CN101224411A - Natural plant material of processing cationic dye in industrial wastewater and method thereof - Google Patents
Natural plant material of processing cationic dye in industrial wastewater and method thereof Download PDFInfo
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- CN101224411A CN101224411A CNA2007101340180A CN200710134018A CN101224411A CN 101224411 A CN101224411 A CN 101224411A CN A2007101340180 A CNA2007101340180 A CN A2007101340180A CN 200710134018 A CN200710134018 A CN 200710134018A CN 101224411 A CN101224411 A CN 101224411A
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Abstract
The invention pertains to the technical field of industrial effluents treatment, which more particularly relates to the adoption of a natural plant material, grapefruit shell, which is widely available but not utilized at present. After the grapefruit shell is ground, the optimality condition for treating effluents is obtained through test according to the characteristics of the cations in the grapefruit shell and industrial effluents to achieve the effect of better removing the cationic dyes in the effluents. The preferred process method is that: Under the condition of room temperature and stirring, the pH of the effluents is adjusted to 3 to 12 by acid or alkali, and 0.25 to 7 g of grapefruit shell particles with the particle size of 40 to 140mm is added to each liter of water, then the effluents are stirred at least for 15 minutes. The grapefruit shell particles are separated and the purpose of removing the cationic dyes in the effluents is achieved. Under the best treatment condition, the removing rate can reach above 95%. Compared with the activated carbon which is widely used at present, the invention has obvious cost advantages in the treatment of dyeing effluents. Compared with the existing adsorbent made from natural plant materials, the removal efficiency is much better.
Description
One, technical field
The invention belongs to the industrial sewage treatment technology field, be specifically related to adopt a kind of natural plant material shaddock skin that can extensively obtain that does not utilize as yet at present, according to cation characteristics in shaddock skin and the waste water, draw the optimum condition of handling waste water through test, to reach the method for dye of positive ion effect in the better removal waste water.
Two, background technology
At present, domestic treatment of dyeing wastewater is based on biochemical method, and is also like this substantially abroad.Some research work have been carried out in domestic in recent years outside, mainly are new biological treatment and the exploration of efficient special-purpose bacterium and new chemical medicament and the researchs such as development of efficient decolorizing coagulant.The removal of colourity is a great problem of treatment of dyeing wastewater.
Method of wastewater treatment generally has: physical method, chemical method, biological method.
The physics method: the physics method of using in the wastewater treatment mainly is an absorption method.Absorption is that a kind of material is attached to the process on the another kind of material surface.Porous material can be made adsorbent, as active carbon, polymeric adsorbent, wood chip and natural minerals etc.Absorption can be divided into physical absorption by its active force, chemisorbed and ion-exchange absorption Annex III kind.Most of adsorption phenomenas all are above-mentioned three kinds of adsorbing synthesis result in the water treatment.Absorption method has been widely used in the advanced treating of waste water and has removed colourity.Wherein active carbon is used for engineering of water treatment in a large number as a kind of good adsorbent.Absorption method is to utilize porous solid matter, makes one or more materials in the waste water be attracted to the surface of solids and the method removed.Industrial adsorbent commonly used has active carbon, active diatom soil, activated coal, natural illiteracy holder soil and cinder etc.Main and traditional adsorbent is an activated carbon both at home and abroad.Activated carbon has absorption property preferably to water-soluble dyes such as the dye of positive ion, direct dyes, acid dyes, reactive dye.
Chemical method: chemical method is to adopt oxidizing process or reducing process to destroy the chromophoric group of dyestuff, makes it to generate the little material of molecular weight, thereby loses the colour developing ability.The oxidant of oxidative decoloration method mainly contains ozone.Adopt the decolouring of ozone oxidation method, water-soluble dye wastewaters such as reactive dye, the dye of positive ion, acid dyes, direct dyes almost completely can be decoloured, even insoluble disperse dyes using ozone decolouring also can obtain good effect, but it is to insoluble dyes such as sulfide, reduzates, decolorizing effect is relatively poor, therefore the ozone oxidation decolouring is best suited for hydrophilic dye content height, the wastewater treatment that suspension is few.The major defect of ozone oxidation is bad to the clearance effect of waste water COD at present, and energy consumption is big simultaneously, and operating cost is higher relatively, the large-scale promotion difficulty.
Bioanalysis: biological degradation method is to utilize microbial growth to degrade, and dissolving is dispersed in the dyestuff in the water.Because the biodegradability of most of dyestuff is relatively poor, industries such as at present domestic many weavings, printing and dyeing begin to adopt the method for anaerobic-aerobic series connection to handle.For the waste water from dyestuff of low concentration, the anaerobism part generally only adopts Hydrolyze method.At anaerobism or hydrolysis stage, anaerobic bacteria carries out fragmentation to dyestuff, thereby improves the biodegradability of waste water, is beneficial to follow-up Aerobic Process for Treatment.U.S.'s dyer is done NAB National Association 0f Broadcasters a large amount of dye well medicaments is tested, and finds nearly half dyestuff BOD5/COD value less than 0.1, so uses biological treatment to handle this part pollutant and need select good bacterial classification.Must bioanalysis, BOD is removed fine, but to COD, the general effect of the removal of colourity is bad.So needing physics, chemical method simultaneously assists.
Although active carbon is to organic matter, the removal effect of colourity is all fine, and most dye molecule all there is very strong adsorption effect, but because the restriction of its adsorption capacity and the economical efficiency of regeneration techniques, active carbon can not be directly used in original treatment of dyeing wastewater, and relatively be fit to advanced treating.When developed country handles dye chemical industry waste water, use the tertiary treatment method always, promptly after the routine biological treatment, carry out the adsorption treatment of active carbon again.Though the organic matter colourity in the dye chemical industry waste water can be effectively removed in tertiary treatment, but disposal cost is very expensive, and the regeneration problem of active carbon all is difficult to solve with both economical effective method all the time, and this just becomes influences the key issue that active carbon more generally uses.So the expensive price of active carbon and the difficulty of regeneration have just restricted being extensive use of of active carbon greatly.If can be with feedstock production active carbon cheap and easy to get, the cost of active carbon is reduced, just can be directly used in active carbon the processing of waste water, solve handling the economical efficiency of waste water, be exactly the content of this paper research so seek a kind of material of alternative active carbon of suitable cheapness.Through repeatedly experiment repeatedly, we find this natural material of shaddock skin to can be used as the cheap material that substitutes active carbon.
Three, summary of the invention
1, goal of the invention
Dyestuff also produces a large amount of waste water from dyestuff and is discharged in the environment water when the life of giving people brings bright and colourful color and produces great economic benefit, causes the pollution of natural water.Painted water body not only influences the attractive in appearance of water environment but also reduces the water body light transmission capacity, influences the photosynthesis of water plant, and then causes the infringement of whole water ecosystem.Waste water from dyestuff has not only polluted environment, and some dyestuff or its catabolite are poisonous, even can modificator gene sudden change or carcinogenic.According to statistics, in the DYE PRODUCTION process, approximately lose 2% product, and in the dyestuff use, this loss is then up to 10% with waste water.China is first big country of textile printing and dyeing, and textile printing and dyeing industry is the rich and influential family of industrial wastewater discharge, thereby will realize the sustainable development of dyeing, must solve the pollution problem of dyeing.
The dye of positive ion is the bigger dye type of content common in the dyeing waste water.Ten thousand tons of about 1.4-1.6 of the annual requirement of the dye of positive ion on the China market since 2003.Though the present industrial active carbon that is used for removing the water coloring matter is the good cost height of effect.So the problem that the present invention need solve is to find a kind of low cost, the material of absorbing dye substitutes the processing that active carbon is used for industrial wastewater efficiently.
Shaddock (Citrus grandis L.Osbeck) is a Rutaceae oranges and tangerines subfamily citrus fruit.China's shaddock aboundresources is distributed widely in ground such as Guangdong, Guangxi, Fujian, sells and spreads all over all parts of the country.In recent ten years, the intensification shaddock class commodity base that a collection of scale is big, standard is high progressively forms.Calendar year 2001, the gross output of China shaddock class just reached 800,000 tons.The edible rate of shaddock is at 46%-56%, and remaining shaddock skin major part is not utilized and abandons, and causes the significant wastage of resource, and contaminated environment.We think, because the shaddock skin is rich in fiber, and the design feature of porous, it structurally has the potentiality as sorbing material.The experiment proved that the shaddock skin is good to the cation adsorption effect.Simultaneously because its cost is low, and need not to consider regeneration expense as active carbon, it has a clear superiority on economic benefit.On the other hand,, prove that the shaddock skin removes dyestuff and removing on the dye of positive ion methylene blue especially, compare than the removal effect of the cheap sorbing material of having reported at present and also have good advantages through consulting the contrast lot of documents.Test through us under the optimum condition of acquisition, the maximum of shaddock skin absorption methylene blue is: 456.6mg/g, promptly every gram shaddock skin particle absorption methylene blue 456.6mg.The cheap sorbing material of present research: rice hulls is 312mg/g to the maximal absorptive capacity of methylene blue, and cotton is 278mg/g, and perlite is 162.3mg/g, and marine alga is 104mg/g, and peanut shell is 68.03mg/g.Than these cheap materials, shaddock skin adsorption effect is much better than them.As seen as long as according to shaddock skin and waste water characteristic, find optimum condition, just the advantage of the adsorbent new material of the efficient cheapness of this conduct of the fine performance shaddock skin of energy.As seen the alternative active carbon of shaddock skin particle is promoted as novel absorption material.
2, technical scheme
The invention provides a kind of cheap and the material that adsorbs the dye of positive ion is efficiently arranged and use this material---with shaddock skin treatment of dyeing and printing, methylene blue and dimethyl diaminophenazine chloride in the absorption dye of positive ion.
With the adsorbent of shaddock skin, under room temperature (25-30 ℃), concussion stirring condition, with acid or alkali (1mol/L HNO as treatment of dyeing and printing
3With 1mol/L NaOH) the adjusting pH value of waste water is 3-12, and shaddock skin consumption is 0.25-7g in every liter of waste water, and adding the shaddock skin is graininess, 40-140 purpose shaddock skin.Stirred at least 0.25 minute, available centrifugal process is isolated the shaddock skin.
Preferred processing condition is under room temperature, stirring condition, with acid or alkali (1mol/L HNO
3And 1mol/LNaOH) after dyestuff pH value is 4-12 in the adjusting waste water, adds shaddock skin 0.25-3g in every liter of waste water.Stirred at least 1 hour, and isolated the shaddock skin.
The optimum process condition is under room temperature, stirring condition, with acid or alkali (1mol/L HNO
3With 1mol/L NaOH) regulate after dyestuff pH value is 6-12 in the waste water adding shaddock skin 1-2g in every liter of waste water.Stirred at least 3 hours, and isolated the shaddock skin.
3, the invention has the beneficial effects as follows:
(1) the inventive method is simple to operate.Active carbon is present most widely used dye sorbent, but the problem that higher relatively operating cost of active carbon and regeneration are produced has hindered the large-scale application of this technology.And use the shaddock skin to make adsorbent, and only need describedly according to the inventive method, adjust suitable pH value of solution value, the shaddock skin that adds suitable dosage get final product, and isolated shaddock skin need not to regenerate, and has saved the regeneration expense.
(2) this method uses financial cost low.Calendar year 2001, the gross output of China shaddock class just reached 800,000 tons.Because the edible rate of shaddock is at 46%-56%, remaining shaddock skin major part is not utilized and abandons, and causes the significant wastage of resource.This shows that the shaddock skin not only originates extensively, procurement cost is also very low.And present most widely used dye sorbent activated carbon, its Price Range is 4000～20000 yuan/ton, and the price height adds the regeneration expense, and cost is very high.
(3) advantages of good adsorption effect.According to our experimental result, the active carbon that discovery shaddock skin and absorption affinity are strong is compared, and the ability of the absorption dye of positive ion is very approaching.The methylene blue adsorption value of general commercial active carbon is 100-500mg/g, the active carbon maximal absorptive capacity 580mg/g that pitch is made, the ability of shaddock skin particle absorption methylene blue near or be better than these expensive active carbons.And the shaddock micromicro after the absorption does not need to regenerate with direct burning.Compare with cheap sorbing material rice hulls, cotton, peanut shell, pomace, banana pith and the palm fruit branch etc. of present research, the shaddock skin all is better than them to the adsorption effect of the dye of positive ion.
This shows, derive from the dye of positive ion sorbing material of shaddock skin,, very big application prospect is arranged owing to have advantages such as advantages of good adsorption effect, cost is low, economic benefit is obvious.
Four, description of drawings
Fig. 1 dye of positive ion MB, the calibration curve of NR
For obtain the linear equation of two kinds of standard dye curves through test, can stay the concentration of dyestuff in the solution by accompanying drawing 1, and then calculate amount of dye, obtain the dyestuff clearance by shaddock skin particle removal in order to calculating.
Fig. 2 pH removes the influence of dye of positive ion MB, NR to the shaddock skin
By accompanying drawing 2 as can be seen, pH does not have much affect to two kinds of dye of positive ion adsorption rates between 4-11, and adsorption rate is all very high.The MB adsorption rate is between 85%-90%, and the NR adsorption rate is between 90%-95%.MB is between pH 11-12, and adsorption rate increases, and obviously surpasses 96%.See that thus the shaddock skin is very high to the cation adsorption rate, and the pH value scope that is suitable for is bigger.
Fig. 3 quantity of sorbent is removed the influence of MB, NR to the shaddock skin
By accompanying drawing 3 as seen, adsorption rate is all more than 85% in the quantity of sorbent 0.25-7g/L scope, and quantity of sorbent is when 0.5-5g/L, and the adsorption rate of two kinds of dyes of positive ion is all more than 90%,
Fig. 4 particle diameter is removed the influence of dye of positive ion MB, NR to the shaddock skin
By accompanying drawing 4 as seen, this absorbent particles size is little to the influence of MB and NR adsorption rate in 40-140 purpose scope, and shaddock skin particle is in 40-140 order scope, and the adsorption rate of MB is between 96%-97%, and the adsorption rate of NR is between 95%-96%.
Fig. 5 time of stirring is removed MB, NR to the shaddock skin influence
Shown in accompanying drawing 5, increase with mixing time, clearance raises, and the clearance of two kinds of dyestuffs just reaches more than 94% when 0.25h, and MB reaches 97% after 1 hour, and NR reaches 95%.In the time of behind the stirring time 3h, two kinds of dyestuff clearances are basicly stable constant.
Five, the specific embodiment
1. the preparation of shaddock skin particle:
The shaddock skin is shredded, in 80 ℃ of thermostatic drying chambers, dry to constant weight, removed dust foreign matter etc. in 2 hours with distilled water immersion then, taking out then places 80 ℃ of thermostatic drying chambers to dry to constant weight again, get 40-60 order, 60-80 order, 80-100 order, 100-120 order and 120-140 order particle with the pulverizer grinding and sieving, place dry place standby.
2. dye of positive ion screening
Methylene blue is called for short MB, λ
Max=660nm; Dimethyl diaminophenazine chloride is called for short NR, λ
Max=520nm is all available from Shanghai San'aisi Reagent Co., Ltd..Be made into 200mg/l with distilled water and store liquid, the time spent dilutes according to needed concentration.
2.1 dye of positive ion calibration curve
Get 1,2,3,5,6,8, two kinds of dye solutions of 10mg/l, survey light absorption value under the maximum absorption wavelength separately at two kinds of dye solutions, drawing standard curve, result such as accompanying drawing 1.
Obtain the linear equation of two kinds of standard dye curves, can stay the concentration of dyestuff in the solution in order to calculating.Formula is as follows:
MB：C(mg/L)＝(A+0.0075)/0.1887
NR：C(mg/L)＝(A+0.0154)/0.071
2.2pH the shaddock skin is removed the analytic process of the influence of dye of positive ion MB, NR
2.2.1 test procedure
Join MB, NR concentration is 50mg/l, with 0.1M HNO3 or NaOH MB is adjusted to 3,4,5,6,7,8,9,10,11,12 respectively; NR is adjusted to 4,5,6,7 (pH＞7, the dimethyl diaminophenazine chloride color changes), and each triangular flask adds the 40ml dye solution, and adding the 0.2g diameter is 80-100 purpose shaddock skin particle, does three repetitions for every group.With sealing the film sealing, at room temperature put into desk-top constant temperature oscillator (THZ-C), with 150rpm speed concussion 24 hours, after the concussion absorption, take out sample, behind the centrifugal 15min of 10000rpm, get supernatant.
2.2.2 detection method
Record the light absorption value (MB:660nm that remains in two kinds of dyes of positive ion that are not adsorbed in the solution respectively with ultraviolet-visible spectrophotometer (VIS-7220); NR:520nm).Calculate dye strength in the solution, dyestuff adsorption rate according to calibration curve
Q＝(C
0-C
e)V/W
In the formula, C
0(mg/L) be the dye solution initial concentration, C
eDye strength in the solution when (mg/L) being adsorption equilibrium, V is the initial concentration of dye solution, W is the quality of adsorbent in the solution.
2.2.3 result of the test
(1) as shown in Figure 2, pH does not have much affect to two kinds of dye of positive ion adsorption rates between 4-11, and adsorption rate is all very high.The MB adsorption rate is between 85%-90%, and the NR adsorption rate is between 90%-95%.MB is between pH11-12, and adsorption rate increases, and obviously surpasses 96%.
(2) see that thus the shaddock skin is very high to dye of positive ion adsorption rate, and the pH value scope that is suitable for is bigger.Preferred pH value is 4-12.
2.3 quantity of sorbent is to the influence of dye of positive ion MB, NR
2.3.1 test procedure
Join MB, NR concentration is 50mg/l, with the HNO3 of 0.1M or NaOH the pH of MB solution is transferred to 11-12 respectively; NR is adjusted to 4-6 (pH＞7, the dimethyl diaminophenazine chloride color changes), and each triangular flask adds 100-120 purpose shaddock skin particle, and quantity of sorbent is respectively 0.25,0.5,1,2,3,5 and 7g/L.Do three repetitions for every group.Seal with sealing film, at room temperature put into oscillator,, after the concussion absorption, take out sample, after process 10000rpm is centrifugal, get supernatant with 150rpm speed concussion 24 hours.
2.3.2 detection method
Record the light absorption value (MB:660nm that remains in two kinds of dyes of positive ion that are not adsorbed in the solution respectively with ultraviolet-visible spectrophotometer (VIS-7220); NR:520nm).Calculate dye strength in the solution, dyestuff adsorption rate according to calibration curve
Q＝(C
0-C
e)V/W
In the formula, C
0(mg/L) be the dye solution initial concentration, C
eDye strength in the solution when (mg/L) being adsorption equilibrium, V is the initial concentration of dye solution, W is the quality of adsorbent in the solution.
2.3.3 result of the test
By accompanying drawing 3 as seen, adsorption rate is all more than 85% in the quantity of sorbent 0.25-7g/L scope, and quantity of sorbent is when 0.5-5g/L, and the adsorption rate of two kinds of dyes of positive ion is all more than 90%, but quantity of sorbent is during greater than 2g/L, and adsorption rate increases with quantity of sorbent and descends.Optimizing adsorption effect is at quantity of sorbent 0.25-2g/L.Optimum quantity of sorbent is 1-2g/L.
2.4 adsorption particle size influence
2.4.1 test procedure
Join MB, NR concentration is 50mg/l, uses the HNO of 0.1M respectively
3Or NaOH transfers to 11-12 with the pH of MB solution; NR is adjusted to 4-6 (pH＞7, the dimethyl diaminophenazine chloride color changes), adds 1-2g/L shaddock skin particle 40-60 order in each triangular flask, 60-80 order, 80-100 order, 100-140 order.Do three repetitions for every group.With sealing the film sealing, at room temperature put into oscillator, with 150rpm speed concussion 24 hours.After the concussion absorption, take out sample, after process 10000rpm is centrifugal, get supernatant.
2.4.2 detection method
Record the light absorption value (MB:660nm that remains in two kinds of dyes of positive ion that are not adsorbed in the solution respectively with ultraviolet-visible spectrophotometer (VIS-7220); NR:520nm).Calculate dye strength in the solution, dyestuff adsorption rate according to calibration curve
Q＝(C
0-C
e)V/W
In the formula, C
0(mg/L) be the dye solution initial concentration, C
eDye strength in the solution when (mg/L) being adsorption equilibrium, V is the initial concentration of dye solution, W is the quality of adsorbent in the solution.
2.4.3 result of the test such as accompanying drawing 4
As can be seen, shaddock skin particle is in 40-140 order scope, and the adsorption rate of MB is between 96%-97%, and the adsorption rate of NR is between 95%-96%.So this absorbent particles size is little to the influence of MB and NR adsorption rate in 40-140 purpose scope.Consider that absorbent particles is more little, adsorption particle is difficult to separated more, so preferred shaddock skin granular size is all can between the 40-80 order.
2.5 the stirring time influences clearance
Join MB, NR concentration is 50mg/l, uses the HNO of 0.1M respectively
3Or NaOH transfers to 11-12 with the pH of MB solution; NR is adjusted to 4-6 (pH＞7, the dimethyl diaminophenazine chloride color changes), and each triangular flask adds 40-60 order, 1-2g/L shaddock skin particle.With sealing film sealing, at room temperature put into oscillator, with the concussion of 150rpm speed, respectively 0.2,0.5,1,3,5,10 and during 24h sample thief centrifugal, separation of supernatant.
2.5.2 detection method
Record the light absorption value (MB:660nm that remains in two kinds of dyes of positive ion that are not adsorbed in the solution respectively with ultraviolet-visible spectrophotometer (VIS-7220); NR:520nm).Calculate dye strength in the solution, dyestuff adsorption rate according to calibration curve
Q＝(C
0-C
e)V/W
In the formula, C
0(mg/L) be the dye solution initial concentration, C
eDye strength in the solution when (mg/L) being adsorption equilibrium, V is the initial concentration of dye solution, W is the quality of adsorbent in the solution.
2.5.3 result of the test
As shown in Figure 5, increase with mixing time, clearance raises, and the clearance of two kinds of dyestuffs just reaches more than 94% when 0.25h, and MB reaches 97% after 1 hour, and NR reaches 95%.In the time of behind the stirring time 3h, two kinds of dyestuff clearances are basicly stable constant, and the MB clearance reaches 97.5%, and NR reaches 96%.So the most preferred stirring time is no less than 3 hours.
Claims (4)
1. new and effective cheap natural plants of handling the dye of positive ion in the industrial wastewater, it is characterized in that the shaddock skin is shredded, in 80 ℃ of thermostatic drying chambers, dry to constant weight, removed the dust foreign matter in 2 hours with distilled water immersion, place 80 ℃ of thermostatic drying chambers to dry again, get 40-140 order shaddock skin particle with the pulverizer grinding and sieving to constant weight.
2. according to the method for the dye of positive ion in the described shaddock skin of the claim 1 particle disposal waste water, it is characterized in that: under the condition of room temperature, stirring, with the HNO of certain low concentration
3Or H
2SO
4With NaOH dye of positive ion wastewater pH is adjusted to 3-12, adds 0.25-7g in every liter of waste water, particle diameter is a 40-140 purpose shaddock skin particle, stirs at least 0.25 hour, isolates shaddock skin particle.
3. the method for the dye of positive ion in the shaddock skin particle disposal waste water according to claim 2 is characterized in that: preferred processing condition is the HNO with certain low concentration
3Or H
28O
4With NaOH dye of positive ion wastewater pH is adjusted to 4-12, adds 0.25-3g in every liter of waste water, particle diameter is a 40-100 purpose shaddock skin particle.Stirred at least 1 hour, and isolated shaddock skin particle.
4. the method for the dye of positive ion in the shaddock skin particle disposal waste water according to claim 2 is characterized in that: optimum process is the HNO with certain low concentration
3Or H
28O
4With NaOH dye of positive ion wastewater pH is adjusted to 6-12, adds 1-2g in every liter of waste water, particle diameter is a 60-80 purpose shaddock skin particle.Stirred at least 3 hours, and isolated shaddock skin particle.
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