CN102145914A - Method for preparing nano zinc oxide - Google Patents
Method for preparing nano zinc oxide Download PDFInfo
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- CN102145914A CN102145914A CN 201110049055 CN201110049055A CN102145914A CN 102145914 A CN102145914 A CN 102145914A CN 201110049055 CN201110049055 CN 201110049055 CN 201110049055 A CN201110049055 A CN 201110049055A CN 102145914 A CN102145914 A CN 102145914A
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- zine oxide
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Abstract
The invention relates to application of nano zinc oxide in removal of heavy metal (copper or lead) ions from water, which belongs to the technical field of water treatment. An application method of the nano zinc oxide comprises the following steps of: (1) synthesizing the nano zinc oxide; (2) adsorbing copper ions or lead ions in the water by using the nano zinc oxide; and (3) testing the adsorption capacity of the nano zinc oxide to the copper ions or the lead ions. The method is high in adsorption speed and adsorption capacity and is easy and convenient to operate and equipment is simple; and by the method, the copper ions or the lead ions are easy to remove from the water on a large scale.
Description
Technical field
The present invention relates to a kind of nano-ZnO preparation, belong to water-treatment technology field.
Background technology
Copper is the necessary bioelement of a kind of human body.Lack copper in the body, can cause the function corresponding obstacle, even can't form blood, lose basic life condition; But human body if in diet the excess intake copper, also easily cause vomiting, spasm, tic, even toxicity symptom such as death.Lead is a kind of cumulative toxicant that acts on each system of human body whole body and organ, mainly influences human nerve, hematopoiesis, digestion, system and kidney such as cardiovascular, can cause illnesss such as autonomic nervous dysfunction, anaemia, hypoimmunity.Because it is copper, lead ion can not be harmless material by biological degradation, have long-term persistence in environment, therefore very important to the removal of copper, lead ion in the water.
The method of Treatment of Copper, lead ion waste water has at present: chemical coagulation-sedimentation method, absorption method, ion exchange method, electrolytic process, reverse osmosis method, membrane technique etc.Wherein the economy and the high efficiency that show when handling low concentration heavy metal water of absorption method is subjected to extensive concern just day by day.
Nano material is described as the novel material of 21 century.The generalized nano material is meant the various solid-state materials that have at least one dimension to be in nano-scale in the three-dimensional dimension.Owing to have volume effect, surface effects, quantum size effect, dielectric confinement effect and macro quanta tunnel effect etc., nano material has shown the not available many unusual light of body phase material, heat, magnetic and chemical property.Wherein the most noticeable is along with the reducing of nano particle diameter, and its surface tension and surface energy increase, and make most of atom instability, easily and other atomic linkages, thereby shows very high chemically reactive.In recent years, the development and use of nano material have caused people's attention, its synthetic method economy, simple, especially the specific surface area of nano material is big, loading capacity is big, is used as a kind of sorbent material just more and more, is applied in the research of removing heavy metal ion in the water.
Summary of the invention
The object of the present invention is to provide a kind of nano-ZnO preparation.
A kind of nano-ZnO preparation of the present invention is characterized in that having following process and step:
A. 1:1 prepares the Zn (NO of equal volume respectively in molar ratio
3)
26H
2O and (NH
4)
2CO
3The aqueous solution; At first under agitation heat Zn (NO
3)
26H
2O solution to 50 ℃ adds an amount of Triton X-100 (Triton X-100) then, and dropwise adds the above-mentioned (NH for preparing
4)
2CO
3Solution; Behind the reaction 30min, regulate pH value to 9～10 of above-mentioned reaction solution with NaOH solution; Its reaction is continued to make in back elevated temperature to 80～90 ℃, and continuous stirring reaction 1～2 hour;
B. reaction is left standstill cooling after finishing, and shifts out lower floor's material, uses deionized water and dehydrated alcohol supersound washing then respectively; Centrifugation subsequently, and, finally make nano zine oxide 60 ℃ of following vacuum-dryings 24 hours.
The purposes of the prepared nano zine oxide of a kind of nano-ZnO preparation is its application method, is heavy metal copper or the lead ion of removing in the water; Its treatment process is as follows:
Get an amount of environmental water sample, through 0.45 μ m micro-pore-film filtration; Regulating pH value with phosphate buffer solution then is 4.0～5.0, adds the above-mentioned nano zine oxide 0.025～0.045g that makes, centrifugation behind vibration 15～30min; Draw the supernatant liquid of above-mentioned solution then, measure the amount of being adsorbed of cupric ion or lead ion with graphite furnace atomic absorption spectrometry.
Advantage of the present invention and characteristics are as described below:
(1) nano zine oxide has characteristics such as rate of adsorption is fast, high adsorption capacity.
(2) the inventive method is easy and simple to handle, equipment is simple, consuming time less, the efficient height, be easy to mass-producing and remove cupric ion or lead ion in the water.
Description of drawings
Fig. 1 is adsorption isothermal line (1a) and the adsorptive capacity curve (1b) of the nano zine oxide in the research trial of the present invention to cupric ion.
Fig. 2 is adsorption isothermal line (2a) and the adsorptive capacity curve (2b) of the nano zine oxide in the research trial of the present invention to lead ion.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment
The preparation process of present embodiment nano zine oxide is as described below:
(1) Zn (NO of preparation 0.25 mol/L
3)
26H
2O solution 50 mL, (the NH of 0.25 mol/L
4)
2CO
3Solution 50 mL.
(2) stir down heating Zn (NO
3)
26H
2O solution to 50 ℃ adds 1 mL Triton X-100, and dropwise adds (NH
4)
2CO
3Solution; After reacting 30 min, be 10 with the pH value of the NaOH solution conditioned reaction liquid of 1 mol/L; Rising temperature of reaction to 80 ℃ continues to stir 1 h.
(3) reaction is left standstill cooling after finishing, and shifts out lower floor's material, uses deionized water and dehydrated alcohol ultrasonic respectively, centrifuge washing, and, finally make nano zine oxide at 60 ℃ of following vacuum-drying 24 h.
The application of nano zine oxide cupric ion in removing environmental water sample, its concrete steps are as described below:
(1) get this laboratory from the beginning water sample and on dissolve the pond water sample greatly, respectively through 0.45 μ m micro-pore-film filtration, regulating the pH value with phosphate buffer solution is 5.0, adds 0.0250 g nano zine oxide, centrifugal behind 15 min that vibrate.
(2) draw the supernatant liquid of above-mentioned solution respectively, measure the amount of being adsorbed of cupric ion with graphite furnace atomic absorption spectrometry.Nano zine oxide is as shown in table 1 to the removal experimental result of cupric ion in the environmental water sample.
Table 1 nano zine oxide is to the removal experiment of cupric ion in the environmental water sample
In this experiment, adopt and draw supernatant liquid, and by the hot adsorptive capacity of calculating indirect measurement nano zine oxide counterweight metal copper ion.
Relevant applied research test of the present invention
Applied research test 1
The application of nano zine oxide cupric ion in removing water, concrete steps are as follows:
(1) be respectively in the copper ion solution of 1 mg/L, 2 mg/L, 5 mg/L, 10 mg/L, 20 mg/L, 30 mg/L and 40 mg/L in concentration, regulating the pH value with phosphate buffer solution is 5.0, adds 0.0250 g nano zine oxide, centrifugal behind 15 min that vibrate.
(2) draw the supernatant liquid of above-mentioned solution respectively, measure the amount of being adsorbed of cupric ion with graphite furnace atomic absorption spectrometry.Nano zine oxide to the adsorption isothermal line of cupric ion and loading capacity curve referring to Fig. 1.By Fig. 1 (b), nano zine oxide to the loading capacity curve of cupric ion as can be known, its maximum adsorption capacity is 13.85 mg/g.
Applied research test 2
The application of nano zine oxide lead ion in removing water, concrete steps are as follows:
(1) is respectively in the lead ion solution of 2 mg/L, 5 mg/L, 10 mg/L, 30 mg/L, 50 mg/L, 100 mg/L and 200 mg/L in concentration, regulating the pH value with phosphate buffer solution is 4.0, add 0.0450 g nano zine oxide, centrifugal behind 60 min that vibrate.
(2) draw the supernatant liquid of above-mentioned solution respectively, measure the amount of being adsorbed of lead ion with graphite furnace atomic absorption spectrometry.Nano zine oxide to the adsorption isothermal line of lead ion and loading capacity curve referring to Fig. 2.Fig. 2 (b), nano zine oxide to the loading capacity curve of lead ion as can be known, its maximum adsorption capacity is 104.8 mg/g.
To using the explanation of test and accompanying drawing thereof
Application test example 1,2 is respectively the experimentation of nano zine oxide to cupric ion, the volumetric determination of lead ion Static Adsorption.Loading capacity is to weigh an important indicator of adsorbents adsorb performance, and its size has determined the amount of the sorbent material that need drop into when the Treatment Analysis thing.
With nano zine oxide in removing water cupric ion be applied as example, figure (1a) is a nano zine oxide absorbing copper ionic isothermal curve, when the cupric ion in the solution is adsorbed by nano zine oxide, adsorptive capacity increases with the increase of starting point concentration, when the starting point concentration of cupric ion was more and more higher, the rangeability of adsorptive capacity was more and more littler, after reaching a certain value, its adsorptive capacity no longer increases, and has promptly reached the maximal absorptive capacity of nano zine oxide to cupric ion.C among the figure
EThe concentration (mg/L) of cupric ion to be measured in the solution when referring to adsorption equilibrium, Q
EThe amount (mg/g) of the adsorbed cupric ion to be measured of every gram sorbent material when referring to adsorption equilibrium.
Fig. 1 (b) is the loading capacity curve of nano zine oxide to cupric ion, and this curve meets the Langmuir model of correction:
Wherein b is Langmuir constant (L/mg), Q
0Be the maximum adsorption capacity (mg/g) of nano zine oxide, can get by the inverse that calculates the loading capacity rate of curve to cupric ion.The loading capacity curvilinear equation is among Fig. 1 (b):
, that is, calculating can get Q
0Be 13.85 mg/g.
In like manner, in figure (2b), nano zine oxide to the loading capacity curvilinear equation of lead ion is:
Claims (2)
1. nano-ZnO preparation is characterized in that having following process and step:
A. 1:1 prepares the Zn (NO of equal volume respectively in molar ratio
3)
26H
2O and (NH
4)
2CO
3The aqueous solution; At first under agitation heat Zn (NO
3)
26H
2O solution to 50 ℃ adds an amount of Triton X-100 (Triton X-100) then, and dropwise adds the above-mentioned (NH for preparing
4)
2CO
3Solution; Behind the reaction 30min, regulate pH value to 9～10 of above-mentioned reaction solution with NaOH solution; Its reaction is continued to make in back elevated temperature to 80～90 ℃, and continuous stirring reaction 1～2 hour;
B. reaction is left standstill cooling after finishing, and shifts out lower floor's material, uses deionized water and dehydrated alcohol supersound washing then respectively; Centrifugation subsequently, and, finally make nano zine oxide 60 ℃ of following vacuum-dryings 24 hours.
2. the purposes of the prepared nano zine oxide of the described a kind of nano-ZnO preparation of claim 1 is its application method, is heavy metal copper or the lead ion of removing in the water; Its treatment process is as follows:
Get an amount of environmental water sample, through 0.45～μ m micro-pore-film filtration; Regulating pH value with phosphate buffer solution then is 4.0～5.0, adds the above-mentioned nano zine oxide 0.025～0.045g that makes, centrifugation behind vibration 15～30min; Draw the supernatant liquid of above-mentioned solution then, measure the amount of being adsorbed of cupric ion or lead ion with graphite furnace atomic absorption spectrometry.
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| CN 201110049055 CN102145914A (en) | 2011-03-02 | 2011-03-02 | Method for preparing nano zinc oxide |
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|---|---|---|---|
| CN 201110049055 CN102145914A (en) | 2011-03-02 | 2011-03-02 | Method for preparing nano zinc oxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109467248A (en) * | 2018-12-27 | 2019-03-15 | 浙江大学 | Small-sized river water cleaning device based on zinc oxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060021945A1 (en) * | 2004-07-29 | 2006-02-02 | Board Of Trustees Of Michigan State University | Synthetic layered silicate nanolayers |
| CN101785982A (en) * | 2010-02-05 | 2010-07-28 | 北京化工大学 | Method for preparing hollow nanospheres by a hot emulsion method |
| CN101825569A (en) * | 2010-01-21 | 2010-09-08 | 上海大学 | Application of ZnSe nano fluorescence probe material in detecting copper ion or nickel ion |
-
2011
- 2011-03-02 CN CN 201110049055 patent/CN102145914A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060021945A1 (en) * | 2004-07-29 | 2006-02-02 | Board Of Trustees Of Michigan State University | Synthetic layered silicate nanolayers |
| CN101825569A (en) * | 2010-01-21 | 2010-09-08 | 上海大学 | Application of ZnSe nano fluorescence probe material in detecting copper ion or nickel ion |
| CN101785982A (en) * | 2010-02-05 | 2010-07-28 | 北京化工大学 | Method for preparing hollow nanospheres by a hot emulsion method |
Non-Patent Citations (2)
| Title |
|---|
| 《中南民族大学学报(自然科学版)》 20070630 詹国庆等 纳米氧化锌的制备表征及其对Cu(Ⅱ)、Co(Ⅱ)、Fe(Ⅲ)的吸附 第19-21页 权利要求2 第26卷, 第2期 * |
| 《稀有金属材料与工程》 20040930 贾晓林等 均匀沉淀法制备ZnO纳米粉体 第992-995页 权利要求1 第33卷, 第9期 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109467248A (en) * | 2018-12-27 | 2019-03-15 | 浙江大学 | Small-sized river water cleaning device based on zinc oxide |
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Application publication date: 20110810 |