州大学 | Method for treating industrial pickling wastewater |
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| CN102150685A (en) * | 2011-01-31 | 2011-08-17 | 浙江工业大学 | Binary magnesium-aluminum hydrotalcite and use thereof as disinfectant |
| CN102150685B (en) * | 2011-01-31 | 2013-07-24 | 浙江工业大学 | Binary magnesium-aluminum hydrotalcite and use thereof as disinfectant |
| CN102976517A (en) * | 2012-11-28 | 2013-03-20 | 常州大学 | Method for treating industrial pickling wastewater |
| CN103193276A (en) * | 2013-04-28 | 2013-07-10 | 北京化工大学 | Method for synthesizing iron-containing hydrotalcite-like compound by utilizing prussian blue as raw material |
| CN103193276B (en) * | 2013-04-28 | 2014-07-09 | 北京化工大学 | Method for synthesizing iron-containing hydrotalcite-like compound by utilizing prussian blue as raw material |
| CN106076357A (en) * | 2016-06-12 | 2016-11-09 | 常州大学 | A kind of preparation method of magnetic loading manganese dioxide-catalyst |
| CN106076350B (en) * | 2016-06-12 | 2018-08-14 | 常州大学 | A kind of preparation method for handling the magnetic loading cerium oxide of exhaust gas |
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| CN106076350A (en) * | 2016-06-12 | 2016-11-09 | 常州大学 | A kind of preparation method of the magnetic loading cerium oxide for processing waste gas |
| CN105964262A (en) * | 2016-06-12 | 2016-09-28 | 常州大学 | Preparation method of magnetic composite nickel oxide catalyst |
| CN106076362B (en) * | 2016-06-12 | 2018-05-04 | 常州大学 | It is a kind of can magnetic separation silver oxide catalyst preparation method |
| CN106076339B (en) * | 2016-06-12 | 2018-05-04 | 常州大学 | A kind of preparation method of magnetism synergistic oxidation Co catalysts |
| CN105964262B (en) * | 2016-06-12 | 2018-06-26 | 常州大学 | A kind of preparation method of magnetic coupling nickel oxide catalyst |
| CN106000324A (en) * | 2016-06-12 | 2016-10-12 | 常州大学 | Preparation method of magnetic organic hydrotalcite |
| CN110304660A (en) * | 2019-04-03 | 2019-10-08 | 沈阳化工大学 | A kind of ZnFe-CO3/SO4The preparation method of type hydrotalcite |
| CN110102246A (en) * | 2019-04-28 | 2019-08-09 | 华东交通大学 | A kind of magnetic layered double-metal hydroxide adsorbent and its dephosphorization remove chromium application |
| CN110102246B (en) * | 2019-04-28 | 2021-11-12 | 华东交通大学 | Magnetic layered double-metal hydroxide adsorbent and application thereof in removing phosphorus and chromium |
| CN111604053A (en) * | 2020-06-07 | 2020-09-01 | 重庆工商大学 | Ternary hydrotalcite photocatalyst and preparation method and application thereof |
| CN111604053B (en) * | 2020-06-07 | 2022-09-02 | 重庆工商大学 | Ternary hydrotalcite photocatalyst and preparation method and application thereof |
| CN112062203A (en) * | 2020-09-19 | 2020-12-11 | 邵阳天堂助剂化工有限公司 | Method for removing humic acid in water by adsorption of roasted Ca-Al hydrotalcite |
| CN112062204A (en) * | 2020-09-19 | 2020-12-11 | 邵阳天堂助剂化工有限公司 | Method for removing humic acid in water by adsorption of calcined hydrocalumite |
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