CN108840419A - A kind of carboxymethyl cellulose graphene flocculant aid and preparation method thereof - Google Patents
A kind of carboxymethyl cellulose graphene flocculant aid and preparation method thereof Download PDFInfo
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- CN108840419A CN108840419A CN201810563249.1A CN201810563249A CN108840419A CN 108840419 A CN108840419 A CN 108840419A CN 201810563249 A CN201810563249 A CN 201810563249A CN 108840419 A CN108840419 A CN 108840419A
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- carboxymethyl cellulose
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- flocculant
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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
- C02F1/54—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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- 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
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
The present invention provides a kind of carboxymethyl cellulose graphene flocculant aids and preparation method thereof.The carboxymethyl cellulose graphene flocculant aid includes following component in parts by weight：70 ~ 90 parts of carboxymethyl cellulose graphene microcapsules, 10 ~ 30 parts of dispersing agent；The carboxymethyl cellulose graphene microcapsules include core material and the wall material for wrapping up the core material, and the mass ratio of the wall material and core material is 0.5:1~2:1；The core material is graphene, and the wall material is carboxymethyl cellulose.Carboxymethyl cellulose graphene 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 carboxymethyl cellulose graphene
Flocculant aid and preparation method thereof.
Background technique
Flocculation process is indispensable key link in sewage treatment process.During sewage treatment, often need
Flocculant is added, gathers the suspended particulates in sewage and becomes larger to form floc sedimentation, to make the coagulation of particle.Flocculated principle is such as
Under：The group that positive (negative) electrical property is had in flocculant can neutralize in water and electrically be difficult to isolated particle with negative (just), reduce
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 treatment system
Rate (i.e. removal rate) is not improved but, or even decline, so that needing to add more flocculants can be only achieved original wadding
Solidifying purifying rate, increases economic cost, loses more than gain instead in this way.
Summary of the invention
The present invention is solves the problems, such as described in the above-mentioned prior art, provides a kind of carboxymethyl cellulose graphene and flocculates and helps
Agent, the carboxymethyl cellulose graphene flocculant aid can improve the net of unit flocculant while improving flocculation efficiency
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 carboxymethyl cellulose graphene flocculant aid.
In order to solve the above technical problems, the technical solution adopted by the present invention is that：
A kind of carboxymethyl cellulose graphene flocculant aid, including following component in parts by weight：Carboxymethyl is fine
Tie up plain 70~90 parts, 10~30 parts of dispersing agent of microcapsules of graphene；The carboxymethyl cellulose graphene microcapsules include core material
With the wall material for wrapping up the core material, the mass ratio of the wall material and core material is 0.5:1~2:1；The core material is graphene, described
Wall material is carboxymethyl cellulose.
Present inventor studies the conductive agent of existing flocculant, is found that while that conductive agent is played in flocculation process
Charge transfer effect improves flocculated speed, but its charge consumption for also accelerating flocculant simultaneously, flocculant are 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 high-efficient, but the not high reason of flocculating and purifying rate (i.e. removal rate) of entire sewage treatment system.
In this regard, the present invention improves the conductive agent of existing flocculant, graphene is chosen as conductive agent, and by graphite
Alkene is made into microcapsules, combines together with dispersing agent, and in flocculation process, the carboxymethyl cellulose graphene microcapsules can be fast
Speed dispersion, graphene during dispersion in carboxymethyl cellulose graphene microcapsules can gradually be discharged, to flocculating
Journey plays the role of charge transfer, improves flocculated speed.Compared with existing conductive agent, due to herein described carboxymethyl cellulose
Plain graphene microcapsules are gradually to discharge, and the charge of flocculant can just disperse together with graphene equal before being consumed totally
It is even, therefore flocculated speed and whole flocculating and purifying rate can be improved.
In order to reach said effect, the dispersion of graphene and release opportunity are keys, in the present invention, it is preferred to water-soluble
Wall material of the carboxymethyl cellulose as coated graphite alkene, and by the ratio of design wall material and core material, so that carboxymethyl cellulose
Graphene in plain graphene microcapsules can effectively play a role in flocculation process.
In order to enable carboxymethyl cellulose graphene microcapsules efficiently and effectively to disperse, carboxymethyl cellulose of the present invention
Graphene flocculant aid also includes dispersing agent, and studies the proportion for obtaining carboxymethyl cellulose graphene microcapsules and dispersing agent.
Preferably, the carboxymethyl cellulose graphene flocculant aid includes following component in parts by weight：Carboxymethyl cellulose
82 parts of plain graphene microcapsules, 18 parts of dispersing agent.
Preferably, the dispersing agent is one or more of polyvinyl alcohol, polyethylene, Sodium Polyacrylate.
It is highly preferred that the dispersing agent is the mixture of polyvinyl alcohol and Sodium Polyacrylate；The polyvinyl alcohol and poly- third
The mass ratio of olefin(e) acid sodium is 1:1.
The release opportunity of graphene be the key that it is of the invention, with wall material in existing microcapsules and the ratio of core material very much not phase
Together, the present invention show that the zone of reasonableness of the mass ratio of wall material and core material is 0.5 by research:1~2:1.Preferably, the wall material
Mass ratio with core material is 1:1.
Preferably, the preparation method of the carboxymethyl cellulose graphene microcapsules includes the following steps：
S1. graphene is placed in ultrasonic disperse in pure water, obtains graphene dispersing solution；
S2. wall material is added to the graphene dispersing solution, in the inertia that temperature is 30~45 DEG C, pressure is 0.5~2MPa
Under atmosphere, 30~60min is stirred, mixing speed is 800~1500r/min；
S3. after stirring terminates, solid product is collected in filtering, is freeze-dried to get the micro- glue of carboxymethyl cellulose graphene
Capsule.
Further, in step S1, the ratio of the graphene 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 dispersing solution.
Preferably, the partial size of the graphene is 300~1200nm, preferably 500~800nm.Preferably, the inertia
Gas is nitrogen.
Preferably, in step S2, wall material is added to the graphene dispersing solution, temperature is 35 DEG C, pressure is 1MPa's
Under inert atmosphere, 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 can first coat a thin layer of air film, and wall material is coated on outside again, and wall material is effectively prevent to block stone in this way
The aperture of black alkene material, and after freeze-drying, in carboxymethyl cellulose graphene microcapsules between wall material and graphene still
Certain gap is stayed, is contacted convenient for the release of graphene and with flocculant.
The present invention also provides the preparation methods of the carboxymethyl cellulose graphene flocculant aid.The preparation method includes
Following steps：
S1. carboxymethyl cellulose graphene microcapsules are prepared；
S2. carboxymethyl cellulose graphene microcapsules are mixed with dispersing agent in proportion.
The present invention further provides the applications of the carboxymethyl cellulose graphene flocculant aid.The carboxymethyl cellulose
Graphene flocculant aid can be applied in sewage treatment.
Further, the application is the flocculation efficiency for improving flocculant in sewage treatment.Specifically, the application is to incite somebody to action
The carboxymethyl cellulose graphene flocculant aid and flocculant are added in sewage, are stirred, and are flocculated, sedimentation.The flocculant
Mass ratio with carboxymethyl cellulose graphene flocculant aid is 8~10：1, preferably 9:1.
The carboxymethyl cellulose graphene flocculant aid can be efficiently applied to existing flocculant system, further
Ground, the flocculant include but is 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 improves the conductive agent of existing flocculant, chooses graphene and does as conductive agent, and by graphene
It at microcapsules, is combined together with dispersing agent, in flocculation process, the carboxymethyl cellulose graphene microcapsules can divide rapidly
It dissipates, graphene during dispersion in carboxymethyl cellulose graphene microcapsules can gradually be discharged, and be risen to flocculation process
It is acted on to charge transfer, improves flocculated speed, while can also improve the purifying rate (removal rate) of unit flocculant, maintain or subtract
The dosage of few flocculant.
Specific embodiment
By following specific embodiments, present invention be described in more detail, it should be understood that specific implementation described herein
Example for explaining only the invention, is not intended to limit the present invention, and 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 is raw for Hunan Guo Sheng graphite Science and Technology Ltd.
It produces, partial size is 500~800nm.Polyacrylamide is purchased from Sinopharm Chemical Reagent Co., Ltd., and molecular weight is 3,000,000.
Examples 1 to 7 and comparative example 1~4
A kind of carboxymethyl cellulose graphene flocculant aid includes carboxymethyl cellulose graphene microcapsules and dispersing agent.Carboxylic
Methylcellulose graphene microcapsules include core material and wall material, and core material is graphene, and wall material is carboxymethyl cellulose.
In each embodiment and comparative example, dosage (A), the dosage of dispersing agent of carboxymethyl cellulose graphene microcapsules
(B), the design parameters such as mass ratio (D) of the type (C), wall material of dispersing agent and core material are as shown in table 1.
The preparation method of carboxymethyl cellulose graphene flocculant aid includes the following steps：
S1. carboxymethyl cellulose graphene microcapsules are prepared, are included the following steps：
S11. graphene is placed in ultrasonic disperse in pure water, the ratio of graphene and pure water is 0.1g:10ml obtains graphite
Alkene dispersion liquid；
S12. wall material is made into the solution that mass fraction is 30wt%, gained graphene dispersing solution is added, be 35 in temperature
DEG C, pressure be 1MPa nitrogen atmosphere under, stir 30min, mixing speed 800r/min.
S13. after stirring terminates, solid product is collected in filtering, is freeze-dried micro- to get carboxymethyl cellulose graphene
Capsule.
S2. carboxymethyl cellulose graphene microcapsules are mixed with dispersing agent according to the above ratio.
Table 1
Embodiment 8
Unlike the first embodiment, in the present embodiment the preparation method of carboxymethyl cellulose graphene microcapsules include with
Lower step：
S11. graphene is placed in ultrasonic disperse in pure water, the ratio of graphene and pure water is 0.1g:10ml obtains graphite
Alkene dispersion liquid；
S12. wall material is made into the solution that mass fraction is 30wt%, gained graphene dispersing solution is added, be 35 in temperature
DEG C, pressure be 0.5MPa nitrogen atmosphere under, stir 30min, mixing speed 800r/min.
S13. after stirring terminates, solid product is collected in filtering, is freeze-dried micro- to get carboxymethyl cellulose graphene
Capsule.
Other Step By Condition parameters are same as Example 1.
Embodiment 9
Unlike the first embodiment, in the present embodiment the preparation method of carboxymethyl cellulose graphene microcapsules include with
Lower step：
S11. graphene is placed in ultrasonic disperse in pure water, the ratio of graphene and pure water is 0.1g:10ml obtains graphite
Alkene dispersion liquid；
S12. wall material is made into the solution that mass fraction is 30wt%, gained graphene dispersing solution is added, be 35 in temperature
DEG C, pressure be 2MPa nitrogen atmosphere under, stir 30min, mixing speed 800r/min.
S13. after stirring terminates, solid product is collected in filtering, is freeze-dried micro- to get carboxymethyl cellulose graphene
Capsule.
Other Step By Condition parameters are same as Example 1.
Embodiment 10
Unlike the first embodiment, in the present embodiment the preparation method of carboxymethyl cellulose graphene microcapsules include with
Lower step：
S11. graphene is placed in ultrasonic disperse in pure water, the ratio of graphene and pure water is 0.1g:10ml obtains graphite
Alkene dispersion liquid；
S12. wall material is made into the solution that mass fraction is 30wt%, gained graphene dispersing solution is added, be 30 in temperature
DEG C, pressure be 1MPa nitrogen atmosphere under, stir 30min, mixing speed 1500r/min.
S13. after stirring terminates, solid product is collected in filtering, is freeze-dried micro- to get carboxymethyl cellulose graphene
Capsule.
Other Step By Condition parameters are same as Example 1.
Embodiment 11
Unlike the first embodiment, in the present embodiment the preparation method of carboxymethyl cellulose graphene microcapsules include with
Lower step：
S11. graphene is placed in ultrasonic disperse in pure water, the ratio of graphene and pure water is 0.1g:10ml obtains graphite
Alkene dispersion liquid；
S12. wall material is made into the solution that mass fraction is 30wt%, gained graphene dispersing solution is added, be 45 in temperature
DEG C, pressure be 1MPa nitrogen atmosphere under, stir 30min, mixing speed 800r/min.
S13. after stirring terminates, solid product is collected in filtering, is freeze-dried micro- to get carboxymethyl cellulose graphene
Capsule.
Other Step By Condition parameters are same as Example 1.
Comparative example 5
Unlike the first embodiment, in the present embodiment the preparation method of carboxymethyl cellulose graphene microcapsules include with
Lower step：
S11. graphene is placed in ultrasonic disperse in pure water, the ratio of graphene and pure water is 0.1g:10ml obtains graphite
Alkene dispersion liquid；
S12. wall material is made into the solution that mass fraction is 30wt%, gained graphene dispersing solution is added, be 35 in temperature
DEG C, pressure be normal pressure nitrogen atmosphere under, stir 30min, mixing speed 800r/min.
S13. after stirring terminates, solid product is collected in filtering, is freeze-dried micro- to get carboxymethyl cellulose graphene
Capsule.
Other conditional parameters are same as Example 1.
Comparative example 6
Unlike the first embodiment, in the present embodiment the preparation method of carboxymethyl cellulose graphene microcapsules include with
Lower step：
S11. graphene is placed in ultrasonic disperse in pure water, the ratio of graphene and pure water is 0.1g:10ml obtains graphite
Alkene dispersion liquid；
S12. wall material is made into the solution that mass fraction is 30wt%, gained graphene dispersing solution is added, be 35 in temperature
DEG C, pressure be 3MPa nitrogen atmosphere under, stir 30min, mixing speed 800r/min.
S13. after stirring terminates, solid product is collected in filtering, is freeze-dried micro- to get carboxymethyl cellulose graphene
Capsule.
Other Step By Condition parameters are same as Example 1.
Test
Water purification performance survey is carried out using carboxymethyl cellulose graphene flocculant aid obtained by the various embodiments described above and comparative example
Examination, condition are as follows：Take identical outdoor elements polluted-water water sample (abbreviation raw water, the turbidity of raw water is 820NTU after tested,
Turbidity tests foundation《The measurement of GB 13200-1991 water turbidity》), flocculant and the flocculation of carboxymethyl cellulose graphene are helped
Certain usage ratio is pressed in agent, adds in the water sample of isometric raw water (stirring 5min), is calculated when the turbidity of water sample is down to
The dosage of required flocculant when 1NTU, and record static balance time (stopping the used time after stirring to settlement stability).
Flocculant chooses polyacrylamide, and flocculant and carboxymethyl cellulose graphene flocculant aid are 9 in mass ratio:1
Ratio add in the water sample of isometric raw water.In addition, using be added without carboxymethyl cellulose graphene flocculant aid as pair
As usual.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
Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention
Protection scope within.
Claims (7)
1. a kind of carboxymethyl cellulose graphene flocculant aid, which is characterized in that including following component in parts by weight：
70 ~ 90 parts of carboxymethyl cellulose graphene microcapsules, 10 ~ 30 parts of dispersing agent；The carboxymethyl cellulose graphene microcapsules
The mass ratio of wall material including core material and the package core material, the wall material and core material is 0.5:1~2:1；The core material is graphite
Alkene, the wall material are carboxymethyl cellulose.
2. carboxymethyl cellulose graphene flocculant aid according to claim 1, which is characterized in that including it is following by weight
The component that number calculates：82 parts of carboxymethyl cellulose graphene microcapsules, 18 parts of dispersing agent.
3. carboxymethyl cellulose graphene flocculant aid according to claim 1, which is characterized in that the wall material and core material
Mass ratio be 1:1.
4. carboxymethyl cellulose graphene flocculant aid according to claim 1 or 2, which is characterized in that the dispersing agent
For one or more of polyvinyl alcohol, polyethylene, Sodium Polyacrylate.
5. carboxymethyl cellulose graphene flocculant aid according to claim 4, which is characterized in that the dispersing agent is poly-
The mixture of vinyl alcohol and Sodium Polyacrylate；The mass ratio of the polyvinyl alcohol and Sodium Polyacrylate is 1:1.
6. carboxymethyl cellulose graphene flocculant aid according to claim 1, which is characterized in that the carboxymethyl cellulose
The preparation method of plain graphene microcapsules includes the following steps：
S1. graphene is placed in ultrasonic disperse in pure water, obtains graphene dispersing solution；
S2. wall material is added to the graphene dispersing solution, in the inert atmosphere that temperature is 30 ~ 45 DEG C, pressure is 0.5 ~ 2MPa
Under, 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 carboxymethyl cellulose graphene microcapsules.
7. the preparation method of any one of the claim 1 ~ 6 carboxymethyl cellulose graphene flocculant aid, which is characterized in that packet
Include following steps：
S1. carboxymethyl cellulose graphene microcapsules are prepared；
S2. carboxymethyl cellulose graphene microcapsules are mixed with dispersing agent in proportion.
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Application publication date: 20181120 |