CN109453753A - A kind of floating vapor and its preparation method and application - Google Patents
A kind of floating vapor and its preparation method and application Download PDFInfo
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- CN109453753A CN109453753A CN201811458941.4A CN201811458941A CN109453753A CN 109453753 A CN109453753 A CN 109453753A CN 201811458941 A CN201811458941 A CN 201811458941A CN 109453753 A CN109453753 A CN 109453753A
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- coupling agent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28011—Other properties, e.g. density, crush strength
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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Abstract
The invention discloses a kind of floating vapors and its preparation method and application, the floating vapor includes hollow glass micropearl and silane coupling agent, the silane coupling agent is grafted on the hollow glass micropearl outer surface, wherein, the silane coupling agent is the silane coupling agent for having specificity to dyestuff, and the mass ratio of hollow glass micropearl and silane coupling agent is 1~2:1.The preparation method includes: first to pre-process hollow glass micropearl, then pretreated hollow glass micropearl is reacted with silane coupling agent, finally by being dried to obtain floating vapor, dissolubility pollutant can be effectively treated in the present invention, and the floating vapor that pollutant is enriched after handling can stablize floating, to realize the quick separating of pollutant and water body.
Description
Technical field
The invention belongs to field of environment engineering, and in particular to a kind of floating vapor and its preparation method and application.
Background technique
In water treatment procedure, the pollutant how separation of economical and efficient has been enriched with is extremely important.Researchers exist
How to improve and is made that many effort in water treatment agent separation property.In past research, usually using the mode of precipitating to it
It is separated.Occur being embedded in Fe in water treatment agent in recent years3O4Nano particle, and the magnetic separated by external magnetic field
Separation；But due to Fe3O4In there is unstable ferrous iron, be easily oxidized and lose magnetism, cause to handle unstable.?
Having using aerobic particle mud as water treatment agent, advantage is to remove organic matter and with cramped construction and high settling property,
But granule sludge is as a kind of bioremediation, for biodegradability (Biodegradability, the also referred to as biology of waste water
The complexity that degradability, i.e. Organic Pollutants in Wastewater are biodegradable is one of key property of waste water) it is relatively high
Wastewater treatment efficiency is relatively good, but for substance difficult to degrade, such as dyestuff, heavy metal, antibiotic etc., effect is bad.
Compared to Magneto separate and granule sludge, floating partition method is a kind of efficient and convenient separation method, floats separation not
It needs by external magnetic field, and pollutant can be directly separated from the water surface.That applies at present more widely has vapor floating method.Vapour
Float glass process is to be adhered on Pollutants in Wastewater using the micro-bubble of high degree of dispersion as carrier, its buoyancy is made to be greater than gravity and upper
Floating resistance forms foam so that pollutant be made to float up to the water surface, then scrapes foam-expelling from the water surface with scraping slag equipment, realizes solid-liquid
Or the process of Liquid liquid Separation.Vapor floating method is mainly used for the indissoluble solution suspended matter in water removal, for the dissolution contact scar in waste water
Object, such as dyestuff, heavy metal, antibiotic.And in vapor floating method, since there are microbubbles, and microbubble is not sufficiently stable, with
The rupture of microbubble, it is possible to create the secondary pollution to water.These defects limit floating separation in water treatment field
Using.
With the rapid development and production-scale continuous expansion of industrial technology, the amount of industrial wastewater in China is increasing,
Wherein dyeing waste water amount accounts for about the 10% of total wastewater flow rate, and about 6 ~ 700,000,000 tons of dyeing waste waters are discharged into water environment every year.Heavy metal
(such as contain cadmium, nickel, mercury, zinc, copper) waste water is environmental pollution most serious and endangers one of maximum industrial wastewater to the mankind, I
State's heavy metal pollution of water body problem is very prominent, and the pollution rate of river,lake and reservior substrate is up to 80.1%.
Dyeing waste water is mainly derived from the processes such as the refining of the drift in dyeing and printing process, dyeing, stamp, arrangement, and each process produces
The different sewage of part is generated, so that its is complex in composition, coloration is deep, and alkalinity is strong, and water is big, and serious containing poisonous and harmful substances
Pollute environment, one of oneself of the comprehensive treatment of dyeing waste water the problem of becoming current urgent need to resolve.In recent years due to pharmaceuticals industry
Rapid development, the especially appearance of antibiotic bring serious pollution to the water resource in the world.Waste water containing antibiotic is
A kind of biodegrade difficulty is big, and residual quantity is high in environment, the strong high concentrated organic wastewater of bio-toxicity.
Not yet occur at present one kind can convenient and efficient processing dissolubility pollutant, and by floating method by separated from contaminants
Inorganic agent.Therefore, a kind of water treatment agent how is designed, dissolves contact scar to realize quickly and easily to handle and separate in waste water
Object is the direction of those skilled in the art's research.
Summary of the invention
In view of the above shortcomings of the prior art, it is an object of the invention to solve in the prior art in dyeing waste water
Difficult problem is separated after dissolubility pollutant processing, a kind of floating vapor is provided, dissolubility pollutant can be effectively treated, and locate
Pollutant after reason can float, to realize the quick separating of pollutant and water body.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is that it is such:
A kind of floating vapor, including hollow glass micropearl and silane coupling agent, the silane coupling agent are grafted on the hollow glass
Microballon outer surface, wherein the silane coupling agent is the silane coupling agent for having specificity to dyestuff, and hollow glass micropearl and silicon
The mass ratio of alkane coupling agent is 1~2:1.It is described to dyestuff have specificity silane coupling agent refer to can with dyestuff itself yin from
Subbase group or cation group interaction are to adsorb the silane coupling agent of the dyestuff.
Further, macromolecule organic monomer is grafted on the silane coupling agent of the floating vapor.
Further, the macromolecule organic monomer is 2- acrylamide-2-methyl propane sulfonic or methacryloxypropyl second
Base trimethyl ammonium chloride.
Further, the silane coupling agent be KH550, KH540, KH551, KH580, KH602, KH791, KH792,
One of KH901, KH902, ND-22, ND-42 or SI-69 or a variety of.
Further, the hollow glass micropearl is U.S. 3MTMThe iM16K type of company's production.
The present invention also provides a kind of preparation method of floating vapor, specific method includes the following steps:
S1, hollow glass micropearl is put at 70 DEG C~90 DEG C concentration range be 0.3mol/L~3mol/L sodium hydroxide it is molten
0.5~3h is stirred in liquid, pre-processed with increase the silanol group on its surface and 50 DEG C~120 DEG C at a temperature of it is dry,
S2, pretreated hollow glass micropearl is taken to be put into the mixed solution of ultrapure water, dehydrated alcohol and silane coupling agent,
The mass ratio of middle ultrapure water and dehydrated alcohol is 1:1, and mass fraction adds up to 95%~99%, and the mass fraction of silane coupling agent is
1%~5%, 0.5~3h is stirred under the conditions of temperature range is 40 DEG C~90 DEG C, and hollow glass micropearl surface is made to cover enough silicon
Alkane coupling agent, the hollow glass micropearl then coated in 50 DEG C~120 DEG C of at a temperature of drying to get silane coupling agent.
The present invention also provides a kind of preparation method of floating vapor, specific method includes the following steps:
S11, hollow glass micropearl is put into the sodium hydroxide that concentration range is 0.3mol/L~3mol/L at 70 DEG C~90 DEG C
0.5~3h is stirred in solution, pre-processed with increase the silanol group on its surface and 50 DEG C~120 DEG C at a temperature of it is dry
It is dry,
S12, pretreated hollow glass micropearl is taken to be put into the mixed solution of ultrapure water, dehydrated alcohol and silane coupling agent,
Wherein the mass ratio of ultrapure water and dehydrated alcohol is 1:1, and mass fraction adds up to 95%~99%, the mass fraction of silane coupling agent
It is 1%~5%, 0.5~3h is stirred under the conditions of temperature range is 40 DEG C~90 DEG C, covers hollow glass micropearl surface enough
Silane coupling agent, the hollow glass micropearl then coated in 50 DEG C~120 DEG C of at a temperature of drying to get silane coupling agent.
S13, be by volume by hollow glass micropearl obtained in S2 and ultrapure water 1:1~1:3 ratio mixing juxtaposition
In nitrogen environment, the potassium peroxydisulfate that quality accounts for reaction system gross mass 1%~5% is added, is 40 DEG C~90 DEG C in temperature range
Under the conditions of 5~20min of stirring to activate the amino of silane coupling agent institute band, quality is added later and accounts for reaction system total mass fraction
For 5%~25% macromolecule organic monomer, stirring, 1~5h of reaction are under the conditions of temperature range is 30 DEG C~60 DEG C to form
Products obtained therefrom is finally floated vapor for 24 hours in 50 DEG C~120 DEG C of at a temperature of drying to get final product by organic matter grafting.
Further, in the step S1 and S11, sodium hydroxide solution is prepared by ultrapure water, and the ultrapure water resistivity is
18.0MΩ/cm.In described step S1, S2, S11, S12 and S13, stirring rate is 60~240rpm.
Invention additionally discloses application of the floating vapor in sewage treatment.
Compared with prior art, the present invention has the advantage that
1, the floating vapor in the present invention uses hollow glass micropearl of the density less than 1, passes through the grafting pair on hollow glass micropearl
Dyestuff has the silane coupling agent of specificity, is grafted with the floating vapor of silane coupling agent after adsorbing soluble pollutants, can be fast
The stable floating of speed, subsequent separation process is also more economical convenient, so that the absorption and separation of dissolubility pollutant are realized, from root
Change existing separating technology on this.Using the floating vapor of grafted silane coupling agent KH550 on hollow glass micropearl, to orange 2
Removal rate be 92.35%.
2, the floating vapor in the present invention, which is used using silane coupling agent as bridge, is grafted on sky for macromolecule organic monomer
On heart glass microballoon, so that macromolecule organic monomer after adsorbing soluble pollutants, is also capable of the floating of fast and stable, and
It quickly can be separated to realize absorption and the quick separating of dissolubility pollutant from sewage.Had using grafting polymer
The floating vapor of machine object monomer, the removal rate to orange 2 are 87.53%, to the adsorption capacity of methylene blue be 436.82~
519.14mg/g, the adsorption capacity to malachite green are 637.36mg/g, and the adsorption capacity to basic fuchsin is 457.85mg/g,
Adsorption capacity to crystal violet is 399.40mg/g.
3, it due to the shape that hollow glass micropearl is in approximate spheres, is gathered around using vapor is floated made of hollow glass micropearl
There is biggish adsorption capacity.It is bigger using vapor specific surface area is floated made of hollow glass micropearl relative to traditional adsorbent,
Effective rate of utilization is higher, and the loss of raw material during the preparation process is small, therefore, can reduce being processed into for soluble contaminant
This, it is with good economic efficiency.
4, since hollow glass micropearl has, low in cost, intensity is high, water absorption rate is small, partial size concentration, good dispersion etc. are excellent
Therefore point has excellent stability using floating vapor prepared by the hollow glass micropearl, so that it is guaranteed that sewage treatment at work
Stability.
5, floating vapor prepared by the present invention, adsorption process are reversible.Floating vapor realize under alkaline condition to sun from
Desorption is realized in the absorption of sub- dyestuff at acid condition (pH < 1.5)；Or floating vapor is realized in acid condition to anion
Desorption is realized in the absorption of dyestuff at alkaline condition (pH > 12.5).Floating vapor after desorption is washed with neutral solution can be completed
Regenerative process further improves the economy of floating vapor to realize the recycling of floating vapor.
6, the preparation method of the floating vapor in the present invention is simple, and preparation cost is cheap, and in floating vapor preparation process, no
Using poisonous and hazardous chemicals, whole preparation process sanitation and hygiene, environmentally protective, low-carbon energy-saving.
Specific embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1:
S1, weighing 10g hollow glass micropearl are placed in the beaker of 500mL, and it is molten to add the NaOH that 300mL concentration is 0.5mol/L
Liquid stirs 1.5h in 80 DEG C of thermostat water bath with 100 revs/min of speed, after white suspension is cooling, uses ultrapure water
Cleaning and filtering repeatedly is carried out to it, until filtrate is neutrality, gained white solid is in thermostatic drying chamber with 60 DEG C of temperature
Degree is dry for 24 hours, obtains white powder.
S2, weigh 10g S1 in gained white powder, be placed in the beaker of 500mL, be added 150mL ultrapure water, 150mL without
Water-ethanol and 10mL Silane coupling agent KH550 stir 2h in 80 DEG C of thermostat water bath with 100 revs/min of speed, to white
After color suspension is cooling, it is cleaned and is filtered with ultrapure water, gained white solid is dry in 60 DEG C of thermostatic drying chamber
For 24 hours, products obtained therefrom is white powder.
The floating vapor of preparation carries out adsorption test in water bath with thermostatic control concussion case, and initial pH is 2, and floating vapor dosage is
1mg/ml, environment temperature are 45 DEG C, and dyestuff initial concentration is 100 mg/L, adsorption time 5h, and the removal rate to orange 2 is
92.35%。
Embodiment 2:
S11, weighing 10g hollow glass micropearl are placed in the beaker of 500mL, add the NaOH that 300mL concentration is 0.5mol/L
Solution stirs 1.5h in 80 DEG C of thermostat water bath with 100 revs/min of speed, and after white suspension is cooling, use is ultrapure
Water carries out cleaning and filtering repeatedly to it, until filtrate is neutrality, gained white solid is in thermostatic drying chamber with 60 DEG C
Temperature is dry for 24 hours, obtains white powder.
S12, gained white powder in 10g S1 is weighed, be placed in the beaker of 500mL, 150 mL ultrapure waters, 150mL is added
Dehydrated alcohol and 10mL Silane coupling agent KH550 stir 2h in 80 DEG C of thermostat water bath with 100 revs/min of speed, to
After white suspension is cooling, it is cleaned and is filtered with ultrapure water, gained white solid is dry in 60 DEG C of thermostatic drying chamber
For 24 hours, products obtained therefrom is white powder.
Products obtained therefrom is placed in 500mL round-bottomed flask in S13, weighing 10g S2, and 200mL ultrapure water is added, is passed through N2Punching
5min is washed, places it under closed oxygen free condition in 50 DEG C of thermostat water bath and is stirred with 100 revs/min of speed.Claim
Potassium peroxydisulfate 0.5g is measured, 2- acrylamide-2-methyl propane sulfonic (AMPS) 10g is respectively placed in 100mL beaker, and 10mL is added
Ultrapure water is stirred to being completely dissolved, and is passed through N2It rinses after 5min and is stirring concentration for the addition of 0.05g/mL persulfate aqueous solution
In the round-bottomed flask mixed, continuing stirring 10min makes the amino (- NH on surface2) activation, it is later that 1g/mLAMPS is water-soluble by concentration
Liquid is added in round-bottomed flask, continues to stir 3h, and the hollow glass for making AMPS be grafted on the grafting of AHGM(Silane coupling agent KH550 is micro-
Pearl) on, after white suspension is cooling, it is cleaned and is filtered with ultrapure water, freeze-day with constant temperature of the gained white solid at 60 DEG C
In case after drying for 24 hours, gained white powder is floating vapor.
The floating vapor of preparation carries out adsorption test in water bath with thermostatic control concussion case, and initial pH is 9, and floating vapor dosage is
1mg/ml, environment temperature are 50 DEG C, and dyestuff initial concentration is 1000 mg/L, adsorption time 5h, are held to the absorption of methylene blue
Amount is 436.82mg/g, and the adsorption capacity to malachite green is 637.36mg/g, and the adsorption capacity to basic fuchsin is
457.85mg/g, the adsorption capacity to crystal violet are 399.40mg/g.
Embodiment 3:
S11, weighing 10g hollow glass micropearl are placed in the beaker of 500mL, add the NaOH that 300mL concentration is 0.5mol/L
Solution stirs 2h in 80 DEG C of thermostat water bath with 100 revs/min of speed, after white suspension is cooling, uses ultrapure water
Cleaning and filtering repeatedly is carried out to it, until filtrate is neutrality, gained white solid is in thermostatic drying chamber with 60 DEG C of temperature
Degree is dry for 24 hours, obtains white powder.
S12, gained white powder in 10g S1 is weighed, be placed in the beaker of 500mL, 150mL ultrapure water, 150mL is added
Dehydrated alcohol and 10mL Silane coupling agent KH550 stir 2h in 80 DEG C of thermostat water bath with 100 revs/min of speed, to
After white suspension is cooling, it is cleaned and is filtered with ultrapure water, gained white solid is dry in 60 DEG C of thermostatic drying chamber
For 24 hours, products obtained therefrom is white powder.
Products obtained therefrom is placed in 500mL round-bottomed flask in S13, weighing 10g S2, and 200mL ultrapure water is added, is passed through N2Punching
5min is washed, places it under closed oxygen free condition in 50 DEG C of thermostat water bath and is stirred with 100 revs/min of speed.Claim
Potassium peroxydisulfate 0.5g is measured, 2- acrylamide-2-methyl propane sulfonic (AMPS) 10g is respectively placed in 100mL beaker, and 10mL is added
Ultrapure water is stirred to being completely dissolved, and is passed through N2It rinses after 5min and is stirring concentration for the addition of 0.05g/mL persulfate aqueous solution
In the round-bottomed flask mixed, continuing stirring 10min makes the amino (- NH on surface2) activation, it is later that 1g/mLAMPS is water-soluble by concentration
Liquid is added in round-bottomed flask, continues to stir 3h, is grafted on AMPS on AHGM, after white suspension is cooling, with ultrapure water pair
It cleans and filters, and for gained white solid in 60 DEG C of thermostatic drying chamber after drying for 24 hours, gained white powder is floating inhales
Agent.
Adsorption test is carried out in water bath with thermostatic control concussion case, initial pH is 9, and floating vapor dosage is 1mg/mL, environment temperature
Degree is 50 DEG C, and dyestuff initial concentration is 1000mg/L, adsorption time 5h, and the adsorption capacity to methylene blue is 502.33mg/
g。
Embodiment 4:
S11, weighing 10g hollow glass micropearl are placed in the beaker of 500mL, add the NaOH that 300mL concentration is 0.5mol/L
Solution stirs 1.5h in 80 DEG C of thermostat water bath with 100 revs/min of speed, and after white suspension is cooling, use is ultrapure
Water carries out cleaning and filtering repeatedly to it, until filtrate is neutrality, gained white solid is in thermostatic drying chamber with 60 DEG C
Temperature is dry for 24 hours, obtains white powder.
S12, gained white powder in 10g S1 is weighed, be placed in the beaker of 500mL, 150mL ultrapure water, 150mL is added
Dehydrated alcohol and 20mL Silane coupling agent KH550 stir 2h in 80 DEG C of thermostat water bath with 100 revs/min of speed, to
After white suspension is cooling, it is cleaned and is filtered with ultrapure water, gained white solid is dry in 60 DEG C of thermostatic drying chamber
For 24 hours, products obtained therefrom is white powder.
Products obtained therefrom is placed in 500mL round-bottomed flask in S13, weighing 10g S2, and 200mL ultrapure water is added, is passed through N2Punching
5min is washed, places it under closed oxygen free condition in 50 DEG C of thermostat water bath and is stirred with 100 revs/min of speed.Claim
Potassium peroxydisulfate 0.5g is measured, 2- acrylamide-2-methyl propane sulfonic (AMPS) 10g is respectively placed in 100mL beaker, and 10mL is added
Ultrapure water is stirred to being completely dissolved, and is passed through N2It rinses after 5min and is stirring concentration for the addition of 0.05g/mL persulfate aqueous solution
In the round-bottomed flask mixed, continuing stirring 10min makes the amino (- NH on surface2) activation, it is later that 1g/mL AMPS is water-soluble by concentration
Liquid is added in round-bottomed flask, continues to stir 3h, is grafted on AMPS on AHGM, after white suspension is cooling, with ultrapure water pair
It cleans and filters, and for gained white solid in 60 DEG C of thermostatic drying chamber after drying for 24 hours, gained white powder is floating inhales
Agent.
Adsorption test is carried out in water bath with thermostatic control concussion case, initial pH is 9, and floating vapor dosage is 1mg/mL, environment temperature
Degree is 50 DEG C, and dyestuff initial concentration is 1000 mg/L, adsorption time 5h, and the adsorption capacity to methylene blue is 455.27mg/
g。
Embodiment 5:
S11, weighing 10g hollow glass micropearl are placed in the beaker of 500mL, add the NaOH that 300mL concentration is 0.5mol/L
Solution stirs 1.5h in 80 DEG C of thermostat water bath with 100 revs/min of speed, and after white suspension is cooling, use is ultrapure
Water carries out cleaning and filtering repeatedly to it, until filtrate is neutrality, gained white solid is in thermostatic drying chamber with 60 DEG C
Temperature is dry for 24 hours, obtains white powder.
S12, gained white powder in 10g S1 is weighed, be placed in the beaker of 500mL, 150mL ultrapure water, 150mL is added
Dehydrated alcohol and 10mL Silane coupling agent KH550 stir 2h in 80 DEG C of thermostat water bath with 100 revs/min of speed, to
After white suspension is cooling, it is cleaned and is filtered with ultrapure water, gained white solid is dry in 60 DEG C of thermostatic drying chamber
For 24 hours, products obtained therefrom is white powder.
Products obtained therefrom is placed in 500mL round-bottomed flask in S13, weighing 10g S2, and 200mL ultrapure water is added, is passed through N2Punching
5min is washed, places it under closed oxygen free condition in 50 DEG C of thermostat water bath and is stirred with 100 revs/min of speed.Claim
Potassium peroxydisulfate 1g is measured, 2- acrylamide-2-methyl propane sulfonic (AMPS) 10g is respectively placed in 100mL beaker, and it is super that 10mL is added
Pure water is stirred to being completely dissolved, and is passed through N2It rinses after 5min and is stirring concentration for the addition of 0.1g/mL persulfate aqueous solution
Round-bottomed flask in, continuing to stir 10min makes the amino (- NH on surface2) activation, it is later 1g/mL AMPS aqueous solution by concentration
It is added in round-bottomed flask, continues to stir 3h, be grafted on AMPS on AHGM, after white suspension is cooling, with ultrapure water to it
It cleans and filters, for gained white solid in 60 DEG C of thermostatic drying chamber after drying for 24 hours, gained white powder is floating vapor.
Adsorption test is carried out in water bath with thermostatic control concussion case, initial pH is 9, and floating vapor dosage is 1mg/mL, environment temperature
Degree is 50 DEG C, and dyestuff initial concentration is 1000 mg/L, adsorption time 5h, and the adsorption capacity to methylene blue is 485.84mg/
g。
Embodiment 6:
S11, weighing 10g hollow glass micropearl are placed in the beaker of 500mL, add the NaOH that 300mL concentration is 0.5mol/L
Solution stirs 1.5h in 80 DEG C of thermostat water bath with 100 revs/min of speed, and after white suspension is cooling, use is ultrapure
Water carries out cleaning and filtering repeatedly to it, until filtrate is neutrality, gained white solid is in thermostatic drying chamber with 60 DEG C
Temperature is dry for 24 hours, obtains white powder.
S12, gained white powder in 10g S1 is weighed, be placed in the beaker of 500mL, 150mL ultrapure water, 150mL is added
Dehydrated alcohol and 10mL Silane coupling agent KH550 stir 2h in 80 DEG C of thermostat water bath with 100 revs/min of speed, to
After white suspension is cooling, it is cleaned and is filtered with ultrapure water, gained white solid is dry in 60 DEG C of thermostatic drying chamber
For 24 hours, products obtained therefrom is white powder.
Products obtained therefrom is placed in 500mL round-bottomed flask in S13, weighing 10g S2, and 200mL ultrapure water is added, is passed through N2Punching
5min is washed, places it under closed oxygen free condition in 50 DEG C of thermostat water bath and is stirred with 100 revs/min of speed.Claim
Potassium peroxydisulfate 0.5g is measured, 2- acrylamide-2-methyl propane sulfonic (AMPS) 15g is respectively placed in 100mL beaker, and 10mL is added
Ultrapure water is stirred to being completely dissolved, and is passed through N2It rinses after 5min and is stirring concentration for the addition of 0.05g/mL persulfate aqueous solution
In the round-bottomed flask mixed, continuing stirring 10min makes the amino (- NH on surface2) activation, it is later 1.5g/mL AMPS water by concentration
Solution is added in round-bottomed flask, continues to stir 3h, is grafted on AMPS on AHGM, after white suspension is cooling, uses ultrapure water
It is cleaned and is filtered, for gained white solid in 60 DEG C of thermostatic drying chamber after drying for 24 hours, gained white powder is floating inhales
Agent.
Adsorption test is carried out in water bath with thermostatic control concussion case, initial pH is 9, and floating vapor dosage is 1mg/mL, environment temperature
Degree is 50 DEG C, and dyestuff initial concentration is 1000 mg/L, adsorption time 5h, and the adsorption capacity to methylene blue is 519.14mg/
g。
Embodiment 7:
S11, weighing 10g hollow glass micropearl are placed in the beaker of 500mL, add the NaOH that 300mL concentration is 0.5mol/L
Solution stirs 1.5h in 80 DEG C of thermostat water bath with 100 revs/min of speed, and after white suspension is cooling, use is ultrapure
Water carries out cleaning and filtering repeatedly to it, until filtrate is neutrality, gained white solid is in thermostatic drying chamber with 60 DEG C
Temperature is dry for 24 hours, obtains white powder.
S12, gained white powder in 10g S1 is weighed, be placed in the beaker of 500mL, 150mL ultrapure water, 150mL is added
Dehydrated alcohol and 10mL Silane coupling agent KH550 stir 2h in 80 DEG C of thermostat water bath with 100 revs/min of speed, to
After white suspension is cooling, it is cleaned and is filtered with ultrapure water, gained white solid is dry in 60 DEG C of thermostatic drying chamber
For 24 hours, products obtained therefrom is white powder.
Products obtained therefrom is placed in 500mL round-bottomed flask in S13, weighing 10g S2, and 200mL ultrapure water is added, is passed through N2Punching
5min is washed, places it under closed oxygen free condition in 50 DEG C of thermostat water bath and is stirred with 100 revs/min of speed.Claim
Potassium peroxydisulfate 0.5g is measured, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (DMC) 20mL is respectively placed in 100mL beaker, in mistake
10mL ultrapure water is added in potassium sulfate to stir to being completely dissolved, is passed through N2Rinse 5min after by concentration be 0.05g/mL potassium peroxydisulfate
Aqueous solution is added in the round-bottomed flask stirred, and continuing stirring 10min makes the amino (- NH on surface2) activation, later by quality
The DMC aqueous solution that score is 75% is added in round-bottomed flask, continues to stir 3h, is grafted on DMC on AHGM, to white suspension
After cooling, it is cleaned and is filtered with ultrapure water, after gained white solid is dried for 24 hours in 50 DEG C of thermostatic drying chamber, gained
White powder is floating vapor.
The floating vapor of preparation carries out adsorption test in water bath with thermostatic control concussion case, and initial pH is 2, and floating vapor dosage is
1mg/ml, environment temperature are 45 DEG C, and dyestuff initial concentration is 100 mg/L, adsorption time 5h, and the removal rate to orange 2 is
87.53%。
Finally, it should be noted that technical side the above examples are only used to illustrate the technical scheme of the present invention and are not limiting
Case, those skilled in the art should understand that, modification or equivalent replacement of the technical solution of the present invention are made for those, and
The objective and range for not departing from the technical program, are intended to be within the scope of the claims of the invention.
Claims (10)
1. a kind of floating vapor, which is characterized in that including hollow glass micropearl and silane coupling agent, the silane coupling agent is grafted on
The hollow glass micropearl outer surface, wherein the silane coupling agent is the silane coupling agent for having specificity to dyestuff, and hollow
The mass ratio of glass microballoon and silane coupling agent is 1~2:1.
2. floating vapor according to claim 1, which is characterized in that be grafted with high score on the silane coupling agent of the floating vapor
Sub- Orqanics Monomer.
3. floating vapor according to claim 2, which is characterized in that the macromolecule organic monomer is 2- acrylamide-
2- methyl propane sulfonic acid or MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride.
4. floating vapor according to claim 1 or 2, which is characterized in that the silane coupling agent be KH550, KH540,
One of KH551, KH580, KH602, KH791, KH792, KH901, KH902, ND-22, ND-42 or SI-69 or a variety of.
5. floating vapor according to claim 1 or 2, which is characterized in that the hollow glass micropearl is U.S. 3MTMCompany is raw
The iM16K type of production.
6. a kind of prepare the preparation method for floating vapor in claim 1, which is characterized in that specific method includes the following steps:
S1, hollow glass micropearl is put at 70 DEG C~90 DEG C concentration range be 0.3mol/L~3mol/L sodium hydroxide it is molten
0.5~3h is stirred in liquid, pre-processed with increase the silanol group on its surface and 50 DEG C~120 DEG C at a temperature of it is dry,
S2, pretreated hollow glass micropearl is taken to be put into the mixed solution of ultrapure water, dehydrated alcohol and silane coupling agent,
The mass ratio of middle ultrapure water and dehydrated alcohol is 1:1, and mass fraction adds up to 95%~99%, and the mass fraction of silane coupling agent is
1%~5%, 0.5~3h is stirred under the conditions of temperature range is 40 DEG C~90 DEG C, and hollow glass micropearl surface is made to cover enough silicon
Alkane coupling agent, the hollow glass micropearl then coated in 50 DEG C~120 DEG C of at a temperature of drying to get silane coupling agent.
7. a kind of prepare the preparation method for floating vapor in claim 2, which is characterized in that specific method includes the following steps:
S11, hollow glass micropearl is put into the sodium hydroxide that concentration range is 0.3mol/L~3mol/L at 70 DEG C~90 DEG C
0.5~3h is stirred in solution, pre-processed with increase the silanol group on its surface and 50 DEG C~120 DEG C at a temperature of it is dry
It is dry,
S12, pretreated hollow glass micropearl is taken to be put into the mixed solution of ultrapure water, dehydrated alcohol and silane coupling agent,
Wherein the mass ratio of ultrapure water and dehydrated alcohol is 1:1, and mass fraction adds up to 95%~99%, the mass fraction of silane coupling agent
It is 1%~5%, 0.5~3h is stirred under the conditions of temperature range is 40 DEG C~90 DEG C, covers hollow glass micropearl surface enough
Silane coupling agent, the hollow glass micropearl then coated in 50 DEG C~120 DEG C of at a temperature of drying to get silane coupling agent.
S13, be by volume by hollow glass micropearl obtained in S2 and ultrapure water 1:1~1:3 ratio mixing be placed in nitrogen
In compression ring border, the potassium peroxydisulfate that quality accounts for reaction system gross mass 1%~5% is added, is 40 DEG C~90 DEG C conditions in temperature range
For the lower 5~20min that stirs to activate the amino of silane coupling agent institute band, it is 5% that quality is added later and accounts for reaction system total mass fraction
~25% macromolecule organic monomer, stirring, 1~5h of reaction are organic to be formed under the conditions of temperature range is 30 DEG C~60 DEG C
Products obtained therefrom is finally floated vapor for 24 hours in 50 DEG C~120 DEG C of at a temperature of drying to get final product by object grafting.
8. the preparation method of floating vapor according to claim 6 or 7, which is characterized in that in the step S1 and S11, hydrogen
Sodium hydroxide solution is prepared by ultrapure water, and the ultrapure water resistivity is 18.0M Ω/cm.
9. the preparation method of floating vapor according to claim 6 or 7, which is characterized in that described step S1, S2, S11, S12
In S13, stirring rate is 60~240rpm.
10. a kind of be used for the application in sewage treatment for the described in any item floating vapors of claim 1-9.
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