CN104163464B - A kind of method of utilizing Oil-tea-cake to remove Wastewater Dyes - Google Patents
A kind of method of utilizing Oil-tea-cake to remove Wastewater Dyes Download PDFInfo
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- CN104163464B CN104163464B CN201410404428.2A CN201410404428A CN104163464B CN 104163464 B CN104163464 B CN 104163464B CN 201410404428 A CN201410404428 A CN 201410404428A CN 104163464 B CN104163464 B CN 104163464B
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Abstract
The present invention relates to a kind of method of utilizing Oil-tea-cake to remove Wastewater Dyes, belong to technical field of waste water processing. Described method comprises: clean after Oil-tea-cake, pulverize and sieve, obtain Oil-tea-cake adsorbent; Described Oil-tea-cake adsorbent is joined in the waste water containing active red 15 and sodium chloride, at 20～50 DEG C, stir or vibrate after 24h, isolated by filtration, filtrate is adjusted to neutral rear discharge, completes the absorption to active red in waste water 15. In the method for the invention, in Oil-tea-cake adsorbent Adsorption waste water, active red 15 dyestuffs maximum mono layer adsorption amount of active red 15 dyestuffs at 20 DEG C is 74.63mg/g, simple to operate, with low cost, high-efficiency environment friendly.
Description
Technical field
The invention belongs to technical field of waste water processing, relate to one and utilize Oil-tea-cake to remove in waste waterThe method of dyestuff, particularly relates to one and utilizes Oil-tea-cake adsorbent to remove active red in waste waterThe method of 15 dyestuffs.
Background technology
Dyeing waste water is mainly one of harmful industrial wastewater of China, is by sources divided into printing and dyeing industry uselessWater and waste water in dye production. According to statistics, now existing more than 10000 kind of commercial dye weaved, madeThe industries such as paper, rubber, plastics, leather, cosmetics, pharmacy and food industry are applied widely.So use widely dyestuff to cause a large amount of waste water from dyestuff to be discharged in natural water. Dyestuff is uselessMost of pollutant in water is synthesis of organic substance, and intractability is larger, and biodegradability is poor. DyeMaterial contains in waste water and multiplely has bio-toxicity or cause " three cause " (carcinogenic, teratogenesis, mutagenesis)The organic matter of performance is Industrial Wastewater Treatment difficult point always. In addition, the colourity dirt of dyestuffDye even more serious, even if concentration very low (as 1mg/L) also can have a strong impact on light transmittance, and thenDestroy the ecosystem. In a large number without any processing or process waste water from dyestuff not up to standard to the mankind,Animals and plants and natural water have caused immeasurable significant damage. Active red 15 (C.I.ReactiveRed15), be a kind of azo dyes, there is the features such as bright in colour and water-fastness,Be widely used in the dyeing of wollen fabrics and chemical fibre fabric. Azo dyes is owing to having azoKey and benzene ring structure, still can make waste water maintain in mass concentration lower than 1mg/L in the situation that and holdColourity of a specified duration, and azo dyes and intermediates thereof are much three of poisonous, difficult degradationsCause material, can cause serious pollution to environment.
Biosorption process is a kind of typical low cost absorption, it be adopt dead/there is no an activityBiological substance or biogenic material remove organic or inorganic pollutant as metal,Dyestuff and stink etc. are a kind of methods of emerging processing Wastewater Pollutant. Biosorption processAs a new technology processing waste water, technology similar with other compared tool and had the following advantages: (1)Can not introduce new pollutant, environmentally friendly; (2) invest littlely, operating cost is low; (3)Biological adsorption agent is cheap, renewable, easily obtain, raw material wide material sources. Along with peopleWhat environmental protection and sustainable development were required improves constantly, based on " treatment of wastes with processes of wastes against one another " theoryEnvironmentally friendly pollutant treatment technology becomes the direction of domestic and international research and effort. Agricultural are discardedThing aboundresources, but mostly by burning, landfill or abandon, if the agricultural wastes such as stalk are in fieldBetween burn, the byproduct of food processing is taken as garbage loading embeading as shell, skin etc., forestry products addsWood chip, sawdust etc. that work produces are simply discarded, and have not only polluted environment, have also caused resourceSerious waste. In recent years, the exploitation of Cheap highly effective biological adsorption agent become both domestic and externalStudy hotspot problem. Bacterium, fungi, algae, agriculture and forestry discarded object, trade waste etc. areThrough the studied adsorbent that is developed to. Research discovery, many agriculture and forestry discarded objects only need carry out simplyProcess the superperformance that just can possess absorption Wastewater Dyes, therefore can be used as cheap lifeThing adsorbent. In recent years, researcher proposes that multiple to utilize agriculture and forestry organic waste material to prepare Cheap highly effective rawThe method of thing adsorbent, these agriculture and forestry organic waste materials comprise bamboo bits, pomelo peel, chestnut shell, sunflowerStalk, walnut shell, wood chip etc.
Oil tea is the important woody oil tree species of south China, is four large woody edible oil sources, the worldOne of seeds, equally celebrated for their achievements with oil palm, olive, coconut. The more than 90% of whole world camellia seed oil outputFrom China. When B.C. more than 100 years Emperors Wu Di of the Han dynasty, China starts to plant oil tea, existing so farMore than 2000 year history. " national camellia oleiferaindustry development plan (2009～the year two thousand twenty) " pointed out, cutOnly 2009, China's oil tea area approximately had 4,500 ten thousand mu, 1,000,000 tons of left sides of tea seed annual productionThe right side, produces approximately 260,000 tons of tea oil per year. Oil-tea-cake, claims again tea cake, the tea dregs of rice, oil cake etc., is oilThe residue obtaining after the oil expression of tea seed, its output is equivalent to 3 times of tea oil. Due to Oil-tea-cakeBitter, goes out of use at present substantially, has caused the very large wasting of resources. If the Oil-tea-cake system of utilizationActive red 15 in standby sorbent treatment waste water, not only turns waste into wealth, and is waste water from dyestuff placeReason provides a kind of new biological adsorption material, reaches the effect of " treatment of wastes with processes of wastes against one another ". At present, existingUtilize Oil-tea-cake as heavy metal nickel (Ran Xiuzhi, Yuan Hongjiang learn military affairs entirely. cake of camellia oleifera seeds biologyAdsorbent is to Ni2+Absorption property [J]. Journal of Chemical Industry and Engineering .2011 (04): 986 – 993.) adsorbentResearch, but utilize the research of Oil-tea-cake dye wastewater treatment using to have no report.
Summary of the invention
The object of the present invention is to provide one to utilize efficiently, cheaply Oil-tea-cake adsorbent to goExcept the method for active red 15 dyestuffs in waste water.
To achieve these goals, technical scheme of the present invention is as follows:
Utilize Oil-tea-cake to remove a method for Wastewater Dyes, comprising:
Step 1: after Oil-tea-cake is cleaned, dry 12～36h at 60～100 DEG C;
Step 2: after being dried, Oil-tea-cake is pulverized, and being screened to particle diameter is 0.3～0.6mm, obtainsOil-tea-cake adsorbent;
Step 3: described Oil-tea-cake adsorbent is joined to giving up containing active red 15 and sodium chlorideIn water, at 20～50 DEG C, stir or vibrate after 24h, isolated by filtration, filtrate is adjusted to after neutralityDischarge, completes the absorption to active red in waste water 15;
Described Oil-tea-cake adsorbent content in described waste water is 2～6g/L.
Wherein, described Oil-tea-cake cleans and uses distilled water to clean removal impurity.
In described waste water, the mass percent concentration of sodium chloride is 0～30%.
In described waste water, the mass concentration of active red 15 is no more than 300mg/L, is preferably no more than250mg/L。
The Initial pH of described waste water is 1～11, is preferably 1～5.
In described waste water, sodium chloride content is preferably 0%.
The invention has the beneficial effects as follows:
In the method for the invention, in Oil-tea-cake adsorbent Adsorption waste water, active red 15 dyesMaterial maximum mono layer adsorption amount of active red 15 dyestuffs at 20 DEG C is 74.63mg/g, meetsThe theory of recycling economy, has opened up the new way of Oil-tea-cake resource, and originate abundant, priceCheap. The method of the invention has solved problem of environmental pollution, and receptor 1 activity red 15 is pollutedWaste water is purified, environmentally friendly and do not cause secondary pollution. Under the prerequisite of protection of the environment,Reach the effect that turns waste into wealth, controls useless (waste water from dyestuff) with give up (agricultural wastes), at one strokeMany.
The method of the invention is simple to operate, with low cost, high-efficiency environment friendly.
Brief description of the drawings
Fig. 1 is that initial pH on wastewater is to active red 15 in Oil-tea-cake adsorbent Adsorption waste waterThe impact of dyestuff effect;
Fig. 2 be in waste water sodium chloride concentration to active in Oil-tea-cake adsorbent Adsorption waste waterThe impact of red 15 dyestuff effects;
At the beginning of Fig. 3 is the Adsorption effect and active red 15 dyestuffs of active red 15 dyestuffs in waste waterThe relation curve of beginning concentration and adsorption time;
Fig. 4 is that under the red 15 dyestuff initial concentrations of different activities, temperature is inhaled Oil-tea-cake adsorbentThe impact of active red 15 dyestuff effects in attached removal waste water;
Fig. 5 is the Langmuir of active red 15 dyestuffs in Oil-tea-cake adsorbent Adsorption waste water(Lang Gemiaoer) adsorption isotherm;
Fig. 6 is the Temkin of active red 15 dyestuffs in Oil-tea-cake adsorbent Adsorption waste water alive(Te Mujin) adsorption isotherm;
Fig. 7 is infrared spectrum (FTIR) figure of Oil-tea-cake adsorbent.
Fig. 8 a～8c is ESEM (SEM) figure of Oil-tea-cake adsorbent.
Detailed description of the invention
Further illustrate the present invention below in conjunction with specific embodiment. Be noted that following detailedIllustrate it is all exemplary, the present invention is not limited thereto. The all technology that use herein andScientific terminology has the phase of conventionally understanding with general technical staff of the technical field of the inventionSame implication.
In following examples, be to calculate adsorption capacity according to following formula:
Wherein: qeFor adsorption capacity, mg/g; C0And CeBe respectively while adsorbing initial and balanceActive red 15 concentration, mg/L; V is wastewater volume, mL; M is adsorbent mass, g.
Embodiment 1
By clean the Oil-tea-cake of removing after impurity through distilled water, under 100 DEG C of conditions, dry 12h,Through pulverizing, being screened to particle diameter is 0.3～0.6mm, obtains Oil-tea-cake adsorbent A again.
Get Oil-tea-cake adsorbent A and sodium chloride add pH value be respectively 1,2,3,5,7,9,11, contain in the waste water of active red 15 of 300mg/L, wherein, Oil-tea-cake adsorbent AIn waste water, content is 2g/L, and sodium chloride mass percent is at 2%, 20 DEG C, to stir or vibrationAfter 24h, isolated by filtration, filtrate is adjusted to neutral rear discharge, completes active red in waste water 15Absorption.
Initial pH on wastewater on the impact of active red 15 removal effects as shown in Figure 1. By Fig. 1Visible, pH is very large on the impact of active red 15 removal effects. Initial pH value is increased to from 1In 5 process, the adsorption capacity of active red 15 obviously reduces, and drops to from 64.04mg/g9.01mg/g; PH value was at 5～11 o'clock, and the adsorption capacity of active red 15 slightly reduces until notBecome. The low pH of evidence is conducive to the Adsorption of Oil-tea-cake adsorbent to active red 15,Initial pH on wastewater=1 o'clock Adsorption effect is best.
Embodiment 2
By clean the Oil-tea-cake of removing after impurity through distilled water, under 100 DEG C of conditions, dry 24h,Through pulverizing, being screened to particle diameter is 0.3～0.6mm, obtains Oil-tea-cake adsorbent B again.
Get Oil-tea-cake adsorbent B and add pH=1, containing 300mg/L active red 15, sodium chloride matterAmount percent concentration is respectively in 0%, 2%, 5%, 10%, 20%, 30% waste water, itsIn, Oil-tea-cake adsorbent B content in waste water is 3g/L, stirs at 35 DEG C or vibration 24hAfter, isolated by filtration, filtrate is adjusted to neutral rear discharge, completes the suction to active red in waste water 15Attached.
Sodium chloride concentration on the impact of active red 15 removal effects as shown in Figure 2, can find out,Along with the rising gradually of sodium chloride mass concentration, Oil-tea-cake adsorbent B Adsorption active red15 ability constantly declines. Therefore, in Adsorption waste water of the present invention, active red 15 dyesPreferred sodium chloride-containing not in the method for material.
Embodiment 3
By clean the Oil-tea-cake of removing after impurity through distilled water, under 80 DEG C of conditions, dry 24h, thenThrough pulverizing, being screened to particle diameter is 0.3～0.6mm, obtains Oil-tea-cake adsorbent C.
Get Oil-tea-cake adsorbent C add pH=1, respectively containing 100,150,200,250,300mg/LIn the waste water of active red 15, wherein, Oil-tea-cake adsorbent C content in waste water is 6g/L,At 50 DEG C, stir or vibrate after 24h, isolated by filtration, filtrate is adjusted to neutral rear discharge.
Active red 15 initial concentrations on the impact of active red 15 removal effects as shown in Figure 3, canTo find out, the active red 15 of significant proportion is removed in initial 30min, shows thisThe method of bright Adsorption active red 15 is efficiently rapid. Along with active red 15 initial concentrations by100mg/L is increased to 250mg/L, and adsorption capacity rises to 38.46mg/g by 15.13mg/g,Amount of increase is large. And active red 15 initial concentrations are while being increased to 300mg/L from 250mg/L, absorptionVolume change is little. This shows that the method for Adsorption active red 15 of the present invention is more suitable for processingLower than the waste water containing 250mg/L active red 15.
Embodiment 4
By clean the Oil-tea-cake of removing after impurity through distilled water, under 80 DEG C of conditions, dry 36h, thenThrough pulverizing, being screened to particle diameter is 0.3～0.6mm, obtains Oil-tea-cake adsorbent D.
Get Oil-tea-cake adsorbent D join respectively pH=1, active red 15 concentration be respectively 100,150,200,250, in the waste water of 300mg/L active red 15, wherein, Oil-tea-cake adsorbentD content in waste water is 6g/L, at 20 DEG C, 35 DEG C, 50 DEG C, stirs or vibrates after 24h,Isolated by filtration, filtrate is adjusted to neutral rear discharge.
Temperature on the impact of active red 15 removal effects as shown in Figure 4, along with temperature is from 20 DEG CRise to 50 DEG C, adsorption capacity increases gradually, but variation is very little, illustrates that temperature is to Oil-tea-cakeThe impact of adsorbent D Adsorption active red 15 is little, shows Adsorption activity of the present inventionThe method of red 15 dyestuffs larger temperature range to waste water in active red 15 dyestuffs have fineRemoval effect.
Langmuir and the matching of Temkin adsorption isotherm for absorption result, under different temperaturesAs shown in Figure 5,6, fitting result is as shown in table 1 for adsorption isotherm.
From Fig. 5,6 and table 1 can find out, from thermoisopleth parameter and fitting coefficient, phaseRatio is in Langmuir model, and Temkin model can be described Oil-tea-cake adsorbent D couple betterThe isothermal adsorption test data of active red 15.
20 DEG C time, the Oil-tea-cake adsorbent D adsorption activity that Langmuir thermoisopleth calculatesRed 15 maximum mono layer adsorption amount Q074.63mg/g. Different adsorbents dye activityThe Q of material0More as shown in table 2, with the Q of other efficient low-cost sorbents in table0Compare, thisIt is efficiently cheap that the Oil-tea-cake adsorbent of invention can be used as the one of processing containing active red 15 waste waterAdsorbent.
Table 1 adsorption isotherm parameter
The Q of the different adsorbents of table 2 to reactive dye0Relatively
| Adsorbent | Reactive dye | Maximum mono layer adsorption amount Q0(mg/g) |
| Pinus sylvestris var. mongolica pine nut | REACTIVE Red 195 | 6.69 |
| Eggshell powder | Active red 198 | 46.90 |
| Deactivation aerobic particle mud | Active red 15 | 62.89 |
| Oil-tea-cake (the present invention) | Active red 15 | 74.63 |
| Handle mushroom | Active red 120 | 117.80 |
Embodiment 5
By clean the Oil-tea-cake of removing after impurity through distilled water, under 60 DEG C of conditions, dry 36h, thenThrough pulverizing, being screened to particle diameter is 0.3～0.6mm, obtains Oil-tea-cake adsorbent E.
Oil-tea-cake adsorbent E prepared by the present embodiment characterizes.
Infrared spectrum analysis
The infrared spectrogram of Oil-tea-cake adsorbent E prepared by the present embodiment as shown in Figure 7. SpectrumAnalysis shows, 3430cm–1The absworption peak at place may be the stretching vibration due to O – H, simultaneouslyHave that N – H's is overlapping; 2926cm–1And 2855cm–1What the absworption peak at place represented is-CH2GroupAsymmetric vibration and alkane in the stretching vibration of C – H group; Be positioned at 1638cm–1PlaceAbsworption peak is that in protein, the stretching vibration of C=O causes; 1400cm–1The absworption peak at placeWei – CH3Symmetric curvature; 1248cm–1The stretching vibration of the C=O that the absworption peak at place is carboxylic acid;1029cm–1The absworption peak at place is the stretching vibration of C – OH; 617cm–1The absworption peak at place representsBe the stretching vibration of C – N. The above results shows, Oil-tea-cake adsorbent surface be rich in amido,Carboxyl, hydroxyl, carbonyl isoreactivity group.
Scanning electron microscope analysis
That Fig. 8 a, Fig. 8 b and Fig. 8 c all represent is the scanning mirror figure of Oil-tea-cake adsorbent E.As shown in Figure 8, inhomogeneous (Fig. 8 a), exists a large amount of Oil-tea-cake adsorbent E apparent height(Fig. 8 b) for irregular strip skeleton structure. Fig. 8 c is that Oil-tea-cake adsorbent E amplifies 80000Micro-structure diagram doubly, can find out, has a large amount of hole knots in Oil-tea-cake adsorbent EStructure. Skeleton structure in Oil-tea-cake adsorbent and a large amount of pore structure are that dye molecule enters intoOil-tea-cake adsorbent inside provides passage, is conducive to the Adsorption of active red 15 dyestuffs.
Above-described embodiment shows, Oil-tea-cake adsorbent is efficiently cheap, is easy to preparation, adsorption operationsCondition easily realizes, and can be widely used in the processing containing active red 15 waste water.
Claims (1)
1. utilize Oil-tea-cake to remove a method for Wastewater Dyes, it is characterized in that, comprising:
By clean the Oil-tea-cake of removing after impurity through distilled water, under 80 DEG C of conditions, dry 36h, then through pulverizing,Being screened to particle diameter is 0.3～0.6mm, obtains Oil-tea-cake adsorbent D;
Get described Oil-tea-cake adsorbent D join respectively pH=1, active red 15 concentration be respectively 100,150,200,250, in the waste water of 300mg/L active red 15, wherein, described Oil-tea-cake adsorbent DIn described waste water, content is 6g/L, at 35 DEG C, stir or vibrate after 24h, and isolated by filtration, filtrate is adjustedAfter neutral, discharge;
Langmuir adsorption isotherm matching for absorption result, described Oil-tea-cake adsorbent D is to described activityRed 15 maximum mono layer adsorption amount Q0For 101.01mg/g.
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Citations (3)
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| JP2009248006A (en) * | 2008-04-07 | 2009-10-29 | Zeo Sorb:Kk | Adsorption-coagulation type wastewater treatment agent |
| CN103657593A (en) * | 2013-12-09 | 2014-03-26 | 北京工业大学 | Sunflower husk biomass carbon adsorbent, preparation method and method for removing methylene blue from water |
| CN103922433A (en) * | 2014-03-13 | 2014-07-16 | 北京工业大学 | Method for removing reactive brilliant blue KN-R dye in waste water by using walnut shell biomass charcoal adsorbent |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009248006A (en) * | 2008-04-07 | 2009-10-29 | Zeo Sorb:Kk | Adsorption-coagulation type wastewater treatment agent |
| CN103657593A (en) * | 2013-12-09 | 2014-03-26 | 北京工业大学 | Sunflower husk biomass carbon adsorbent, preparation method and method for removing methylene blue from water |
| CN103922433A (en) * | 2014-03-13 | 2014-07-16 | 北京工业大学 | Method for removing reactive brilliant blue KN-R dye in waste water by using walnut shell biomass charcoal adsorbent |
Non-Patent Citations (1)
| Title |
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| Study on processing technology of oil-tea-cake on acid dye neutral red wastewater;Xinlong Jiang等;《Advanced Materials Research》;20140409;第915－916卷;第922－923页及图1 * |
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