CN106140100A - A kind of methylene blue method of wastewater treatment - Google Patents
A kind of methylene blue method of wastewater treatment Download PDFInfo
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- CN106140100A CN106140100A CN201510245328.4A CN201510245328A CN106140100A CN 106140100 A CN106140100 A CN 106140100A CN 201510245328 A CN201510245328 A CN 201510245328A CN 106140100 A CN106140100 A CN 106140100A
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- phosphoric acid
- methylene blue
- wood flour
- acid modification
- arachidis hypogaeae
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Abstract
The invention discloses a kind of methylene blue method of wastewater treatment, comprise the steps: that (1) prepares phosphoric acid modification Pericarppium arachidis hypogaeae；(2) phosphoric acid modification wood flour is prepared；(3) the phosphoric acid modification wood flour that phosphoric acid modification Pericarppium arachidis hypogaeae step (1) prepared and step (2) prepare mixes with the mass ratio of 1:1～4, prepares compound adsorbent；(4) with the amount of 0.1～0.7g/100mL, above-mentioned compound adsorbent is put in methylene blue waste water, at a temperature of 25～65 DEG C, 40～140r/min concussion absorption 20～120min, the pH value of above-mentioned methylene blue waste water is 2～12, and the content of its Methylene Blue is 5～10mg/L.The method of the present invention uses the waste water that phosphoric acid modification Pericarppium arachidis hypogaeae and phosphoric acid modification wood flour mixed processing are polluted by methylene blue, and high to the adsorption efficiency of methylene blue, operating process is simple, and adsorption conditions requires low, and adsorbing material is with low cost, reaches " with useless pollution treatment ".
Description
Technical field
The invention belongs to field of waste water treatment, be specifically related to a kind of methylene blue method of wastewater treatment.
Background technology
Methylene blue is a kind of water solublity polycyclic aromatic hydrocarbon dyestuff, mainly as chemistry stain for fiber crops, silk fabric, paper,
Manufacture ink, color lake and biology, the dyeing of bacterial organisms and the coloring of bamboo wood.In chemical experiment, analytical pure methylene blue
Adsorption indicator, oxidation-reduction indicator and the biological dyies being used as in chemical reagent more.At pharmaceuticals industry, methylene blue
Injection is used to treat methaemoglobinaemia, and poisoner slight for carbon monoxide also can pass through intravenous injection methylene
Indigo plant is detoxified.At present, methylene blue is widely used in dye industry and textile and dyeing industry, dye industry and textile printing and dyeing
The produced wastewater discharge of industry is very big, has the feature of " high concentration, high chroma, high pH, difficult degradation, change " more,
Dyeing waste water is administered and improper will directly affect a regional water quality, and then harm surrounding enviroment and human health.
Hemoglobin is played Oxidation by the methylene blue solution of high concentration, makes generation metahemoglobin.When intravenous injection or
Eat by mistake, suck and time percutaneous absorbtion methylene blue solution dosage is excessive, can cause nauseating, stomachache, precordial pain, dizziness,
The untoward reaction such as headache, perspiration and obnubilation.Methylene blue may have harm to environment, excessive concentration in water body, meeting
Affect the character such as the colourity of water, turbidity.
For reducing the adverse effect that methylene blue causes to water quality, physical method, chemical method or biological method can be used to carry out
Desolventing technology.Absorption method is simple, efficient, economical, is not easily introduced other chemical substances, therefore becomes a kind of most important,
Processing method widely.(what is tender, Kong Huoliang, high to include straw for biological material as the research of adsorbent in recent years
A man of virtue and ability levies. and surface modification straw biomass environmentally conscious materials is to absorption research [J] of PAHs in water. China Environmental Science, 2011,
31 (1): 50-55.), bagasse (tested by Liu Jingyong, Huang Guihong, Deng Junqiang etc. bagasse by the absorption property of methylene blue
Research [J]. Guangdong University of Technology's journal, 2013,30 (2): 124-128.), Arillus Longan (Jinbei Y, Meiqiong Y, Wentao C.
Adsorption of hexavalent chromium from aqueous solution by activated carbon prepared from
longan seed:Kinetics,equilibrium and thermodynamics[J],Journal of Industrial and
Engineering Chemistry, 2014,02 (054): 1-9.) etc..
Pericarppium arachidis hypogaeae is as the leftover bits and pieces of peanut processing and underuses, and major part is used as fuel or discards as waste residue, causes
The significant wastage of natural resources, directly affects the comprehensive utilization value of Semen arachidis hypogaeae.And Pericarppium arachidis hypogaeae contains catechol, Jiao's property no food
The polyhydric phenols such as son acid and phloroglucinol, easily exchange with heavy metal ion due to the hydrogen atom in phenolic hydroxyl group, and existing researcher utilizes
Pericarppium arachidis hypogaeae is as adsorbent, and (Zhang Qingfang, Yang Guodong, etc. Cr in modified peanut absorption water to remove metal ion in waste water6+
Research [J]. chemistry and biological engineering, 2008,25 (2): 29-31.), dyestuff (Yang Li, Zhao Hui. it is useless that peanut hull meal removes printing and dyeing
The research [J] of reactive dye in water. hubei agricultural science, 2013,52 (9): 2035-2037.).Prepare with zinc chloride for activator
The Activated Carbon Made from Peanut Shells gone out, the absorption to methylene blue dye is spontaneous process, meets Langmuir adsorption isotherm and two
Order reaction rate equation (Liu Yana, Tang Hongyan, Zhu Shufa, etc. the Activated Carbon Made from Peanut Shells characterization of adsorption to methylene blue. ring
Border engineering journal, 2013,7 (8): 3048-3052.).The modified Pericarppium arachidis hypogaeae of NaOH solution with 5% makees sorbent treatment
The research of methylene blue dye wastewater shows, under optimum process condition, the adsorption rate of methylene blue is reached by modified peanut
99.57%, for Pericarppium arachidis hypogaeae comprehensive utilization provide basis (Chen Yu, endanger abundant east .NaOH modified peanut to methylene blue contaminate
The research of material absorption property. application chemical industry, 2014,43 (10): 1863-1866.).
The wood flour that pile up like a mountain, occupies substantial amounts of soil, and tiny wood pellet thing adds the amount of dust in air.Empty
PM10 and PM2.5 in gas increases, and pellet is inhaled into human body, works the mischief human health.In order to enter
One step utilize resource, wood flour be widely used in adsorbent research (Yang Zhongzhi, Jiang Jianchun, Xu Junming, surplus etc. the liquefaction of. wood flour
Excess prepares the exploratory development [J] of activated carbon. charcoal element technology, and 2013,32 (2): 11-15.).Additionally, through modified wood flour pair
Heavy metal ion Cr (VI) in waste water has preferable adsorption effect.With optimal conditions, Nitric Acid Modified wood flour compares phosphorus
Acid modified wood chips advantages of good adsorption effect, Nitric Acid Modified wood flour reaches 85% to Cr (VI) adsorption rate, and phosphoric acid modification wood flour is
76% (Zhao Hui, Liao Xiang, Chen Jinwen, etc. modified wood chips adsorption treatment contains Cr (VI) waste water. chemical industry environmental protection,
2011,31(5):402-405.).Wood flour is grafted season amine groups and is prepared for modified wood chips, when pH is 3～10, change
Cr (VI) is all had significant adsorption, adsorption process to meet pseudo-second order kinetic equation (liuqin, Hao Lin by property wood flour
Woods, Zheng Tong, etc. the modified wood chips absorption property to Cr in water (VI). environmental project journal, 2015,
9(3):1021-1026.).Through epoxychloropropane cross-link, by with acrylamide graft, the modified wood chips prepared is to containing 10
The hybrid analog-digital simulation waste water clearance of mg/LCd (II) and Cr (III) all can reach more than 95% (Hu Yixu, Xia Lu, gold
General, etc. the absorption of cadmium chromium hybrid ionic is studied by modified wood chips. metal mine, 2012, (3): 145-148,162.).Thus change
Property wood flour for heavy metal ion there is certain adsorption effect, but the composite adsorption that modified peanut and modified wood chips are mixed
Agent is applied to the absorption of methylene blue in waste and does not appear in the newspapers.
Summary of the invention
It is an object of the invention to overcome prior art defect, it is provided that a kind of methylene blue method of wastewater treatment.
The technical scheme that the present invention is concrete is as follows:
A kind of methylene blue method of wastewater treatment, comprises the steps:
(1) Pericarppium arachidis hypogaeae is placed in phosphoric acid solution, after stirring 50～90min, carries out solid-liquid separation, by solid at 45～60 DEG C
Lower drying, is warming up to 170～200 DEG C of post-heating 60～70min, 480～520 DEG C of activation 45～60min in Muffle furnace,
Then clean with 70～80 DEG C of deionized waters and remove free phosphoric acid, cool down after then drying at 45～60 DEG C, obtain phosphoric acid modification
Pericarppium arachidis hypogaeae；
(2) wood flour is stood after phosphoric acid mixing and stirring, make wood flour be sufficiently impregnated with swelling, be positioned over 110～160 DEG C
Dry solidification 60～90min in baking oven, period every 15～20min stirring once, be subsequently placed in Muffle furnace in 480～520 DEG C
Lower activation 60～75min, activation is first pickling after terminating, then washing is until rinsing liquid is neutrality, is positioned in drying baker 45～60 DEG C
It is dried, cools down to obtain phosphoric acid modification wood flour；
(3) the phosphoric acid modification wood flour that phosphoric acid modification Pericarppium arachidis hypogaeae step (1) prepared and step (2) prepare is with 1:1～4
Mass ratio mixing, prepare compound adsorbent；
(4) above-mentioned compound adsorbent is put in methylene blue waste water, in 25～65 DEG C with the amount of 0.1～0.7g/100mL
At a temperature of, 40～140r/min concussion absorption 20～120min, the pH value of above-mentioned methylene blue waste water is 2～12, its Central Asia
The content of methyl blue is 5～10mg/L.
In a preferred embodiment of the invention, described step (1) is: is placed in phosphoric acid solution by Pericarppium arachidis hypogaeae, stirs
After mixing 60min, carry out solid-liquid separation, solid is dried at 50 DEG C, be warming up to 180 DEG C of post-heating 60min, then at horse
Not 500 DEG C of activation 60min in stove, then clean with 75 DEG C of deionized waters and remove free phosphoric acid, then dry at 50 DEG C
Rear cooling, obtains phosphoric acid modification Pericarppium arachidis hypogaeae.
In a preferred embodiment of the invention, described step (2) is: after wood flour and phosphoric acid mixing and stirring
Standing, make wood flour be sufficiently impregnated with swelling, be positioned over dry solidification 60min in 120～150 DEG C of baking ovens, period is every 15min
Stirring once, is subsequently placed in Muffle furnace at 500 DEG C and activates 60min, and activation is first pickling after terminating, then washing is until floating
Washing liquid is neutrality, is positioned in drying baker 50 DEG C and is dried, cools down to obtain phosphoric acid modification wood flour.
In a preferred embodiment of the invention, described step (3) is: phosphoric acid modification flower step (1) prepared
The phosphoric acid modification wood flour that raw shell and step (2) prepare mixes with the mass ratio of 1:3.5～4, prepares compound adsorbent.
In a preferred embodiment of the invention, described step (4) is: the amount with 0.3～0.7g/100mL is by above-mentioned
Compound adsorbent puts in methylene blue waste water, at a temperature of 35～65 DEG C, and 60～140r/min concussion absorption 40～100min,
The pH value of above-mentioned methylene blue waste water is 10～12, and the content of its Methylene Blue is 6～10mg/L.
It is further preferred that in described step (1), Pericarppium arachidis hypogaeae mass concentration in phosphoric acid solution is 5～6%, and phosphoric acid
The concentration of solution is 1～1.2mol/L.
It is further preferred that wood flour and phosphoric acid quality are than for 1:2～4 in described step (2).
The invention has the beneficial effects as follows:
The method of the method for the present invention uses phosphoric acid modification Pericarppium arachidis hypogaeae and phosphoric acid modification wood flour mixed processing to be polluted by methylene blue
Waste water, high to the adsorption efficiency of methylene blue, operating process is simple, and adsorption conditions requires low, and adsorbing material is with low cost,
Reach " with useless pollution treatment ".
Accompanying drawing explanation
Fig. 1 is the initial concentration result figure on the impact of methylene blue clearance of the embodiment of the present invention 2 Methylene Blue；
Fig. 2 is that in the embodiment of the present invention 3, compound adsorbent difference adds the mass ratio result on the impact of methylene blue clearance
Figure；
Fig. 3 is the solution ph result figure on the impact of methylene blue clearance in the embodiment of the present invention 4；
Fig. 4 is the temperature result figure on the impact of methylene blue clearance in the embodiment of the present invention 5；
Fig. 5 is the oscillation rate result figure on the impact of methylene blue clearance in the embodiment of the present invention 6；
Fig. 6 is the compound adsorbent consumption result figure on the impact of methylene blue clearance in the embodiment of the present invention 7.
Detailed description of the invention
Combine accompanying drawing below by way of detailed description of the invention technical scheme is further detailed and describes.
Embodiment 1
(1) weigh 5g Pericarppium arachidis hypogaeae to be placed in the beaker of 1L, add 100mL 1mol/L phosphoric acid solution, stir 60min
After, remove liquid portion with suction filter pump sucking filtration, dry at 50 DEG C, then heat to 180 DEG C of post-heating 60min, then at
500 DEG C of activation 60min in Muffle furnace, clean with 75 DEG C of deionized waters and remove free phosphoric acid, after then drying at 50 DEG C
Cooling, obtains phosphoric acid modification Pericarppium arachidis hypogaeae；
(2) weighing 5g wood flour to be placed in 1L beaker, phosphoric acid mixes by 2: 1 with wood flour, stands 5min after stirring
Making it be sufficiently impregnated with swelling, then be positioned over dry solidification 60min in 120～150 DEG C of baking ovens, period stirs every 15min
Once.Being subsequently placed in Muffle furnace at 500 DEG C activation 60min, activation is first pickling after terminating, and rear washing is until rinsing liquid
In neutrality, after be positioned in drying baker 50 DEG C and be dried cooling, obtain phosphoric acid modification wood flour；
(3) above-mentioned phosphoric acid modification Pericarppium arachidis hypogaeae and phosphoric acid modification wood flour are mixed in mass ratio, obtain compound adsorbent.
Embodiment 2
Taking 5,6,7,8,9,10mg/L methylene blue solution 100mL, in 250mL tool plug conical flask, accurately claim
Take 0.3g compound adsorbent to add in methylene blue solution, be placed in constant temperature oscillator, 100r/min at a temperature of 45 DEG C
Rate oscillation, takes supernatant after 60min, with the absorbance of ultraviolet visible spectrophotometry test residual methylene blue.
Being computed, the clearance of methylene blue is respectively 90.97%, and 98.03%, 95.89%, 94.94%, 94.93%, 95.68%.
As it is shown in figure 1, along with concentration rises to 6mg/L from 5mg/L, methylene blue clearance ascendant trend is big, originally
After beginning concentration 6～10mg/L, methylene blue clearance starts to decline gently.Under the conditions of illustrating to manage in this place, the suitableeest initial concentration
For 6mg/L, therefore initial concentration preferably 6～10mg/L.
Embodiment 3
Take the methylene blue solution that 100mL concentration is 10mg/L to be placed in 250mL tool plug conical flask, accurately weigh 0.3g
Compound adsorbent adds in methylene blue solution, now the mass ratio difference of modified peanut and modified wood chips in compound adsorbent
It is 1: 1,1: 1.5,1: 2,1: 2.5,1: 3,1: 3.5,1: 4.It is placed in constant temperature oscillator, 45 DEG C of temperature
The rate oscillation of lower 100r/min, takes supernatant after 60min, with ultraviolet visible spectrophotometry test residual methylene
Blue absorbance.Being computed, the clearance of methylene blue is respectively 90.14%, and 93.29%, 91.07%, 93.65%, 92.21%,
94.53%, 96.30%.
As in figure 2 it is shown, the mass ratio of modified peanut and modified wood chips when 1: 1～1: 3 because modified peanut and changing
The absorption property of property wood flour is not of uniform size causes methylene blue clearance to fluctuate back and forth between 90～94%, works as modified peanut
With mass ratio 1: 3.5～1: the 4 very fast ascendant trend of methylene blue clearance of modified wood chips, now modified peanut and modification
The adsorption efficiency of both wood flours is stepped up.Therefore ratio preferably 1: 3.5～1: 4 is added.
Embodiment 4
Take the methylene blue solution that 100mL concentration is 10mg/L to be placed in 250mL tool plug conical flask, regulate pH value of solution
Value is respectively 2,3,4,5,6,7,8,9,10,11,12, accurately weighs 0.3g compound adsorbent and adds methylene
In blue solution, it is placed in constant temperature oscillator, the rate oscillation of 100r/min at a temperature of 45 DEG C, after 60min, takes supernatant
Liquid, with the absorbance of ultraviolet visible spectrophotometry test residual methylene blue.Being computed, the clearance of methylene blue divides
It is not 94.90%, 95.89%, 95.45%, 96.08%, 94.34%, 95.31%, 94.39%, 94.98%, 96.37%,
97.03%, 97.40%.
As it is shown on figure 3, pH is relatively low at meta-acid and middle sexual stage methylene blue clearance, and it is that methylene blue goes at meta-alkalescence
Except rate is higher, therefore pH ranges preferably from 10～12.
Embodiment 5
Take the methylene blue solution that 100mL concentration is 10mg/L to be placed in 250mL tool plug conical flask, accurately weigh 0.3g
Compound adsorbent adds in methylene blue solution, is placed in constant temperature oscillator, respectively 25, and 35,45,55,65 DEG C of temperature
The rate oscillation of the lower 100r/min of degree, takes supernatant after 60min, with ultraviolet visible spectrophotometry test residual methylene
The absorbance that base is blue.Being computed, the clearance of methylene blue is respectively 95.00%, and 95.61%, 96.64%, 97.01%,
97.72%.
As shown in Figure 4, temperature is less to Adsorption Effect, is therefore applicable to 25～65 DEG C.
Embodiment 6
Take the methylene blue solution that 100mL concentration is 10mg/L to be placed in 250mL tool plug conical flask, accurately weigh 0.3g
Compound adsorbent adds in methylene blue solution, is placed in constant temperature oscillator, at a temperature of 45 DEG C, respectively with 40, and 60,
The rate oscillation of 80,100,120,140r/min, takes supernatant after 60min, surveys with ultraviolet visible spectrophotometry
The absorbance of examination residual methylene blue.Being computed, the methylene blue clearance of methylene blue is respectively 94.78%, and 95.25%,
96.04%, 96.61%, 97.03%, 97.31%.
As it is shown in figure 5, along with oscillation rate changes greatly from 40～60r/min methylene blue clearances, oscillation rate from
60～140r/min, methylene blue clearance rises slowly, and therefore oscillation rate ranges preferably from is 60～140r/min.
Embodiment 7
Take the methylene blue solution that 100mL concentration is 10mg/L to be placed in 250mL tool plug conical flask, weigh 0.1 respectively,
0.2,0.3,0.4,0.5,0.6,0.7g compound adsorbent adds in methylene blue solution, is placed in constant temperature oscillator,
The rate oscillation of 100r/min at a temperature of 45 DEG C, takes supernatant after 60min, residual with ultraviolet visible spectrophotometry test
Stay the absorbance of methylene blue.Being computed, the clearance of methylene blue is respectively 90.07%, and 92.01%, 96.61%, 97.75%,
98.06%, 98.31%, 98.53%.
As shown in Figure 6, along with the increase methylene blue clearance of dosage constantly rises, sub-after dosage reaches 0.3g
Methyl blue clearance starts to tend towards stability.Under the conditions of illustrating to manage in this place, the suitableeest dosage is 0.3g, therefore compound adsorbent
Dosage preferably 0.3～0.7g.
The above, only presently preferred embodiments of the present invention, therefore the scope that the present invention implements can not be limited according to this, i.e. depend on
The equivalence change that the scope of the claims of the present invention and description are made with modify, all should still belong in the range of the present invention contains.
Claims (7)
1. a methylene blue method of wastewater treatment, it is characterised in that: comprise the steps:
(1) Pericarppium arachidis hypogaeae is placed in phosphoric acid solution, after stirring 50～90min, carries out solid-liquid separation, by solid at 45～60 DEG C
Lower drying, is warming up to 170～200 DEG C of post-heating 60～70min, 480～520 DEG C of activation 45～60min in Muffle furnace,
Then clean with 70～80 DEG C of deionized waters and remove free phosphoric acid, cool down after then drying at 45～60 DEG C, obtain phosphoric acid modification
Pericarppium arachidis hypogaeae；
(2) wood flour is stood after phosphoric acid mixing and stirring, make wood flour be sufficiently impregnated with swelling, be positioned over 110～160 DEG C
Dry solidification 60～90min in baking oven, period every 15～20min stirring once, be subsequently placed in Muffle furnace in 480～520 DEG C
Lower activation 60～75min, activation is first pickling after terminating, then washing is until rinsing liquid is neutrality, is positioned in drying baker 45～60 DEG C
It is dried, cools down to obtain phosphoric acid modification wood flour；
(3) the phosphoric acid modification wood flour that phosphoric acid modification Pericarppium arachidis hypogaeae step (1) prepared and step (2) prepare is with 1:1～4
Mass ratio mixing, prepare compound adsorbent；
(4) above-mentioned compound adsorbent is put in methylene blue waste water, in 25～65 DEG C with the amount of 0.1～0.7g/100mL
At a temperature of, 40～140r/min concussion absorption 20～120min, the pH value of above-mentioned methylene blue waste water is 2～12, its Central Asia
The content of methyl blue is 5～10mg/L.
2. a kind of methylene blue method of wastewater treatment as claimed in claim 1, it is characterised in that: described step (1) is:
Pericarppium arachidis hypogaeae is placed in phosphoric acid solution, after stirring 60min, carries out solid-liquid separation, solid is dried at 50 DEG C, heat up
To 180 DEG C of post-heating 60min, 500 DEG C of activation 60min in Muffle furnace, then clean with 75 DEG C of deionized waters and remove
Free phosphoric acid, cools down after then drying at 50 DEG C, obtains phosphoric acid modification Pericarppium arachidis hypogaeae.
3. a kind of methylene blue method of wastewater treatment as claimed in claim 1, it is characterised in that: described step (2) is:
Wood flour is stood after phosphoric acid mixing and stirring, makes wood flour be sufficiently impregnated with swelling, be positioned in 120～150 DEG C of baking ovens dry
Dry solidification 60min, period stirs once every 15min, is subsequently placed in Muffle furnace at 500 DEG C activation 60min, alive
Change first pickling after terminating, then washing be until rinsing liquid is neutrality, be positioned in drying baker 50 DEG C and be dried, cool down phosphoric acid changes
Property wood flour.
4. a kind of methylene blue method of wastewater treatment as claimed in claim 1, it is characterised in that: described step (3) is:
The phosphoric acid modification wood flour that phosphoric acid modification Pericarppium arachidis hypogaeae step (1) prepared and step (2) prepare is with the mass ratio of 1:3.5～4
Mixing, prepares compound adsorbent.
5. a kind of methylene blue method of wastewater treatment as claimed in claim 1, it is characterised in that: described step (4) is:
Above-mentioned compound adsorbent is put in methylene blue waste water by the amount with 0.3～0.7g/100mL, at a temperature of 35～65 DEG C,
60～140r/min concussion absorption 40～100min, the pH value of above-mentioned methylene blue waste water is 10～12, its Methylene Blue
Content is 6～10mg/L.
6. a kind of methylene blue method of wastewater treatment as described in any claim in claim 1 to 5, its feature exists
In: in described step (1), Pericarppium arachidis hypogaeae mass concentration in phosphoric acid solution is 5～6%, and the concentration of phosphoric acid solution is
1～1.2mol/L.
7. a kind of methylene blue method of wastewater treatment as described in any claim in claim 1 to 5, its feature exists
In: in described step (2), wood flour and phosphoric acid quality are than for 1:2～4.
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| CN107029674A (en) * | 2017-04-18 | 2017-08-11 | 哈尔滨工业大学 | A kind of rare earth modified medical stone and peanut shell composite adsorbing material and preparation method thereof |
| CN108031446A (en) * | 2017-12-20 | 2018-05-15 | 江苏省农业科学院 | A kind of destainer and preparation method for protecting peanut polysaccharide |
| CN108031446B (en) * | 2017-12-20 | 2020-09-11 | 江苏省农业科学院 | Destaining solution for protecting peanut polysaccharide and preparation method thereof |
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