CN102600790A - Nanometer cerium oxide hydrate-based arsenic removing material, preparation method thereof and application in arsenic removing - Google Patents
Nanometer cerium oxide hydrate-based arsenic removing material, preparation method thereof and application in arsenic removing Download PDFInfo
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Abstract
The invention belongs to the inorganic non-metal nanometer material preparation and the environmental friendliness field of water purification, in particular relates to a nanometer cerium oxide hydrate-based adsorbing material with a high specific surface area, a preparation method of the adsorbing material and application in removing arsenic. By using the nanometer cerium oxide hydrate-based adsorbing material, trivalent arsenic and pentavalent arsenic in the water can be removed at one step and the current problem that the content of arsenic in water exceeds the standard can be effectively solved. The cerium oxide hydrate-based adsorbing material is obtained by the steps of depositing a cerium salt (or a mixture of a cerium salt and other metal salt) by an alkali in water (or a non-aqueous solvent) and drying the product. The preparation method is simple in process; the obtained cerium oxide hydrate-based adsorbing material is large in specific surface area, strong in arsenic removing ability, wide in pH applicable range and stable in performance, and the arsenic pollution in a natural water area can be simply and efficiently removed by loading the adsorbing material with no need of pre-treatment, so as to provide a novel arsenic removing material for purification of arsenic-containing sewage and environment friendliness.
Description
Technical field
The invention belongs to inorganic nonmetallic nanometer material preparation and water purification field of environment protection, be specially a kind of nano hydrated cerium oxide base sorbing material and preparation method thereof and application aspect arsenic removal of high-specific surface area.
Background technology
Arsenic is distributed widely in atmosphere, water, soil, rock and the organism, and in natural water, the arsenic of dissolving generally exists with inorganic arsenic hydrochlorate, arsenite form or with methylated arsenic compound form.At present, in the surface water of many countries and regions, found arsenic contamination.In Inner Mongol of China, ground such as Xinjiang, Taiwan, in the drinking-water arsenic content in some areas up to 0.2-2.0mg/L.
China drinking water standard GB5749-2006 regulation arsenic mass concentration must not surpass 10ppb, and the Drinking Water arsenic mass concentration of the U.S., the European Community, WHO must not surpass 10ppb, and arsenic exceeds standard and becomes one of urgent problem in the control water.
Absorption method has the treatment effeciency height, adsorptive hindrance is little, and the renewable repeated use of adsorbent can or seldom not produce secondary pollution to environment.In the current domestic and international absorption method dearsenicating method, composite and material modified arsenic removal efficient are high, and disposal cost is low, has market application foreground; The adsorption effect of active material receives pH value control strict, and the iron-bearing mineral material is prone to cause secondary pollution in the arsenic removal process, and nano material combines afterwards stable in properties and arsenic removal most effective with other atoms, be main developing direction from now on.Nano material has a series of strange physicochemical characteristics and the property that is superior to traditional material, and along with reducing of particle diameter, surface atom number, surface area, surface ability and Surface binding energy all increase rapidly.Owing to lack adjacent atom around the surface atom, have unsaturation, be prone to combine with other atom and settle out, thereby nano material has very strong adsorption capacity to many ions.
At present, existing arsenic-removing adsorption agent ubiquity adsorption capacity is low, and the rate of adsorption is slow, needs problems such as preliminary treatment.Therefore, press for the arsenic contamination problem that a kind of advantages of simplicity and high efficiency novel absorption material solution becomes increasingly conspicuous of seeking.
Summary of the invention
The present invention provides nano hydrated cerium oxide base arsenic removal material of a kind of advantages of simplicity and high efficiency and preparation method thereof and arsenic removal to use; This cerium base arsenic removal material preparation technology is simple; Easy to operate; Can remove the middle arsenic that anhydrates efficiently, the arsenic removal process can effectively solve the problem that arsenic exceeds standard in the present water without any need for preliminary treatment.
Technical scheme of the present invention is:
A kind of nano hydrated cerium oxide base arsenic removal material, this arsenic removal material component contains the nanoscale cerium oxide particle; Perhaps; Contain in nanoscale cerium oxide particle and nano level lanthana, lanthanum hydroxide, iron oxide, iron hydroxide, titanium oxide, manganese oxide, the alumina particle one or more simultaneously; The mol ratio of one or more in cerium oxide particle and lanthana, lanthanum hydroxide, iron oxide, iron hydroxide, titanium oxide, manganese oxide, the aluminium oxide is 10%～100%; It has higher surface area and stronger arsenic removal ability, and its surface area is 200-500m
2/ g.
The preparation method of said nano hydrated cerium oxide base arsenic removal material comprises the steps:
At first, in solvent, its molar concentration is 0.01-0.5mol/L, stirs to add NaOH, potassium hydroxide or ammonia spirit after 5-30 minute with one or more mixed dissolutions in the slaines such as raw material cerium salt or cerium salt and lanthanum, iron, titanium, aluminium, manganese; Then, stir precipitation reaction took place in 10-60 minute, will precipitate and clean to neutrality with secondary deionized water; Then, will be deposited in the absolute ethyl alcohol and soak, stir except that after anhydrating, and at 80-120 ℃ of dry 8-12 hour, obtain cerium base arsenic removal material, its granularity is 5-20nm.
The preparation method of said nano hydrated cerium oxide base arsenic removal material; The mol ratio of NaOH, potassium hydroxide or ammoniacal liquor and raw material is 3: 1-6: 1, and the mol ratio of cerium salt and other slaines (one or more in the slaines such as lanthanum, iron, titanium, aluminium, manganese) is 10%～100%.
The preparation method of said nano hydrated cerium oxide base arsenic removal material, cerium salt can be cerous nitrate or cerous sulfate.
The preparation method of said nano hydrated cerium oxide base arsenic removal material, slaine can be villaumite, sulfate, nitrate or the alkoxide of lanthanoid metal, iron, titanium, aluminium or manganese.
The preparation method of said nano hydrated cerium oxide base arsenic removal material, solvent is the ethanol water of water, absolute ethyl alcohol or different proportionings.
The application of said nano hydrated cerium oxide base arsenic removal material, nano hydrated cerium oxide base arsenic removal material is after overload, but advantages of simplicity and high efficiency is removed the arsenic contamination in the natural water area, and the use amount of nano hydrated cerium oxide base arsenic removal material is 0.01-0.1g/L.
The application of said nano hydrated cerium oxide base arsenic removal material, support materials can be glass fabric, sponge, polyethylene ball, activated alumina or active carbon etc., and carrying method can be infusion process or deposition-cladding process.
The application of described nano hydrated cerium oxide base arsenic removal material is immersed in activated alumina in the cerous nitrate or the cerous sulfate aqueous solution of variable concentrations, and its molar concentration is 0.1M-2M; Time 4-6 hour; Activated alumina was pulled out at 50-70 ℃ of dry 10-14 hour, calcined 0.5-2 hour for 400-500 ℃, obtain the activated alumina of cerium oxide load; Be used for filtering containing the arsenic drinking water, use amount is 0.1-1g/L.
The present invention and comparing with prior art have the following advantages:
1, cerium base arsenic removal material preparation technology of the present invention is simple, easy to operate, need not calcining, saves energy consumption.
2, cerium base arsenic removal material of the present invention has than the high adsorption capacity and the rate of adsorption faster arsenic, and applicable pH range is wide, and stable performance can a step remove trivalent arsenic and pentavalent arsenic in anhydrating, and need not to carry out preliminary treatment, saves cost.
3, the hydrous ceria adsorbing material of gained of the present invention has bigger specific area and stronger arsenic removal ability; Through overload; But this adsorbent advantages of simplicity and high efficiency is removed the arsenic contamination in the natural water area; And need not to carry out preliminary treatment, for the purification that contains arsenic sewage and the protection of environment provide a kind of novel arsenic removal material.
Description of drawings
Fig. 1 is the XRD photo of hydrous ceria of the present invention.
Fig. 2 is the high-resolution TEM photo of hydrous ceria of the present invention.
Fig. 3 is the BET photo of hydrous ceria of the present invention.
Fig. 4 is the isothermal adsorption curve of hydrous ceria of the present invention to trivalent arsenic and pentavalent arsenic.
Fig. 5 (a)-(b) is the kinetic curve to trivalent arsenic and pentavalent arsenic of hydrous ceria of the present invention; Wherein, Fig. 5 (a) is a trivalent arsenic, and Fig. 5 (b) is a pentavalent arsenic.
Fig. 6 (a)-(d) is the SEM and the EDS photo of the glass fabric before and after the load cerium oxide of the present invention.Wherein, Fig. 6 (a)-(b) is the SEM shape appearance figure of the glass fabric before the load cerium oxide; Fig. 6 (c)-(d) is the SEM shape appearance figure of the glass fabric behind the load cerium oxide.
Fig. 7 is the glass fabric arsenic removal testing arrangement sketch map of load cerium oxide of the present invention.
Fig. 8 (a)-(b) is the kinetic curve of the glass fabric of load cerium oxide of the present invention to trivalent arsenic and pentavalent arsenic; Wherein, Fig. 8 (a) is a trivalent arsenic, and Fig. 8 (b) is a pentavalent arsenic.
Fig. 9 is the dynamic breakthrough experiment result of the activated alumina of load cerium oxide to trivalent arsenic and pentavalent arsenic.
The arsenic removal test result of Figure 10 for using the CFT arsenic removal material that Yunnan Yang Zonghai lake water is carried out.
The specific embodiment
2.17g six nitric hydrate ceriums are dissolved in the 200ml ethanol solution, stir adding 0.8g NaOH after 10 minutes, then stirred 20 minutes, deposition becomes glassy yellow by dark-brown.The deposition that obtains is cleaned to neutrality with secondary deionized water, in absolute ethyl alcohol, soak then, stir remove anhydrate after, 100 ℃ of dryings 10 hours, obtain nano hydrated cerium oxide arsenic removal material.Can find out that from XRD result shown in Figure 1 the present invention is prepared to be hydrous ceria, particle diameter is about 4nm, and is consistent with high-resolution TEM result shown in Figure 2.
The nitrogen adsorption-desorption curve of the nano hydrated cerium oxide that Fig. 3 goes out for the present invention is prepared, test gained specific area is 198m
2/ g.
The nano hydrated cerium oxide that obtains is used for doing the arsenic adsorption isothermal curve, and (adding the nano hydrated cerium oxide of 0.1g/L in the arsenic solution of 1ppm～100ppm), is 25 ℃ in temperature at the different initial concentrations of 100mL; PH carries out adsorption experiment under 7 the condition; Mixing time is 24 hours, and the isothermal adsorption curve that obtains is as shown in Figure 4, the accords with Langmuir Adsorption Model; Can know that through calculating to arsenious saturated extent of adsorption be 152.3mg/g, be 107mg/g to the saturated extent of adsorption of pentavalent arsenic.
The nano hydrated cerium oxide that obtains is used for doing arsenic dynamics adsorption curve.Arsenious initial concentration is 124 μ g/L, and the initial concentration of pentavalent arsenic is 92 μ g/L, and arsenic solution pH value is all in nearly neutrality.Arsenic solution in this instance is not done any preliminary treatment; The nano hydrated cerium oxide (0.01g/L, 0.015g/L, 0.02g/L) of difference amount is joined in the arsenic solution of 1L and stir; Getting once at set intervals, appearance is tested; Obtain the kinetic curve of trivalent arsenic and pentavalent arsenic concentration changes with time, as shown in Figure 5.When nano hydrated cerium oxide gets consumption and only 0.02g/L is arranged; Just can in 1 hour, trivalent arsenic and pentavalent arsenic be reduced to below the 10ppb from about 100ppb; If prolong arsenic removal time to 5 hour; Only can trivalent arsenic and pentavalent arsenic be reduced to below the 10ppb, reach arsenic content standard in the drinking water of World Health Organization regulation with the nano-cerium oxide arsenic removal material of 0.01g/L.
2.17g six nitric hydrate ceriums are dissolved in the 200ml ethanol solution, stir adding 0.8g NaOH after 10 minutes, then stirred 20 minutes, deposition becomes glassy yellow by dark-brown.The precipitate with deionized water that obtains is cleaned to neutrality, will be deposited in the absolute ethyl alcohol soak, stir remove anhydrate after, 100 ℃ of dryings 10 hours, obtain cerium base arsenic removal material.Cerium base arsenic removal material is ultrasonic to be distributed in the 200mL deionized water; The glass fabric dipping is taken out after wherein about 1 minute; 100 ℃ of dryings 3 hours; Promptly obtain the glass fabric of load cerium oxide, the glass fabric of the load cerium oxide that obtains is repeatedly flooded, obtain the glass fabric of the load cerium oxide of repeatedly load.Glass fabric to before and after the load is weighed, and can calculate the load capacity of material.
Quality after load capacity (%)=(the preceding quality of quality-load after the load)/load
The load capacity of table 1. different loads number of times
| The load number of times | Before the load (g) | After the load (g) | Load capacity (%) | Clean back (g) | Load capacity (%) |
| 1 | 0.3543 | 0.396 | 10.53％ | 0.3893 | 8.99％ |
| 2 | 0.4266 | 0.5175 | 17.57％ | 0.5046 | 15.46％ |
| 3 | 0.4058 | 0.5229 | 22.39％ | 0.5063 | 19.85％ |
| 5 | 0.4331 | 0.6539 | 33.77％ | 0.6052 | 28.44％ |
The SEM photo of the different amplification of the glass fabric (load capacity is 8.99%) of the load cerium oxide that Fig. 6 prepares for the present invention and EDS analyze.Can find out that cerium oxide particle is dispersed on the glass fabric well, and is firm with matrix bond.
The glass fabric of the load cerium oxide that the present invention prepares is fit to handle by the lake water of arsenic contamination.Using load capacity is that cerium oxide/glass fabric sorbing material of 8.99% is used for doing arsenic dynamics adsorption curve.Experimental provision is as shown in Figure 7, and 1 is the steel wire of the glass fabric of dead load cerium oxide; 2 is the beaker of 500mL; 3 for the glass fabric adsorbent of load cerium oxide; 4 is the arsenic solution with the deionized water preparation; 5 is magneton; 6 is magnetic stirring apparatus; 7 is support.Arsenic solution 4 with the deionized water preparation is housed in the beaker 2 of 500mL; Beaker 2 bottoms of 500mL are provided with magneton 5; Magneton 5 belows are provided with magnetic stirring apparatus 6; Steel wire 1 one ends of the glass fabric of dead load cerium oxide are connected in support 7, and the glass fabric adsorbent 3 of other end suspension load cerium oxide is in the arsenic solution 4 with the deionized water preparation.This tests employed trivalent arsenic initial concentration is 85 μ g/L, and the pentavalent arsenic initial concentration is 89 μ g/L, and arsenic solution pH value is all in nearly neutrality.Arsenic solution in this instance is not done any preliminary treatment.With the 0.04g load capacity is that cerium oxide/glass fabric of 8.99% is fixed on the steel wire that is hanging; Put in the 400mL arsenic solution, magnetic agitation, getting once at set intervals, appearance is tested; Obtain the kinetic curve of trivalent arsenic and pentavalent arsenic concentration changes with time, as shown in Figure 8.When the glass fabric of load cerium oxide only has 0.1g/L, just can in 2 hours, trivalent arsenic and pentavalent arsenic be reduced to below the 10ppb, reach arsenic content standard in the drinking water of World Health Organization regulation.
With activated alumina (sphere; Diameter 3-5mm) was immersed in the cerous nitrate aqueous solution of variable concentrations (0.1M, 0.2M, 0.5M, 2M) 5 hours; Activated alumina is pulled out 60 ℃ of dryings 12 hours, and 450 ℃ of calcinings promptly obtained the activated alumina of load cerium oxide in 1 hour.
The activated alumina load capacity and the specific area of table 2. load cerium oxide
| Al 2O 3 | 0.1M | 0.2M | 0.5M | 2M | |
| Load capacity (%) | 0 | 4.8 | 7.6 | 13.7 | 15.6 |
| Specific area (m 2/g) | 231.7 | 215.4 | 210.8 | 180.8 | 146.7 |
With cerium oxide load capacity in the present embodiment is that 15.6% sample is used for carrying out dynamic penetration test, the activated alumina of load cerium oxide is filled into (Φ 10 * 150cm), and the control flow velocity is at 2ml/min, and initial arsenic concentration is 60ppb in the glass tube.Collect at set intervals and flow out liquid, measure wherein arsenic concentration, it is as shown in Figure 9 to obtain the result.As can beappreciated from fig. 9; When arsenic concentration is 60ppb in initial soln; What the aluminium oxide behind the load cerium oxide can be handled 10000 volumes contains the trivalent arsenic aqueous solution; That can handle 14000 volumes contains the pentavalent arsenic aqueous solution, all can make arsenic content standard in its drinking water that reaches World Health Organization's regulation.
The activated alumina of the load cerium oxide of preparing in the present embodiment can be used for filtering containing the arsenic drinking water, and device is simple, and is easy to use.
With 0.01mol Ce (NO
3)
3.6H
2O is dissolved in the absolute ethyl alcohol of 100ml, then titanium sulfate, ferric nitrate is joined in the cerous nitrate solution one by one, and the mol ratio that makes titanium sulfate, ferric nitrate and cerous nitrate is 1: 1: 1, stirs 0.5 hour, obtains transparent cerium, iron, titanium mixing salt solution.Simultaneously, join in the above mixing salt solution in the NaOH ethanolic solution with 100ml 1mol/L, produce a large amount of yellowish-brown flocculent deposits immediately.Continue to stir after 1 hour, deposition leached, repeatedly clean with secondary deionized water, will be deposited in the absolute ethyl alcohol soak, stir remove anhydrate after, 80 ℃ of dryings 6 hours are ground and can be obtained the CFT arsenic removal material after 10 minutes.
The arsenic removal test result of Figure 10 for using the CFT arsenic removal material that Yunnan Yang Zonghai lake water is carried out; When the consumption of CFT material only is 0.01g/L; Though contain the competing ions (as shown in table 3) of multiple interference effect of removing arsenic in the extra large lake water of sun ancestor; But the sun extra large lake water of ancestor (67ppb) that also can in 3 hours, will contain arsenic is handled below the 10ppb, reaches arsenic safety standard in the drinking water.
Table 3. Yunnan Yang Zong seawater matter is analyzed data
| Ionic species | F - | Cl - | NO 3 - | SO 4 2- | HCO 3 - | Na | K | Ca | Mg | Fe |
| Content (mg/L) | 0.54 | 5.77 | 1.08 | 121.91 | 89 | 170 | 5 | 24 | 29 | ＜1 |
The specific area of the prepared CFT arsenic removal material of this embodiment can reach 347m
2/ g have excellent effect of removing arsenic, and price is relatively cheap, and the preparation method is simple, is a kind of desirable arsenic removal material.
Claims (9)
1. nano hydrated cerium oxide base arsenic removal material, it is characterized in that: this arsenic removal material component contains the nanoscale cerium oxide particle; Perhaps; Contain in nanoscale cerium oxide particle and nano level lanthana, lanthanum hydroxide, iron oxide, iron hydroxide, titanium oxide, manganese oxide, the alumina particle one or more simultaneously; The mol ratio of one or more in cerium oxide particle and lanthana, lanthanum hydroxide, iron oxide, iron hydroxide, titanium oxide, manganese oxide, the aluminium oxide is 10%～100%, and its surface area reaches 200-500m
2/ g.
2. the preparation method of the described nano hydrated cerium oxide base arsenic removal material of claim 1 is characterized in that, comprises the steps:
At first, in solvent, its molar concentration is 0.01-0.5mol/L, stirs to add NaOH, potassium hydroxide or ammonia spirit after 5-30 minute with one or more mixed dissolutions in the slaine of raw material cerium salt or cerium salt and lanthanum, iron, titanium, aluminium, manganese; Then, stir precipitation reaction took place in 10-60 minute, will precipitate and clean to neutrality with secondary deionized water; Then, will be deposited in the absolute ethyl alcohol and soak, stir except that after anhydrating, and at 80-120 ℃ of dry 8-12 hour, obtain cerium base arsenic removal material, its granularity is 5-20nm.
3. according to the preparation method of the described nano hydrated cerium oxide base arsenic removal material of claim 2; It is characterized in that; The mol ratio of NaOH, potassium hydroxide or ammoniacal liquor and raw material is 3: 1-6: 1, and one or more mol ratio is 10%～100% in the slaine of cerium salt and lanthanum, iron, titanium, aluminium, manganese.
4. according to the preparation method of the described nano hydrated cerium oxide base arsenic removal material of claim 2, it is characterized in that cerium salt is cerous nitrate or cerous sulfate.
5. according to the preparation method of the described nano hydrated cerium oxide base arsenic removal material of claim 2, it is characterized in that slaine is villaumite, sulfate, nitrate or the alkoxide of lanthanum, iron, titanium, aluminium or manganese.
6. according to the preparation method of the described nano hydrated cerium oxide base arsenic removal material of claim 2, it is characterized in that solvent is the ethanol water of water, absolute ethyl alcohol or different proportionings.
7. the application of the described nano hydrated cerium oxide base arsenic removal material of claim 1; It is characterized in that; Nano hydrated cerium oxide base arsenic removal material is used for removing the arsenic contamination of natural water area after overload, the use amount of nano hydrated cerium oxide base arsenic removal material is 0.01-0.1g/L.
8. according to the application of the described nano hydrated cerium oxide base arsenic removal material of claim 7, it is characterized in that support materials is glass fabric, sponge, polyethylene ball, activated alumina or active carbon, carrying method is infusion process or deposition-cladding process.
9. according to the application of the described nano hydrated cerium oxide base arsenic removal material of claim 7, it is characterized in that, activated alumina is immersed in the cerous nitrate or the cerous sulfate aqueous solution of variable concentrations; Its molar concentration is 0.1M-2M, time 4-6 hour, activated alumina is pulled out at 50-70 ℃ of dry 10-14 hour; Calcined 0.5-2 hour for 400-500 ℃; Obtain the activated alumina of cerium oxide load, be used for filtering containing the arsenic drinking water, use amount is 0.1-1g/L.
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