CN105498677A - Preparation method and applications of dye-selective adsorbent - Google Patents
Preparation method and applications of dye-selective adsorbent Download PDFInfo
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- CN105498677A CN105498677A CN201410487672.XA CN201410487672A CN105498677A CN 105498677 A CN105498677 A CN 105498677A CN 201410487672 A CN201410487672 A CN 201410487672A CN 105498677 A CN105498677 A CN 105498677A
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Abstract
The present invention discloses a method for mass preparation of a dye-selective adsorbent, and applications of the dye-selective adsorbent. According to the method, evaporation plating is performed on a raw material WO3 powder at a temperature of 500-1000 DEG C under a pressure of about 10<-3> in a vacuum environment by using a conventional thermal evaporation method, the evaporated tungsten oxide vapor contacts coldness and over-saturates at a hemisphere-shaped deposition cover position to deposit so as to form an amorphous WO3 thin film comprising micro-nano-scale particles or thin sheets, the film product on the deposition cover is subjected to scraping or ultrasonic shocking, and drying is performed to obtain the powder, wherein the powder is the adsorbent. The adsorbent prepared by the method of the present invention has the following two characteristics that: 1, the adsorbent has a strong cationic dye molecule adsorption effect, but does not adsorb anionic dye molecules adsorbed or adsorbs trace anionic dye molecules so as to present the selective adsorption characteristic, such that the adsorbent can be used in the dye separation technology; and 2, after the adsorbent adsorbs the dye to achieve a saturated state, the adsorbent can be automatically deposited on the bottom portion of the solution in a precipitate manner, such that the adsorbent is easy to filter and separate from the solution, and the broad application prospects are provided in the fields of dye wastewater treatment, low carbon life, energy-saving and emission-reducing, and the like.
Description
Technical field
The present invention discloses a kind of preparation method of dye selection adsorbent and the application in sewage disposal and dye separation technology thereof.
Background technology
The output of China's dyestuff in 2013 is 89.5 ten thousand tons, accounts for Gross World Product 60%, belongs to undisputed dyestuff big country, but in DYE PRODUCTION and use procedure, nearly 10-20% enters in water, causes the pollution to water resource, and waste water from dyestuff has become one of environment major polluting sources.Waste water from dyestuff contains organic matter and the salt of large amount of complex, has CODCr(chemical oxygen consumption (COC)) high, the feature such as color and luster is dark, Acidity of Aikalinity is strong, bring very large difficulty to wastewater treatment.At present, conventional processing method has Physical, chemical method and bioanalysis, and the process conditions of chemical method are high, easily produce secondary pollution; The efficiency of bioanalysis decolouring fungi is not high, and decolouring scope is single; Physical comprises UF membrane and absorption method, and UF membrane is expensive, and absorption method has twice laid, operating procedure is simple, but absorption regeneration is poor, and adsorbance is little.The most frequently used in the absorption method of physics is the material of the porous such as active carbon, activated coal, graphite and natural montmorillonite or activation, but this type of material is comparatively insoluble in water, is dissolved in swimming in the water surface in adsorption process, reduces with dye contacts, causes the rate of discoloring low.Therefore, research that is cheap and easy to get, that remove the adsorbent of dyestuff in water is efficiently subject to people and pays close attention to widely.
Summary of the invention
What the present invention solved is problem for Treatment of Cationic Dyestuff Wastewater, provides a kind of preparation method of dye of positive ion adsorbent and the application of dye separation technology.
A kind of dye of positive ion adsorbent of the present invention is tungstic acid thin slice or the particle of amorphous, and it is as follows that it prepares scheme:
(1) tungstic acid (99.9%) is put into the heating vessel of carrying as evaporation source, then add a cover deposition shield;
(2) open pumped vacuum systems to vacuumize, treat that vacuum reaches 1.0 × 10
-2-3 × 10
-3pa;
(3) open evaporation source heating system, heat evaporation source, heating-up temperature is 500-1000 DEG C;
(4) after evaporation process, deposition shield is taken out, add wherein and put into ultrasonic oscillator after helping release agent liquid such as () deionized waters and isolate amorphous tungstic acid;
(5) amorphous tungstic acid adsorbent is obtained after drying.
Adsorbent of the present invention has good adsorption effect to the dye of positive ion, be embodied in cationic absorption such as rhodamine, methylene blue, crystal violet, basic fuchsins, the rate of discoloring can reach 50-80%, and arrives the easy isolated by filtration of the saturated rear formation particle coagulation of absorption.
The selective absorption characteristic of adsorbent of the present invention can with dye separation technology, the dye of positive ion that can adsorb and not adsorbable anionic dye carry out crude separation.
Accompanying drawing explanation
Fig. 1 material preparation facilities schematic diagram, WO in deposition shield
3powder is heating sublimation at high temperature, and phase feed carries out meeting cold supersaturation sedimentation in the deposition shield of upper half-space, forms the amorphous oxide W film be made up of the thin slice of micro-nano size or particle.
Fig. 2 material morphology and structural characterization schematic diagram, in figure (a), scanning electron microscope diagram is shown as flake structure, figure (b), (c), (d), (e) are respectively X-ray diffraction spectrum, transmission electron microscope figure and SEAD figure, show that the crystal structure of thin slice is amorphous tungstic acid.
Fig. 3 is adsorbent (3.5mg) is that 25mg/L methylene blue dye solution carries out adsorbing test to 30ml concentration: (a) is the absorption spectrum before and after absorption, after absorption, the color of solution shoals significantly, peak value in absorption spectra significantly weakens, and has blue precipitate to separate out in solution; The relation of b adsorbance that () is adsorbent and methylene blue solution concentration: along with the increase of concentration, adsorbance substantially linearly increases.The critical concentration that the illustration of figure (b) marks when sediment appears in solution is 20mg/L.
Fig. 4 tests the adsorption effect statistical chart of seven kinds of typical dye, can find out in figure that the adsorbent of preparation has good suction-operated to cations such as rhodamine B, methylene blue, crystal violet, basic fuchsins, the rate of discoloring is 30-70%, and the anionic dyes such as methyl orange, eriochrome black T, acid chrome blue K are shown as to trace or do not adsorb.
Fig. 5 selective absorbent is applied to the embodiment of dye separation, from color and absorption spectrum, show the dyestuff that this adsorbent effectively can be separated methylene blue and methyl orange two kinds of different band electric groups.
Detailed description of the invention
Below in conjunction with accompanying drawing and preferred case study on implementation feature that adsorbent has is prepared to the present invention and specific implementation process is further elaborated, its object is to content of the present invention is better described, but not limit the scope of the invention.
embodiment 1: separate out with precipitated form after adsorbent is saturated
First, 1.0gWO is weighed
3powder puts into the boat of heating, evenly spreads out, and then vacuumizes, when vacuum arrives 4.0 × 10
-3during Pa, start to heat up.Lower the temperature be incubated 30min at 700 DEG C after, deposition shield is put into deionized water and carry out ultrasonic, the powder under shake is adsorbent after drying.
Secondly, configure each two groups of the methylene blue dye solution 30ml of variable concentrations respectively, the absorbent powder of load weighted 3.5mg is put into wherein in all solution of a group, other one group as a comparison, after leaving standstill a period of time, (3 hours) carry out absorption spectrum test respectively, same adsorbance is defined as the adsorbent dyestuff quality of unit mass, and formulate is:
, as shown in Figure 3, (a) contrasts with the absorption spectrum do not added for adding absorption, and after absorption, the color of solution shoals significantly, and the peak value in absorption spectrum significantly weakens, and sediment is separated out, and is easy to adsorbent and is separated from dye solution; The relation of b adsorbance that () is adsorbent and the concentration of methylene blue, in figure, curve shows the increase along with concentration, and adsorbance substantially linearly increases, and the adsorbance of adsorbent is up to 600mg/g.What the illustration of scheming (b) provided is that solution occurs that sedimentary critical concentration is at 20mg/L place: after having adsorbed lower than 20mg/L, and deposit-free is separated out, and higher than 20mg/L, starts to occur that sediment is separated out.
embodiment 2: the selective absorption characteristic of adsorbent
First, 1.0gWO is weighed
3powder puts into the boat of heating, evenly spreads out, and then vacuumizes, when vacuum arrives 1.0 × 10
-3during Pa, start to heat up.Lower the temperature be incubated 20min at 600 DEG C after, deposition shield is put into deionized water and carry out ultrasonic, the powder under shake is adsorbent after drying.
Secondly, configure the methylene blue of finite concentration (as 25mg/L or 30mg/L), crystal violet, the representative dye of positive ion solution of basic fuchsin four kinds and methyl orange, eriochrome black T, each two groups of acid chrome blue K three kinds of representative anionic dye solution 30ml, the absorbent powder of load weighted 5.3mg is all put in all solution of a group wherein, another group solution as a control group, measures the absorption spectrum of solution respectively after leaving standstill a period of time (2 hours).Fig. 4 be test seven kinds of typical dye absorption before and after change in concentration statistical chart, can find out in figure that the adsorbent of preparation has obvious suction-operated to cations such as rhodamine B, methylene blue, crystal violet, basic fuchsins, the rate of discoloring is the change percentage that the 30-70%(rate of discoloring is defined as absorbing dye solution absorption spectra highest peak intensity before and after absorption).Adsorbent then shows as trace to anionic dyes such as methyl orange, eriochrome black T, acid chrome blue Ks or does not adsorb completely.
embodiment 3: adsorbent is applied to dye separation
First, 2.0gWO is weighed
3powder puts into the boat of heating, evenly spreads out, and then vacuumizes, when vacuum arrives 1.0 × 10
-2during Pa, start to heat up.At 800 DEG C, be incubated 30min, rear cooling, glass substrate put into deionized water and carry out ultrasonic, the powder under shake is adsorbent after drying.
Secondly, the methylene blue of configuration 25mg/L and each 15ml of methyl orange solution, then carry out being mixed to get bottle-green mixed solution according to 1:1 solution, test its absorption spectrum, the characteristic peak of methylene blue and methyl orange is contained in spectrum, then the amorphous oxide tungsten powder adsorbent of 4.5mg is added, leave standstill a period of time, the color of solution becomes brown, the absworption peak of methyl orange and the ABSORPTION EDGE of adsorbent tungsten oxide material is only there is in its absorption spectrum, and the absworption peak of methylene blue almost disappears completely, illustrate that the methylene blue molecule in solution is adsorbed to the surface of adsorbent completely, methyl orange dye molecule is only there is in solution.
Claims (7)
1. a preparation method for dye selection adsorbent, is characterized in that with high-purity WO
3powder is raw material, adopts traditional thermal evaporation process to be 1.0 × 10 in vacuum
-2-3 × 10
-3pa, temperature is evaporation under the condition of 500-1000 DEG C, and on substrate or bell jar, deposition is formed and receives the amorphous WO of micro-dimension
3thin slice or particle, its processing step is as follows:
(1) by WO
3the heating vessel putting into carrying, as evaporation source, then adds a cover deposition shield;
(2) open pumped vacuum systems to vacuumize, treat that vacuum reaches;
(3) open evaporation source heating system, heat evaporation source, heating-up temperature is 500-1000 DEG C;
(4) after evaporation process, deposition shield is taken out, add wherein and put into ultrasonic oscillator after helping release agent liquid such as () deionized waters and isolate amorphous WO
3;
(5) amorphous WO is obtained after drying
3adsorbent.
2. the preparation method according to right 1 is characterized in that the condition of evaporation be vacuum is 1.0 × 10
-2-3 × 10
-3pa, evaporating temperature is 500-1000 DEG C.
3. the preparation method according to right 1 is characterized in that the substrate chosen has the features such as large area multi-angle.
4. the preparation method according to right 1 is characterized in that preparation is WO
3, its particle size is micro-nano size, and shape is thin slice or graininess, and crystal structure is amorphous state.
5. according to right 1, the adsorbent of preparation is characterized in that having selective absorption to dyestuff, be embodied in, to cations such as rhodamine B, methylene blue, crystal violet, basic fuchsins, there is good suction-operated, to the anionic dyes such as methyl orange, eriochrome black T, acid chrome blue K then trace or do not adsorb completely.
6. according to right 1, the adsorbent of preparation has good adsorption effect to dyestuff, and adsorbance reaches as high as 200-600mg/g(for different dyes, and its adsorbance is different), and arrive the saturated rear formation sediment coagulation of absorption, easy isolated by filtration.
7. the characteristic of the selective absorption according to right 5 and 6 not only can be used for the absorption of dyestuff, also can be used for the Separation & Purification of dyestuff.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106495380A (en) * | 2016-12-21 | 2017-03-15 | 沈阳化工大学 | A kind of catalytic degradation organic dyestuff and the method for food additive sunset yellow |
| CN109364871A (en) * | 2018-11-05 | 2019-02-22 | 江苏大学 | A kind of oxygen defect type tungstic trioxide nano-slice adsorbent and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013027403A1 (en) * | 2011-08-23 | 2013-02-28 | 株式会社 東芝 | Cation adsorbent and method for processing solution using same |
| CN103252206A (en) * | 2013-05-19 | 2013-08-21 | 北京工业大学 | Flowerlike tungsten oxide hydrate adsorbent |
| CN103446993A (en) * | 2013-08-23 | 2013-12-18 | 中国工程物理研究院核物理与化学研究所 | Method for preparing tantalum (Ta)-doped wolfram (W)-oxide adsorption nano-material |
-
2014
- 2014-09-22 CN CN201410487672.XA patent/CN105498677A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013027403A1 (en) * | 2011-08-23 | 2013-02-28 | 株式会社 東芝 | Cation adsorbent and method for processing solution using same |
| CN103252206A (en) * | 2013-05-19 | 2013-08-21 | 北京工业大学 | Flowerlike tungsten oxide hydrate adsorbent |
| CN103446993A (en) * | 2013-08-23 | 2013-12-18 | 中国工程物理研究院核物理与化学研究所 | Method for preparing tantalum (Ta)-doped wolfram (W)-oxide adsorption nano-material |
Non-Patent Citations (1)
| Title |
|---|
| JIAN YI LUO等: "Strong aggregation adsorption of methylene blue from water using amorphous WO3 nanosheets，Jian Yi Luo等，《Applied Surface Science》，第287卷，第270–275页，20131001", 《APPLIED SURFACE SCIENCE》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106495380A (en) * | 2016-12-21 | 2017-03-15 | 沈阳化工大学 | A kind of catalytic degradation organic dyestuff and the method for food additive sunset yellow |
| CN109364871A (en) * | 2018-11-05 | 2019-02-22 | 江苏大学 | A kind of oxygen defect type tungstic trioxide nano-slice adsorbent and preparation method thereof |
| CN109364871B (en) * | 2018-11-05 | 2021-08-03 | 江苏大学 | Oxygen-deficient tungsten trioxide nanosheet adsorbent and preparation method thereof |
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