CN103272560A - Novel composite water treatment material and preparation method thereof - Google Patents
Novel composite water treatment material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a novel composite water treatment material and a preparation method thereof. The novel composite water treatment material contains tourmaline, sepiolite and graphene oxide or graphene. According to the preparation method, the graphene or the graphene oxide is wrapped on the surfaces of the sepiolite and the tourmaline by a reflux method, so the adsorptive property of the sepiolite on organic wastewater can be effectively improved by utilizing the large surface area of the graphene or the graphene oxide. The novel composite material has the characteristics of high adsorption efficiency, small using amount, energy conservation and the like, in particular, the sepiolite and the tourmaline are almost not consumed, so the treatment cost can be greatly reduced, and the dangerousness that dye molecules belonging to organic matters difficult to degrade are immersed into natural water and accumulated in the environment is avoided. Meanwhile, the graphene oxide and the graphene have good antibacterial property, so the phenomenon that activated sludge is increased too fast can be effectively improved, and considerable economic benefit, environmental benefit and social benefit are achieved.
Description
Technical field
The present invention relates to a kind of novel compound material for water treatment, is exactly a kind of prescription, preparation method and application that contains the compound material for water treatment of tourmaline, sepiolite and graphene oxide or Graphene specifically.
Background technology
Along with world population is increased sharply and rapid economic development; city size constantly enlarges; the demand of water resource and the discharge capacity of industrial wastewater rapidly, make the world especially water resources in china be faced with huge crisis, using water wisely, to reduce sewage discharge row extremely urgent.Yet, present industrial wastewater discharge severe overweight, especially dyeing waste water.The dyeing waste water of textile printing and dyeing industry discharging is one of major polluting sources in China's industrial system, and according to State Environmental Protection Administration's statistics, the dyeing waste water total amount of dyeing discharging is positioned at five of total flow controls of each industrial department discharging of the whole nation.2004,13.6 hundred million cubes of whole industry displacement, its gross contamination emission (in COD) then is positioned at six of each Ministry of Industry's family status.Dyeing waste water belongs to the organic wastewater that contains a certain amount of recalcitrant substance.Its pollutant levels height (COD), colourity is dark, is one of unmanageable industrial wastewater.
At present, the printing-dyeing waste water treatment process complexity needs the associating several method usually.Method commonly used at present has two classes: a kind of is physico-chemical process: namely add adsorbent removal pollutants in sewage in sewage.But these class methods because dosing expense height, remove pollutant not thoroughly, sludge quantity is big and be difficult to further processing, can produce certain secondary pollution, generally do not use separately, only as the auxiliary process of biochemical treatment; Another kind is biochemical process: utilize action of microorganisms, make organic matter degradation in the sewage, be adsorbed and a kind of processing method of removing.Yet contain a large amount of bio-refractory dyestuffs in the dyeing waste water, groups such as a large amount of phenyl ring, amido, azo are arranged in these dyestuffs, so biochemical method is not satisfactory to the treatment effect of printing and dyeing water.Therefore, cheap, material for water treatment is favourably welcome efficiently.
Sorbing material is to utilize the porous of solid matter to make one or more materials in the waste water be attracted to the surface of solids or inner and method that remove.The research and development of novel absorption material are significant to energy-saving and emission-reduction and protection environment.
Patent CN1431042A(2003) a kind of fly ash absorbent and wastewater treatment method are provided.The raw material of this adsorbent is flyash, a kind of industrial residue.Flyash has cellular structure, and chemical composition is complicated, is improved through peracid modification and heat modification specific area, dyeing waste water had treatment effect preferably, cheap economic environmental protection, but adsorption capacity is not very big comparatively speaking, and not reproducible utilization.
Patent CN101143312A (2008) provides a kind of manufacturing and renovation process of graininess mud adsorbent.This adsorbent is main raw material(s) with waste residue red mud and flyash, adds adhesive, exciting agent and pore former and makes through roasting.To good sewage processing effect, and renewable, can recycled for multiple times.But manufacturing process is loaded down with trivial details, and needs the high temperature roast, and cost is higher.
Patent CN102531226A(2012) provide a kind of method of handling acid dyes printing and dyeing water, simply summarized its step and be exactly: first adjust pH, aeration decolouring then is at last with the COD in the sepiolite reduction water of solid-carried catalyst.This method has that technology is simple, floor space is little, to the colourity of sour fuel dyeing waste water and COD obvious processing effect etc. characteristics.But the preparation method of sepiolite solid-carried catalyst is loaded down with trivial details, and needs the high-temperature activation of long period, and preparation cost is higher.
Patent CN2611008Y provides a kind of sepiolite membrane filter, sepiolite filter membrane in this equipment is to pull an oar after adding water with sepiolite fibre, wood-fibred, glass fibre, resin glue in container, the filter skeleton all is inserted in the filter pulp, copies with paper technology and be plated on the gauze.This filter membrane can be widely used in drinking water, grape wine, beverage, liquor and edible wet goods industry.But this filter membrane is for the treatment of industrial wastewater the time, and flow velocity is slower, and efficient is lower.
Graphene is made up of the monolayer carbon atom, has cellular two dimensional crystal structure, is present known thin material in the world.Graphene has higher specific surface area (2600m
2/ g), possess electron mobility (15000cm at a high speed under outstanding heat conductivility (3500W/mK) and ultimate strength (1100GPa), the room temperature
2V
-1K
-1), also have antibacterial action simultaneously, obtain broad research and application in fields such as nanometer instrument, composite, hydrogen storage materials.
Graphene oxide a kind of interlamellar spacing that to be flake graphite obtain through degree of depth liquid phase oxidation is much larger than the lamellar compound of former graphite, can form monolithic layer structure (being graphene oxide) after peeling off, be the important growth of Graphene, graphene oxide has characteristics such as the big and ion-exchange capacity of specific area is strong.Graphite through peroxidating has been introduced many oxy radicals in its sheet surfaces, as hydrophilic active groups such as hydroxyl, carboxyl, epoxy radicals, thereby make it be easy in polar solvent to form stable single sheet, make graphene oxide can with most metals and the compound composite that obtains excellent performance of metal oxide.
Minimum and the easiest graphene preparation method of accomplishing scale production of cost is the graphene oxide reducing process at present.And preparation graphene oxide method in common is the HUMMERS method, the graphene oxide reducing process is with crystalline flake graphite and strong acid and strong oxidation material reaction generation graphene oxide, be prepared into graphene oxide (mono-layer graphite oxide alkene) through ultrasonic dispersion, add reducing agent and remove the oxy radical on graphite oxide surface, as carboxyl, epoxy radicals and hydroxyl, obtain Graphene.The graphene oxide reducing process is made lower and efficient, the environmental protection of Graphene cost, and can large-scale industrial production.
Summary of the invention
The invention provides a kind of efficient compound material for water treatment, contain tourmaline, sepiolite and graphene oxide or Graphene in this material, wherein tourmaline has self power generation polarity, the effective organic matter in the degrading waste water, tourmaline can also be releasing far infrared simultaneously, can effectively improve this material to the rate of adsorption of organic matter and ion; Sepiolite has relatively large specific area, can adsorb organic matter and yin, yang ion in the waste water fast; The graphite oxide specific area is big, and contain-OH ,-oxygen-containing functional groups such as COOH, possess hydrophilic property can effectively be removed the pollutant in the water, and Graphene does not then contain functional group, and is water insoluble, but organic compounds such as the hydro carbons in the easy adsorbed water, aromatic hydrocarbons.The present invention makes a kind of efficient compound material for water treatment with this raw material, and the preparation method is simple, and is with low cost, and good to sewage treatment effect, consumption is little, environmental protection.
Technical scheme of the present invention is:
A kind of NEW TYPE OF COMPOSITE material for water treatment, its composition and proportioning comprise:
The preparation method of described NEW TYPE OF COMPOSITE material for water treatment is one of following two kinds of methods, may further comprise the steps:
Method one: take by weighing graphene oxide, add water the mixed solution with ethanol, ultrasonic dispersion obtains graphene oxide suspension, its proportioning is that the mixed solution of per 20~80ml adds 1.5~15g graphene oxide, the graphene oxide suspension that obtains is added in the reactor, add sepiolite fibre and tourmaline powder through the peracid modification again, its proportioning is that per 1.5~15g graphene oxide adds 10~49.95g through sepiolite fibre and 0.05~40g tourmaline powder of peracid modification, add the mixed solution of water and ethanol again, wherein, the every 50g of quality sum of sepiolite and tourmaline need add the mixed solution of 400-600ml water and ethanol; With reactor heating reflux reaction 3 hours, obtain the surface and coat the sepiolite of graphene oxide and the mixed liquor of tourmaline, with mixed liquor suction filtration, drying, grinding, obtain NEW TYPE OF COMPOSITE material for water treatment (being called for short T/GO/S);
Perhaps, method two: take by weighing graphene oxide, add water the mixed solution with ethanol, ultrasonic dispersion obtains graphene oxide suspension, its proportioning is that the mixed solution of per 20~80ml adds 1.5~15g graphene oxide, pour the suspension that obtains into reactor, add sepiolite fibre and tourmaline powder through the peracid modification again, its proportioning is that per 1.5~15g graphene oxide adds 10~49.95g through sepiolite fibre and 0.05~40g tourmaline powder of peracid modification, add the mixed solution of water and ethanol again, wherein, the every 50g of quality sum of sepiolite and tourmaline need add the mixed solution of 400-600ml water and ethanol; With reactor heating reflux reaction 3 hours, in reactor, add the ratio adding hydrazine hydrate of 1~2g hydrazine hydrate then according to per 1~4g graphene oxide, reacted 30 minutes, the graphene oxide of reduced powder surface, then reactant is taken out, suction filtration, drying, grinding obtain NEW TYPE OF COMPOSITE material for water treatment (being called for short T/G/S)
The preparation method of described NEW TYPE OF COMPOSITE material for water treatment also comprises the forming step of composite: get the NEW TYPE OF COMPOSITE material for water treatment that makes previously, add water glass glue again, stir, add then in the mould, take out the back of waiting to finalize the design, and dries under ° C condition of 80 ° of C~300; Its proportioning is that every 20g NEW TYPE OF COMPOSITE material for water treatment adds 1~2ml water glass binder.
Water in described method one or the method two and the mixed solution of ethanol, composition is volume ratio water: ethanol=1:3~3:1.
Compared with prior art, advantage of the present invention is:
The selected tourmaline of the present invention has releasing far infrared function, can activate the especially organic molecule in the dyeing waste water of organic wastewater, accelerates the movement velocity of molecule, thereby improves the rate of adsorption; Tourmaline also has absorption property, can effectively adsorb organic matter and various ion in the waste water; The tourmaline spontaneous polarity of tool also simultaneously, the organic matter in can degrading waste water; Tourmaline is also had a surface-active, hydrone can be resolved into hydroxyl ion and improve dissolved oxygen in the water.
The selected sepiolite of the present invention is a kind of fibrous moisture rich magnesium silicate mineral, and theoretical specific area can reach 900m
2/ g, wherein inner ratio surface area 500m
2/ g, external surface area 400m
2/ g, so big specific area and loose structure are the immediate causes that sepiolite has strong adsorption capacity.But the adsorptivity of natural sepiolite and ion exchangeable are very weak, need carry out modification so its specific area reaches theoretical value far away.After the acid modification, the duct area in the sepiolite fibre and volume increase, and the duct number increases, and specific area significantly increases, the adsorption capacity of organic matter and various ions is obviously strengthened, and cheap.
Graphene or graphene oxide material that the present invention uses have the big characteristics of specific area, can improve 5~10 times with the sepiolite compound afterwards rate of adsorption and the adsorption capacity of sepiolite; After compound with tourmaline, the rate of adsorption and the adsorption capacity that can improve tourmaline can improve 3~10 times.Graphene oxide and Graphene also have antibacterial action, use graphene oxide or Graphene to handle the growth and breeding that waste water can suppress bacterium in the waste water.
The present invention can directly be used as filtrate, for the treatment of sanitary sewage, industrial wastewater, environment accident etc., has solved especially that cost height in the processing procedure of dyeing waste water, decolouring are difficult, COD removes problems such as difficulty, can simplify the treatment process of dyeing waste water.Have cheap, can reuse, the characteristics of efficient, energy-conservation, environmental protection.
The present invention adopts circumfluence method that Graphene or graphene oxide are wrapped in sepiolite and tourmaline powder surface, prepare a kind of advanced composite material (ACM), this material physical properties is stable, function admirable, cheap, and compare with traditional sorbing material and to have absolute predominance.
The present invention has chosen 4 groups of compound material for water treatment and sepiolite and active carbon behind sour modified active compare test, find that four groups of compound material for water treatment generally are improved to the treatment effeciency of organic wastewater, be respectively 86.6%, 80.3%, 95.3%, 90.4%, and sepiolite and active carbon only are 30.4% and 2.3% to the treatment effeciency of simulating dyeing waste water.Compare with other sorbing materials, efficient height of the present invention, energy-conservation, floor space is little, especially the sepiolite among the present invention and tourmaline are consumed hardly, therefore can reduce processing cost greatly, the danger of having avoided belonging to the dye molecule immersion natural water body of hardly degraded organic substance and having accumulated in environment has considerable economic, environmental benefit and social benefit.
The specific embodiment
Improved hummers method is adopted in the preparation of graphene oxide described in the present invention, the preparation method can be with reference to Wei Gao, people's document Engineered Graphite Oxide Materials for Application in Water Purification such as Mainak Majumder, ACS Appl.Mater.Interfaces2011,3,1821 – 1826.
The preparation method through the sepiolite fibre of peracid modification who the present invention relates to is: at first take by weighing the beaker that sepiolite raw ore that 500g crossed 20 mesh sieves places 5000ml, add the 3112ml deionized water, the 388ml mass fraction is 36% hydrochloric acid solution, with the rotating speed high speed dispersion 1h of 1500r/min; With above-mentioned slurries repeated multiple times filtering and washing, be neutral until pH then; At last above-mentioned filter cake is dried under 80 ℃ of conditions, grinding is weighed, and obtains the sepiolite fibre through the peracid modification at last.
Embodiment one
1. take by weighing the 15.00g graphene oxide, add the water of 80mL1:1 and the mixed solution of ethanol, about ultrasonic 20min, obtain finely dispersed graphene oxide suspension, add in the round-bottomed flask, take by weighing sepiolite fibre (particle diameter 100~200 μ m) and 0.05g tourmaline powder (particle diameter 0.3~30 μ m) after the 49.95g acid modification respectively, put into round-bottomed flask, interpolation 520mL volume ratio is water and the alcohol mixed solution of 1:1 in the flask again;
2. flask was put into electrical heating cover heating while condensing reflux 3 hours, make graphene oxide be wrapped on sepiolite fibre and the tourmaline powder, suction filtration, drying, grinding namely obtain the compound material for water treatment of tourmaline/graphene oxide/sepiolite (being called for short T/GO/S).
3. add 20 glass glues that drip in the compound material for water treatment of the 20g that makes (T/GO/S), stir, add in the mould, take out after the moulding, under 100 ° of C conditions, dry, obtain the T/GO/S of moulding.
Embodiment two
1. take by weighing the 1.50g graphene oxide, add the water of 20mL1:1 and the mixed solution of ethanol, about ultrasonic 20min, obtain finely dispersed graphene oxide suspension, add in the round-bottomed flask, take by weighing sepiolite fibre and 0.05g tourmaline powder after the 49.95g acid modification respectively, put into round-bottomed flask, adding the 320mL volume ratio in the flask again is water and the alcohol mixed solution of 1:1;
Step 2~3 are with embodiment one.
Embodiment three
1. take by weighing the 15.00g graphene oxide, add the water of 80mL1:1 and the mixed solution of ethanol, about ultrasonic 20min, obtain finely dispersed graphene oxide suspension, add in the round-bottomed flask, take by weighing sepiolite fibre and 40.00g tourmaline powder after the 10.00g acid modification respectively, put into round-bottomed flask, adding the 520mL volume ratio in the flask again is water and the alcohol mixed solution of 1:1;
Step 2~3 are with embodiment one.
Embodiment four
1. take by weighing the 1.50g graphene oxide, add the water of 20mL1:1 and the mixed solution of ethanol, about ultrasonic 20min, obtain finely dispersed graphene oxide suspension, add in the round-bottomed flask, take by weighing sepiolite fibre and 40.00g tourmaline powder after the 10.00g acid modification respectively, put into round-bottomed flask, adding the 320mL volume ratio in the flask again is water and the alcohol mixed solution of 1:1;
Step 2~3 are with embodiment one.
Embodiment five
1. take by weighing the 15.00g graphene oxide, add the water of 80mL1:1 and the mixed solution of ethanol, about ultrasonic 20min, obtain finely dispersed graphene oxide suspension, add in the round-bottomed flask, take by weighing sepiolite fibre and 0.05g tourmaline powder after the 49.95g acid modification respectively, put into round-bottomed flask, adding the 520mL volume ratio in the flask again is water and the alcohol mixed solution of 1:1;
2. flask was put into electrical heating cover heating while condensing reflux 3 hours, make graphene oxide be wrapped on sepiolite fibre and the tourmaline powder, in flask, add 30g hydrazine hydrate reaction 30 minutes afterwards, the graphene oxide of reduced powder surface, then reactant is taken out, suction filtration, drying, grinding namely obtain the compound material for water treatment of tourmaline/Graphene/sepiolite (being called for short T/G/S).
3. add 20 glass glues that drip in the 20gT/G/S that makes, stir, add in the mould, take out after the moulding, under 100 ° of C conditions, dry, obtain the T/G/S of moulding.
Embodiment six
1. take by weighing the 1.50g graphene oxide, add the water of 20mL1:1 and the mixed solution of ethanol, about ultrasonic 20min, obtain finely dispersed graphene oxide suspension, add in the round-bottomed flask, take by weighing sepiolite fibre and 0.05g tourmaline powder after the 49.95g acid modification respectively, put into round-bottomed flask, adding the 320mL volume ratio in the flask again is water and the alcohol mixed solution of 1:1;
2. flask was put into electrical heating cover heating while condensing reflux 3 hours, make graphene oxide be wrapped on sepiolite fibre and the tourmaline powder, in flask, add 0.375g hydrazine hydrate reaction 30 minutes afterwards, the graphene oxide of reduced powder surface, then reactant is taken out, suction filtration, drying, grinding namely obtain the compound material for water treatment of tourmaline/Graphene/sepiolite (being called for short T/G/S).
Step 3 is with embodiment five.
Embodiment seven
1. take by weighing the 15.00g graphene oxide, add the water of 80mL1:1 and the mixed solution of ethanol, about ultrasonic 20min, obtain finely dispersed graphene oxide suspension, add in the round-bottomed flask, take by weighing sepiolite fibre and 40.00g tourmaline powder after the 10.00g acid modification respectively, put into round-bottomed flask, adding the 520mL volume ratio in the flask again is water and the alcohol mixed solution of 1:1;
Step 2~3 are with embodiment five.
Embodiment eight
1. take by weighing the 1.50g graphene oxide, add the water of 20mL1:1 and the mixed solution of ethanol, about ultrasonic 20min, obtain finely dispersed graphene oxide suspension, add in the round-bottomed flask, take by weighing sepiolite fibre and 40.00g tourmaline powder after the 10.00g acid modification respectively, put into round-bottomed flask, adding the 320mL volume ratio in the flask again is water and the alcohol mixed solution of 1:1;
Step 2~3 are with embodiment six.
Contrast test
Choose 4 groups of compound material for water treatment and common heat radiation coating and compare test, prepare the compound material for water treatment of tourmaline/graphene oxide/sepiolite according to the step of embodiment one, be labeled as " 1# "; Step according to embodiment five prepares the compound material for water treatment of tourmaline/Graphene/sepiolite, is labeled as " 2# "; Step according to embodiment four prepares the compound material for water treatment of tourmaline/graphene oxide/sepiolite, is labeled as " 3# "; Step according to embodiment eight prepares the compound material for water treatment of tourmaline/Graphene/sepiolite, is labeled as " 4# "; Step according to the sour modification of sepiolite prepares sepiolite fibre, is labeled as " S "; Active carbon is labeled as " AC ".Utilize visible spectrophotometer to test and assess above-mentioned material respectively to simulating the treatment effect of dyeing waste water.Experimental procedure is as follows:
1. get the simulation dyeing waste water (methylene blue solution) of six parts of 100mL4mg/L
2. take by weighing #1, #2, #3, #4, S and the AC of equivalent respectively, join simultaneously in the simulation dyeing waste water, survey its light absorption value every 20min with visible spectrophotometer, and calculate its clearance, as table 1.
Table 1, four kinds of composites and sepiolite, active carbon are to the treatment effeciency of simulation dyeing waste water
Sepiolite after the sour modification is higher than active carbon far away to the adsorption efficiency of simulation dyeing waste water as can be seen from Table 1, almost is 10 times of active carbon; And the adsorption efficiency of four kinds of composites has and is higher than sepiolite far away, almost is 3 times of sepiolite, is 30 times of active carbon.
This shows, the present invention adopts circumfluence method that Graphene or graphene oxide are wrapped in sepiolite and tourmaline surface, utilize the bigger surface area of Graphene or graphene oxide, can effectively improve sepiolite to the absorption property of organic wastewater, the rate of adsorption of four kinds of compound water treatment efficiencies obviously improves, treatment effeciency to the simulation dyeing waste water when 20min has reached 98.8%, 85.4%, 96.5%, 84.2%, and sepiolite and active carbon only are 30.4% and 2.3% to the treatment effeciency of simulating dyeing waste water.Compare with other sorbing materials, advanced composite material (ACM) provided by the invention has the adsorption efficiency height, consumption is few, characteristics such as energy-conservation, especially sepiolite and tourmaline are consumed hardly, therefore can reduce processing cost greatly, the danger of having avoided belonging to the dye molecule immersion natural water body of hardly degraded organic substance and in environment, having accumulated, simultaneous oxidation Graphene and Graphene have good antibacterial performance, if the activated sludge process of this composite in wastewater treatment process is combined, can effectively improve activated sludge and increase too fast problem, have considerable economic, environmental benefit and social benefit.
Claims (4)
2. the preparation method of NEW TYPE OF COMPOSITE material for water treatment as claimed in claim 1 is characterized by one of following two kinds of methods, may further comprise the steps:
Method one: take by weighing graphene oxide, add water the mixed solution with ethanol, ultrasonic dispersion obtains graphene oxide suspension, its proportioning is that the mixed solution of per 20~80ml adds 1.5~15g graphene oxide, the graphene oxide suspension that obtains is added in the reactor, add sepiolite fibre and tourmaline powder through the peracid modification again, its proportioning is that per 1.5~15g graphene oxide adds 10~49.95g through sepiolite fibre and 0.05~40g tourmaline powder of peracid modification, add the mixed solution of water and ethanol again, wherein, the every 50g of quality sum of sepiolite and tourmaline need add the mixed solution of 400-600ml water and ethanol; With reactor heating reflux reaction 3 hours, obtain the surface and coat the sepiolite of graphene oxide and the mixed liquor of tourmaline, with mixed liquor suction filtration, drying, grinding, obtain the NEW TYPE OF COMPOSITE material for water treatment;
Perhaps, method two: take by weighing graphene oxide, add water the mixed solution with ethanol, ultrasonic dispersion obtains graphene oxide suspension, its proportioning is that the mixed solution of per 20~80ml adds 1.5~15g graphene oxide, pour the suspension that obtains into reactor, add sepiolite fibre and tourmaline powder through the peracid modification again, its proportioning is that per 1.5~15g graphene oxide adds 10~49.95g through sepiolite fibre and 0.05~40g tourmaline powder of peracid modification, add the mixed solution of water and ethanol again, wherein, the every 50g of quality sum of sepiolite and tourmaline need add the mixed solution of 400-600ml water and ethanol; With reactor heating reflux reaction 3 hours, in reactor, add the ratio adding hydrazine hydrate of 1~2g hydrazine hydrate then according to per 1~4g graphene oxide, reacted 30 minutes, the graphene oxide of reduced powder surface, then reactant is taken out, suction filtration, drying, grinding obtain the NEW TYPE OF COMPOSITE material for water treatment.
3. the preparation method of NEW TYPE OF COMPOSITE material for water treatment as claimed in claim 2, it is characterized by the forming step that also comprises composite: get the NEW TYPE OF COMPOSITE material for water treatment that makes previously, add water glass glue again, stir, add in the mould then, take out after waiting to finalize the design, under ° C condition of 80 ° of C~300, dry; Its proportioning is that every 20g NEW TYPE OF COMPOSITE material for water treatment adds 1~2ml water glass binder.
4. the preparation method of NEW TYPE OF COMPOSITE material for water treatment as claimed in claim 2 is characterized by water in described method one or the method two and the mixed solution of ethanol, forms to be volume ratio water: ethanol=1:3~3:1.
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