CN108726652A - A kind of methylcellulose graphene flocculant aid and preparation method thereof - Google Patents

A kind of methylcellulose graphene flocculant aid and preparation method thereof Download PDF

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Publication number
CN108726652A
CN108726652A CN201810562809.1A CN201810562809A CN108726652A CN 108726652 A CN108726652 A CN 108726652A CN 201810562809 A CN201810562809 A CN 201810562809A CN 108726652 A CN108726652 A CN 108726652A
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graphene
methylcellulose
microcapsules
flocculant
wall material
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CN201810562809.1A
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Chinese (zh)
Inventor
林前锋
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Hunan Guosheng Graphite Technology Co Ltd
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Hunan Guosheng Graphite Technology Co Ltd
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Priority to CN201810562809.1A priority Critical patent/CN108726652A/en
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56Macromolecular compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)

Abstract

The present invention provides a kind of methylcellulose graphene flocculant aids and preparation method thereof.The methylcellulose graphene flocculant aid includes following component in parts by weight:75 ~ 88 parts of methylcellulose graphene microcapsules, 12 ~ 25 parts of dispersant;The methylcellulose graphene 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 0.3:1~1:1;The core material is graphene, and the wall material is methylcellulose.Methylcellulose 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

A kind of methylcellulose graphene flocculant aid and preparation method thereof
Technical field
The present invention relates to the technical fields of water process water purification agent, wad a quilt with cotton more particularly, to a kind of methylcellulose graphene Solidifying auxiliary agent 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 to solve the problems, such as described in the above-mentioned prior art, provides a kind of methylcellulose graphene flocculant aid, The methylcellulose graphene flocculant aid can improve the purifying rate of unit flocculant while improving flocculation efficiency (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 flocculant aid.
In order to solve the above technical problems, the technical solution adopted by the present invention is:
A kind of methylcellulose graphene flocculant aid, including following component in parts by weight:Methylcellulose 75~88 parts of graphene microcapsules, 12~25 parts of dispersant;The methylcellulose graphene microcapsules include core material and package The mass ratio of the wall material of the core material, the wall material and core material is 0.3:1~1:1;The core material is graphene, and the wall material is 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 is chosen as conductive agent, and by graphite Alkene makes microcapsules, is combined together with dispersant, and in flocculation process, the methylcellulose graphene microcapsules can be rapid Dispersion, graphene during dispersion in methylcellulose graphene microcapsules can gradually be discharged, and be risen to flocculation process It is acted on to charge transfer, improves flocculated speed.Compared with existing conductive agent, due to herein described methylcellulose graphite Alkene microcapsules are gradually to discharge, and the charge of flocculant can just be uniformly dispersed together with graphene before being consumed totally, because This can improve flocculated speed and whole flocculating and purifying rate.
In order to reach said effect, the dispersion of graphene and release opportunity are crucial, in the present invention, it is preferred to water-soluble Wall material of the methylcellulose as coated graphite alkene, and pass through the ratio for designing wall material and core material so that Methyl cellulose flat band Graphene in black alkene microcapsules can effectively play a role in flocculation process.
In order to enable methylcellulose graphene microcapsules efficiently and effectively to disperse, methylcellulose graphite of the present invention Alkene flocculant aid also includes dispersant, and studies the proportioning for obtaining methylcellulose graphene microcapsules and dispersant.Preferably, The methylcellulose graphene flocculant aid includes following component in parts by weight:The micro- glue of methylcellulose graphene 80 parts of capsule, 20 parts of dispersant.
Preferably, the dispersant is one or more of polyvinyl alcohol, polyethylene, Sodium Polyacrylate.
It is highly preferred that the dispersant is the mixture of polyvinyl alcohol and polyethylene;The polyvinyl alcohol and polyethylene Mass ratio is 1:1.
The release opportunity of graphene is the key that the present 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 0.3 by research:1~1:1.Preferably, the wall material Mass ratio with core material is 0.6:1.
Preferably, the preparation method of the methylcellulose 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 40~60 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 methylcellulose 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 grain 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 50 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, still stayed between wall material and graphene in methylcellulose graphene microcapsules Certain gap contacts convenient for the release of graphene and with flocculant.
The present invention also provides the preparation methods of the methylcellulose graphene flocculant aid.The preparation method include with Lower step:
S1. methylcellulose graphene microcapsules are prepared;
S2. methylcellulose graphene microcapsules are mixed with dispersant in proportion.
The present invention further provides the applications of the methylcellulose graphene flocculant aid.The methylcellulose graphite Alkene 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 flocculant aid is added to flocculant in sewage, is stirred, and is flocculated, sedimentation.The flocculant with The mass ratio of methylcellulose graphene flocculant aid is 8~10:1, preferably 9:1.
The methylcellulose graphene flocculant aid can be efficiently applied to existing flocculant system, further, The flocculant includes but not limited to aluminum sulfate, polyoxygenated aluminium, iron chloride and ferrous sulfate, polyacrylamide.Preferably, described 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 and is done as conductive agent, and by graphene It at microcapsules, is combined together with dispersant, in flocculation process, the methylcellulose graphene microcapsules can divide rapidly It dissipates, graphene during dispersion in methylcellulose graphene microcapsules can gradually be discharged, and be played to flocculation process Charge transfer acts on, and improves flocculated speed, while can also improve the purifying rate (removal rate) of unit flocculant, 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 is given birth to for Hunan Guo Sheng graphite Science and Technology Ltd. Production, grain 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 methylcellulose graphene flocculant aid includes methylcellulose graphene microcapsules and dispersant.Methyl is fine The plain graphene microcapsules of dimension include core material and wall material, and core material is graphene, and wall material is methylcellulose.
In each embodiment and comparative example, the dosage (A) of methylcellulose graphene microcapsules, the dosage (B) of dispersant, The design parameters such as the mass ratio (D) of the type (C) of dispersant, wall material and core material are as shown in table 1.
The preparation method of methylcellulose graphene flocculant aid includes the following steps:
S1. methylcellulose 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 50 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 to get the micro- glue of methylcellulose graphene Capsule.
S2. methylcellulose graphene 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 microcapsules includes following in the present embodiment 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 50 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 to get the micro- glue of methylcellulose graphene Capsule.
Other Step By Condition parameters are same as Example 1.
Embodiment 9
As different from Example 1, the preparation method of methylcellulose graphene microcapsules includes following in the present embodiment 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 50 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 to get the micro- glue of methylcellulose graphene Capsule.
Other Step By Condition parameters are same as Example 1.
Embodiment 10
As different from Example 1, the preparation method of methylcellulose graphene microcapsules includes following in the present embodiment 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 40 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 to get the micro- glue of methylcellulose graphene Capsule.
Other Step By Condition parameters are same as Example 1.
Embodiment 11
As different from Example 1, the preparation method of methylcellulose graphene microcapsules includes following in the present embodiment 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 60 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 to get the micro- glue of methylcellulose graphene Capsule.
Other Step By Condition parameters are same as Example 1.
Comparative example 5
As different from Example 1, the preparation method of methylcellulose graphene microcapsules includes following in the present embodiment 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 50 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 to get the micro- glue of methylcellulose graphene Capsule.
Other conditional parameters are same as Example 1.
Comparative example 6
As different from Example 1, the preparation method of methylcellulose graphene microcapsules includes following in the present embodiment 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 50 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 to get the micro- glue of methylcellulose graphene Capsule.
Other Step By Condition parameters are same as Example 1.
Test
Water purification performance test is carried out using methylcellulose graphene flocculant aid obtained by the various embodiments described above and comparative example, Condition is as follows:Taking identical outdoor elements polluted-water water sample, (abbreviation raw water, the turbidity of raw water is 820NTU after tested, turbid Degree test foundation《The measurement of GB 13200-1991 water turbidities》), flocculant and methylcellulose graphene flocculant aid are pressed Certain usage ratio adds in the water sample of isometric raw water (stirring 5min), calculates when the turbidity of water sample is down to 1NTU The dosage of required flocculant, and record static balance time (stopping the used time to settlement stability after stirring).
Flocculant chooses polyacrylamide, and flocculant is 9 in mass ratio with methylcellulose graphene flocculant aid:1 Ratio adds in the water sample of isometric raw water.In addition, to be added without methylcellulose graphene flocculant aid example as a contrast. 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 flocculant aid, which is characterized in that including following component in parts by weight:First 75 ~ 88 parts of base cellulose graphene microcapsules, 12 ~ 25 parts of dispersant;The methylcellulose graphene microcapsules include core The mass ratio of material and the wall material for wrapping up the core material, the wall material and core material is 0.3:1~1:1;The core material is graphene, institute It is methylcellulose to state wall material.
2. methylcellulose graphene flocculant aid according to claim 1, which is characterized in that including it is following by weight The component that number calculates:80 parts of methylcellulose graphene microcapsules, 20 parts of dispersant.
3. methylcellulose graphene flocculant aid according to claim 1, which is characterized in that the wall material and core material Mass ratio is 0.6:1.
4. methylcellulose graphene flocculant aid according to claim 1 or 2, which is characterized in that the dispersant is One or more of polyvinyl alcohol, polyethylene, Sodium Polyacrylate.
5. methylcellulose graphene flocculant aid according to claim 4, which is characterized in that the dispersant is poly- second The mixture of enol and polyethylene;The mass ratio of the polyvinyl alcohol and polyethylene is 1:1.
6. methylcellulose graphene flocculant aid according to claim 1, which is characterized in that the Methyl cellulose flat band The preparation method of black alkene 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 40 ~ 60 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 methylcellulose graphene microcapsules.
7. the preparation method of any one of the claim 1 ~ 6 methylcellulose graphene flocculant aid, which is characterized in that including Following steps:
S1. methylcellulose graphene microcapsules are prepared;
S2. methylcellulose graphene microcapsules are mixed with dispersant in proportion.
CN201810562809.1A 2018-06-01 2018-06-01 A kind of methylcellulose graphene flocculant aid and preparation method thereof Pending CN108726652A (en)

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CN202539509U (en) * 2011-12-15 2012-11-21 北京利尔高温材料股份有限公司 Oriented-argon blowing purging upper nozzle of continuous casting tundish
CN103330213A (en) * 2013-05-10 2013-10-02 杭州普丽美地生物科技有限公司 Tea polyphenol liposoluble microcapsules and preparation method thereof
CN105384943A (en) * 2015-11-05 2016-03-09 江苏大学 Preparation method and application of beta-cyclodextrin-cellulose-graphene oxide composite material
CN105747216A (en) * 2016-03-03 2016-07-13 广州市食品工业研究所有限公司 Microcapsules-beta and carotene powder and preparation method thereof
CN106566303A (en) * 2016-10-21 2017-04-19 成都新柯力化工科技有限公司 Graphene micro-sheet used for waterborne anticorrosive coating and preparation method thereof
CN107938365A (en) * 2017-11-30 2018-04-20 英泰时尚服饰(苏州)有限公司 A kind of uvioresistant microcapsule dressing agent and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN202539509U (en) * 2011-12-15 2012-11-21 北京利尔高温材料股份有限公司 Oriented-argon blowing purging upper nozzle of continuous casting tundish
CN103330213A (en) * 2013-05-10 2013-10-02 杭州普丽美地生物科技有限公司 Tea polyphenol liposoluble microcapsules and preparation method thereof
CN105384943A (en) * 2015-11-05 2016-03-09 江苏大学 Preparation method and application of beta-cyclodextrin-cellulose-graphene oxide composite material
CN105747216A (en) * 2016-03-03 2016-07-13 广州市食品工业研究所有限公司 Microcapsules-beta and carotene powder and preparation method thereof
CN106566303A (en) * 2016-10-21 2017-04-19 成都新柯力化工科技有限公司 Graphene micro-sheet used for waterborne anticorrosive coating and preparation method thereof
CN107938365A (en) * 2017-11-30 2018-04-20 英泰时尚服饰(苏州)有限公司 A kind of uvioresistant microcapsule dressing agent and preparation method thereof

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Application publication date: 20181102