CN108689469A - A kind of methylcellulose graphene oxide flocculant aid and preparation method thereof - Google Patents
A kind of methylcellulose graphene oxide flocculant aid and preparation method thereof Download PDFInfo
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- CN108689469A CN108689469A CN201810562871.0A CN201810562871A CN108689469A CN 108689469 A CN108689469 A CN 108689469A CN 201810562871 A CN201810562871 A CN 201810562871A CN 108689469 A CN108689469 A CN 108689469A
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- graphene oxide
- methylcellulose
- microcapsules
- flocculant
- flocculant aid
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
-
- 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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
-
- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
-
- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The present invention provides a kind of methylcellulose graphene oxide flocculant aids and preparation method thereof.The methylcellulose graphene oxide flocculant aid includes following component in parts by weight:75 ~ 88 parts of methylcellulose graphene oxide microcapsules, 12 ~ 25 parts of dispersant;The methylcellulose graphene oxide microcapsules include core material and wrap up the wall material of the core material, and the mass ratio of the wall material and core material is 0.8:1~2:1;The core material is graphene oxide, and the wall material is methylcellulose.Methylcellulose graphene oxide flocculant aid of the present invention can improve the purifying rate of unit flocculant while improving flocculation efficiency, maintain or reduce the dosage of flocculant.
Description
Technical field
The present invention relates to the technical fields of water process water purification agent, more particularly, to a kind of methylcellulose graphite oxide
Alkene flocculant aid and preparation method thereof.
Background technology
Flocculation process is indispensable key link in sewage treatment process.During sewage disposal, often need
Flocculant is added, so that the suspended particulates in sewage is gathered and becomes larger to form floc sedimentation, to make the coagulation of particle.Flocculated principle is such as
Under:Positive (negative) electrical group is carried in flocculant, can neutralize in water and electrically be difficult to the particle detached with negative (just), is reduced
Its potential, and using aggregation property these particles are concentrated, cotton-shaped coagulating sedimentation is formed, and pass through physics or chemical method
It separates.
Conductive agent is added in the meeting having in existing flocculant, and its object is to, to electron transmission, make to flocculate by conductive agent
The charge generated in journey is transmitted to floccule surface by conductive agent, and the charge inside floccule can be also transmitted to by conductive agent
Floccule surface, it is easier to which the balance for breaking sewage system improves flocculated speed (flocculation efficiency).But, it has been found that
Partial flocculation efficiency around flocculant containing conductive agent is to be improved, but the flocculating and purifying of entire sewage disposal system
Rate (i.e. removal rate) is not improved but, or even is declined so that is needed to add more flocculants and be can be only achieved original wadding
Solidifying purifying rate, increases economic cost, loses more than gain instead in this way.
Invention content
The present invention is solves the problems, such as described in the above-mentioned prior art, provides a kind of methylcellulose graphene oxide and flocculates and helps
Agent, the methylcellulose graphene oxide flocculant aid can improve unit flocculant while improving flocculation efficiency
Purifying rate (removal rate) maintains or reduces the dosage of flocculant.
It is a further object of the present invention to provide the preparation methods of the methylcellulose graphene oxide flocculant aid.
In order to solve the above technical problems, the technical solution adopted by the present invention is:
A kind of methylcellulose graphene oxide flocculant aid, including following component in parts by weight:Methyl is fine
Plain 75~88 parts of the graphene oxide microcapsules of dimension, 12~25 parts of dispersant;The methylcellulose graphene oxide microcapsules packet
It includes core material and wraps up the wall material of the core material, the mass ratio of the wall material and core material is 0.8:1~2:1;The core material is oxidation
Graphene, the wall material are methylcellulose.
Present inventor studies the conductive agent of existing flocculant, is found that while that conductive agent is played in flocculation process
Charge transfer acts on, and improves flocculated speed, but it also accelerates the charge consumption of flocculant simultaneously, flocculant is having enough time expanding
Dissipate before, charge has just been consumed, flocculant can only useful effect in part, this has also been resulted in around flocculant
Partial flocculation it is efficient, but the not high reason of flocculating and purifying rate (i.e. removal rate) of entire sewage disposal system.
In this regard, the present invention is improved the conductive agent of existing flocculant, graphene oxide is chosen as conductive agent, and will
Graphene oxide makes microcapsules, is combined together with dispersant, and in flocculation process, the methylcellulose graphene oxide is micro-
Capsule can disperse rapidly, graphene oxide during dispersion in methylcellulose graphene oxide microcapsules can by by
It gradually discharges, plays the role of charge transfer to flocculation process, improve flocculated speed.Compared with existing conductive agent, due to this Shen
Please the methylcellulose graphene oxide microcapsules be gradually to discharge, the charge of flocculant can be before being consumed totally just
It is uniformly dispersed with together with graphene oxide, therefore flocculated speed and whole flocculating and purifying rate can be improved.
In order to reach said effect, the dispersion of graphene oxide and release opportunity are crucial, in the present invention, it is preferred to water
Wall material of the methylcellulose of dissolubility as cladding graphene oxide, and the ratio by designing wall material and core material so that methyl
Graphene oxide in cellulose oxidation graphene microcapsules can effectively play a role in flocculation process.
In order to enable methylcellulose graphene oxide microcapsules efficiently and effectively to disperse, methylcellulose of the present invention
Graphene oxide flocculant aid also includes dispersant, and studies and obtain methylcellulose graphene oxide microcapsules and dispersant
Proportioning.Preferably, the methylcellulose graphene oxide flocculant aid includes following component in parts by weight:Methyl
84 parts of cellulose oxidation graphene microcapsules, 16 parts of dispersant.
Preferably, the dispersant is one or more of polyvinyl alcohol, polyethylene, pyrrolidones.
It is highly preferred that the dispersant is the mixture of polyvinyl alcohol and pyrrolidones;The polyvinyl alcohol and pyrrolidines
The mass ratio of ketone is 1:2.
The release opportunity of graphene oxide is the key that the present invention, very much not with wall material in existing microcapsules and the ratio of core material
Identical, the present invention show that the zone of reasonableness of the mass ratio of wall material and core material is 0.8 by research:1~2:1.Preferably, the wall
The mass ratio of material and core material is 1:1.
Preferably, the preparation method of the methylcellulose graphene oxide microcapsules includes the following steps:
S1. graphene oxide is placed in ultrasonic disperse in pure water, obtains graphene oxide dispersion;
S2. wall material is added to the graphene oxide dispersion, temperature is 30~45 DEG C, pressure is 0.5~2MPa's
Under inert atmosphere, 30~60min is stirred, mixing speed is 800~1500r/min;
S3. after stirring terminates, solid product is collected in filtering, and freeze-drying is micro- to get methylcellulose graphene oxide
Capsule.
Further, in step S1, the ratio of the graphene oxide and pure water is 0.1~0.3g:10ml, preferably
0.1g:10ml。
Further, in step S2, the wall material is made into the solution that mass fraction is 30~40wt%, is added into institute
State graphene oxide dispersion.
Preferably, the grain size of the graphene oxide is 300~1200nm, preferably 500~800nm.Preferably, described
Inert gas is nitrogen.
Preferably, in step S2, wall material is added to the graphene oxide dispersion, temperature is 35 DEG C, pressure is
Under the inert atmosphere of 1MPa, 30min, mixing speed 800r/min are stirred.
The present invention studies the reaction condition of microcapsule coated process, finds the inert gas environment in certain pressure
Under, the surface of graphene oxide can first coat a thin layer of air film, and wall material is coated on outside again, effectively prevent wall material stifled in this way
The aperture of graphene oxide composite material is filled in, and after freeze-drying, wall material and oxygen in methylcellulose graphene oxide microcapsules
Certain gap is still stayed between graphite alkene, is contacted convenient for the release of graphene oxide and with flocculant.
The present invention also provides the preparation methods of the methylcellulose graphene oxide flocculant aid.The preparation method packet
Include following steps:
S1. methylcellulose graphene oxide microcapsules are prepared;
S2. methylcellulose graphene oxide microcapsules are mixed with dispersant in proportion.
The present invention further provides the applications of the methylcellulose graphene oxide flocculant aid.The methylcellulose
Graphene oxide flocculant aid can be applied in sewage disposal.
Further, the application is to improve the flocculation efficiency of flocculant in sewage disposal.Specifically, the application is to incite somebody to action
The methylcellulose graphene oxide flocculant aid is added to flocculant in sewage, is stirred, and is flocculated, sedimentation.The flocculation
The mass ratio of agent and methylcellulose graphene oxide flocculant aid is 8~10:1, preferably 9:1.
The methylcellulose graphene oxide flocculant aid can be efficiently applied to existing flocculant system, further
Ground, the flocculant include but not limited to aluminum sulfate, polyoxygenated aluminium, iron chloride and ferrous sulfate, polyacrylamide.Preferably,
The flocculant is polyacrylamide.
Compared with prior art, the beneficial effects of the invention are as follows:
The present invention is improved the conductive agent of existing flocculant, chooses graphene oxide as conductive agent, and will oxidation
Graphene makes microcapsules, is combined together with dispersant, in flocculation process, the methylcellulose graphene oxide microcapsules
It can disperse rapidly, graphene oxide during dispersion in methylcellulose graphene oxide microcapsules can be released gradually
It puts, plays the role of charge transfer to flocculation process, improve flocculated speed, while can also improve the purifying rate of unit flocculant
(removal rate) maintains or reduces the dosage of flocculant.
Specific implementation mode
By following specific examples, present invention be described in more detail, it should be understood that specific implementation described herein
Example is only used for explaining the present invention, is not intended to limit the present invention, can carry out various change in the range of right of the present invention limits
Become.
Unless otherwise noted, raw material involved in following embodiment are commercially available, equipment used and
Technique is known to those skilled in the art.Wherein, graphene oxide is that the limited public affairs of graphite science and technology are contained by Hunan state
Department's production, grain size is 500~800nm.Polyacrylamide is purchased from Sinopharm Chemical Reagent Co., Ltd., and molecular weight is
3000000.
Examples 1 to 7 and comparative example 1~4
A kind of methylcellulose graphene oxide flocculant aid includes methylcellulose graphene oxide microcapsules and dispersion
Agent.Methylcellulose graphene oxide microcapsules include core material and wall material, and core material is graphene oxide, and wall material is Methyl cellulose
Element.
In each embodiment and comparative example, dosage (A), the dosage of dispersant of methylcellulose graphene oxide microcapsules
(B), the design parameters such as mass ratio (D) of the type (C), wall material of dispersant and core material are as shown in table 1.
The preparation method of methylcellulose graphene oxide flocculant aid includes the following steps:
S1. methylcellulose graphene oxide microcapsules are prepared, are included the following steps:
S11. graphene oxide is placed in ultrasonic disperse in pure water, the ratio of graphene oxide and pure water is 0.1g:10ml,
Obtain graphene oxide dispersion;
S12. wall material is made into the solution that mass fraction is 30wt%, gained graphene oxide dispersion is added, in temperature
Under the nitrogen atmosphere for being 1MPa for 35 DEG C, pressure, 30min, mixing speed 800r/min are stirred.
S13. after stirring terminates, solid product is collected in filtering, is freeze-dried to get methylcellulose graphene oxide
Microcapsules.
S2. methylcellulose graphene oxide microcapsules are mixed with dispersant according to the above ratio.
Table 1
Embodiment 8
As different from Example 1, the preparation method of methylcellulose graphene oxide microcapsules includes in the present embodiment
Following steps:
S11. graphene oxide is placed in ultrasonic disperse in pure water, the ratio of graphene oxide and pure water is 0.1g:10ml,
Obtain graphene oxide dispersion;
S12. wall material is made into the solution that mass fraction is 30wt%, gained graphene oxide dispersion is added, in temperature
Under the nitrogen atmosphere for being 0.5MPa for 35 DEG C, pressure, 30min, mixing speed 800r/min are stirred.
S13. after stirring terminates, solid product is collected in filtering, is freeze-dried to get methylcellulose graphene oxide
Microcapsules.
Other Step By Condition parameters are same as Example 1.
Embodiment 9
As different from Example 1, the preparation method of methylcellulose graphene oxide microcapsules includes in the present embodiment
Following steps:
S11. graphene oxide is placed in ultrasonic disperse in pure water, the ratio of graphene oxide and pure water is 0.1g:10ml,
Obtain graphene oxide dispersion;
S12. wall material is made into the solution that mass fraction is 30wt%, gained graphene oxide dispersion is added, in temperature
Under the nitrogen atmosphere for being 2MPa for 35 DEG C, pressure, 30min, mixing speed 800r/min are stirred.
S13. after stirring terminates, solid product is collected in filtering, is freeze-dried to get methylcellulose graphene oxide
Microcapsules.
Other Step By Condition parameters are same as Example 1.
Embodiment 10
As different from Example 1, the preparation method of methylcellulose graphene oxide microcapsules includes in the present embodiment
Following steps:
S11. graphene oxide is placed in ultrasonic disperse in pure water, the ratio of graphene oxide and pure water is 0.1g:10ml,
Obtain graphene oxide dispersion;
S12. wall material is made into the solution that mass fraction is 30wt%, gained graphene oxide dispersion is added, in temperature
Under the nitrogen atmosphere for being 1MPa for 30 DEG C, pressure, 30min, mixing speed 1500r/min are stirred.
S13. after stirring terminates, solid product is collected in filtering, is freeze-dried to get methylcellulose graphene oxide
Microcapsules.
Other Step By Condition parameters are same as Example 1.
Embodiment 11
As different from Example 1, the preparation method of methylcellulose graphene oxide microcapsules includes in the present embodiment
Following steps:
S11. graphene oxide is placed in ultrasonic disperse in pure water, the ratio of graphene oxide and pure water is 0.1g:10ml,
Obtain graphene oxide dispersion;
S12. wall material is made into the solution that mass fraction is 30wt%, gained graphene oxide dispersion is added, in temperature
Under the nitrogen atmosphere for being 1MPa for 45 DEG C, pressure, 30min, mixing speed 800r/min are stirred.
S13. after stirring terminates, solid product is collected in filtering, is freeze-dried to get methylcellulose graphene oxide
Microcapsules.
Other Step By Condition parameters are same as Example 1.
Comparative example 5
As different from Example 1, the preparation method of methylcellulose graphene oxide microcapsules includes in the present embodiment
Following steps:
S11. graphene oxide is placed in ultrasonic disperse in pure water, the ratio of graphene oxide and pure water is 0.1g:10ml,
Obtain graphene oxide dispersion;
S12. wall material is made into the solution that mass fraction is 30wt%, gained graphene oxide dispersion is added, in temperature
Be for 35 DEG C, pressure normal pressure nitrogen atmosphere under, stir 30min, mixing speed 800r/min.
S13. after stirring terminates, solid product is collected in filtering, is freeze-dried to get methylcellulose graphene oxide
Microcapsules.
Other conditional parameters are same as Example 1.
Comparative example 6
As different from Example 1, the preparation method of methylcellulose graphene oxide microcapsules includes in the present embodiment
Following steps:
S11. graphene oxide is placed in ultrasonic disperse in pure water, the ratio of graphene oxide and pure water is 0.1g:10ml,
Obtain graphene oxide dispersion;
S12. wall material is made into the solution that mass fraction is 30wt%, gained graphene oxide dispersion is added, in temperature
Under the nitrogen atmosphere for being 3MPa for 35 DEG C, pressure, 30min, mixing speed 800r/min are stirred.
S13. after stirring terminates, solid product is collected in filtering, is freeze-dried to get methylcellulose graphene oxide
Microcapsules.
Other Step By Condition parameters are same as Example 1.
Test
Water purification performance is carried out using methylcellulose graphene oxide flocculant aid obtained by the various embodiments described above and comparative example
Test, condition are as follows:Take identical outdoor elements polluted-water water sample (abbreviation raw water, after tested the turbidity of raw water be
820NTU, turbidity test foundation"The measurement of GB 13200-1991 water turbidities"), flocculant and methylcellulose are aoxidized into stone
Black alkene flocculant aid presses certain usage ratio, adds in the water sample of isometric raw water (stirring 5min), calculates when water sample
Turbidity is down to the dosage of required flocculant when 1NTU, and record static balance time (stops the use to settlement stability after stirring
When).
Flocculant chooses polyacrylamide, and flocculant is 9 in mass ratio with methylcellulose graphene oxide flocculant aid:
1 ratio adds in the water sample of isometric raw water.In addition, using be added without methylcellulose graphene oxide flocculant aid as
Reference examples.Shown in test result table 2:
Table 2
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
All any modification, equivalent and improvement etc., should be included in the claims in the present invention made by within the spirit and principle of invention
Protection domain within.
Claims (7)
1. a kind of methylcellulose graphene oxide flocculant aid, which is characterized in that including following group in parts by weight
Point:75 ~ 88 parts of methylcellulose graphene oxide microcapsules, 12 ~ 25 parts of dispersant;The methylcellulose graphene oxide
Microcapsules include core material and wrap up the wall material of the core material, and the mass ratio of the wall material and core material is 0.8:1~2:1;The core material
For graphene oxide, the wall material is methylcellulose.
2. methylcellulose graphene oxide flocculant aid according to claim 1, which is characterized in that including pressing weight below
Measure the component that number calculates:84 parts of methylcellulose graphene oxide microcapsules, 16 parts of dispersant.
3. methylcellulose graphene oxide flocculant aid according to claim 1, which is characterized in that the wall material and core
The mass ratio of material is 1:1.
4. methylcellulose graphene oxide flocculant aid according to claim 1 or 2, which is characterized in that the dispersion
Agent is one or more of polyvinyl alcohol, polyethylene, pyrrolidones.
5. methylcellulose graphene oxide flocculant aid according to claim 4, which is characterized in that the dispersant is
The mixture of polyvinyl alcohol and pyrrolidones;The mass ratio of the polyvinyl alcohol and pyrrolidones is 1:2.
6. methylcellulose graphene oxide flocculant aid according to claim 1, which is characterized in that the Methyl cellulose
The preparation method of plain graphene oxide microcapsules includes the following steps:
S1. graphene oxide is placed in ultrasonic disperse in pure water, obtains graphene oxide dispersion;
S2. wall material is added to the graphene oxide dispersion, in the indifferent gas that temperature is 30 ~ 45 DEG C, pressure is 0.5 ~ 2MPa
Under atmosphere, 30 ~ 60 min are stirred, mixing speed is 800 ~ 1500 r/min;
S3. after stirring terminates, solid product is collected in filtering, is freeze-dried to get the micro- glue of methylcellulose graphene oxide
Capsule.
7. the preparation method of any one of the claim 1 ~ 6 methylcellulose graphene oxide flocculant aid, which is characterized in that
Include the following steps:
S1. methylcellulose graphene oxide microcapsules are prepared;
S2. methylcellulose graphene oxide microcapsules are mixed with dispersant in proportion.
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Application publication date: 20181023 |