CN109502864A - A kind of processing method of graphene oxide waste liquid - Google Patents
A kind of processing method of graphene oxide waste liquid Download PDFInfo
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- CN109502864A CN109502864A CN201811492217.3A CN201811492217A CN109502864A CN 109502864 A CN109502864 A CN 109502864A CN 201811492217 A CN201811492217 A CN 201811492217A CN 109502864 A CN109502864 A CN 109502864A
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
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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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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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
-
- 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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F2001/007—Processes including a sedimentation step
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Agronomy & Crop Science (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The present invention provides a kind of processing methods of graphene oxide waste liquid.The graphene oxide waste liquid includes NO3 ‑And Cl‑At least one of and K+、Mn2+、Fe3+And SO4 2‑, the treating method comprises following steps: will include K2CO3Activated Carbon Production waste liquid mixed with graphene oxide waste liquid, to precipitate the Mn in graphene oxide waste liquid2+And Fe3+And obtain the first intermediate solution；The SO in the first intermediate solution is removed by precipitating reagent4 2‑Or SO4 2‑And CO3 2‑, and obtaining includes KNO3And/or the second intermediate solution of KCl, the precipitating reagent include anion N O3 ‑And/or Cl‑；Second intermediate solution is separated into KNO3And/or KCl and water body.The beneficial effect comprise that the Fe in graphene oxide waste liquid can be removed efficiently3+、Mn2+Etc. heavy metal ion and SO4 2‑And CO3 2‑, while KNO can have been recycled3And KCl；Can the treatment of wastes with processes of wastes against one another saved cost, and method is easy.
Description
Technical field
The present invention relates to the processing of waste liquid in industrial processes, particularly, are related to a kind of place of graphene oxide waste liquid
Reason method.
Background technique
Inorganic acid and inorganic salts etc. can be generated in graphene oxide production process, be not available biochemical method to its into
Row processing.Chemical reagent higher cost used in various ions is currently removed, while also needing through a series of UF membranes and being
Insoluble impurities in system processing waste water.In order to reduce the waste liquid generated in graphene oxide production process as far as possible to environment
Harm, while mitigating operation cost of enterprises, it is very urgent to seek a kind of efficient and inexpensive method for treating waste liquid.
Summary of the invention
For the deficiencies in the prior art, it is an object of the invention to solve above-mentioned one existing in the prior art
Or multiple problems.For example, one of the objects of the present invention is to provide a kind of processing methods of graphene oxide waste liquid, with effectively
Remove the foreign ion in waste liquid.
To achieve the goals above, the present invention provides a kind of processing methods of graphene oxide waste liquid.The oxidation stone
Black alkene waste liquid may include NO3 -And Cl-At least one of and K+、Mn2+、Fe3+And SO4 2-, the processing method may include with
Lower step: will include K2CO3Activated Carbon Production waste liquid mixed with graphene oxide waste liquid, to precipitate graphene oxide waste liquid
In Mn2+And Fe3+And obtain the first intermediate solution；The SO in the first intermediate solution is removed by precipitating reagent4 2-And when described
Existing CO when active carbon waste liquid excess3 2-, and obtaining includes KNO3And/or the second intermediate solution of KCl, the precipitating
Agent includes anion N O3 -And/or Cl-；Second intermediate solution is separated into KNO3And/or KCl and water body.
According to the present invention based on one or more embodiments, the method may further comprise the step of: it is described will be in second
Between solution separation before, second intermediate solution is purified.
According to the present invention based on one or more embodiments, include KNO in the highly concentrated solution3With KCl's
In the case of, described the step of separating the second intermediate solution can include: second intermediate solution is concentrated, is obtained highly concentrated
The KNO of degree3With KCl solution and water body；The solute in the highly concentrated solution is precipitated, to obtain KNO3And KCl.
According to the present invention based on one or more embodiments, it is described to make highly concentrated solution (the i.e. KNO of high concentration3And KCl
Solution) in solute be precipitated the step of can include: KNO is made by the method for recrystallization3, KCl separates from solution.
According to the present invention based on one or more embodiments, include KNO in the highly concentrated solution3With KCl's
In the case of, it is described to make the step of solute is precipitated in highly concentrated solution can include: according to KNO3With KCl solubility and temperature in water
Relationship, make KNO3It is precipitated from solution at different temperature with KCl, and then obtains KNO respectively3And KCl.
According to the present invention based on one or more embodiments, include KNO in the highly concentrated solution3Or KCl
In the case of, described the step of separating the second intermediate solution includes: the KNO made in the second intermediate solution by evaporating3Or KCl
It is separated with water body.
According to the present invention based on one or more embodiments, the precipitating reagent includes CaCl2Solution and Ca (NO3)2Solution
At least one of.
According to the present invention based on one or more embodiments, Mn in the graphene oxide solution2+Concentration can be
0.01~2mol/L, Fe3+Concentration can be 10-5~10-7Mol/L, SO4 2-Concentration can be 0.01~2mol/L, NO3 -Concentration
It can be 0~1mol/L, Cl-Concentration can be 0~0.1mol/L.
According to the present invention based on one or more embodiments, the graphene oxide waste liquid may include oxidation intercalation legal system
The waste liquid generated in standby graphene oxide production process.
According to the present invention based on one or more embodiments, the pH of the Activated Carbon Production waste liquid can be 10~14, institute
State CO in active carbon waste liquid3 2-Concentration can be 0.01~1mol/L.
According to the present invention based on one or more embodiments, the Activated Carbon Production waste liquid includes activation of potassium hydroxide method
The waste liquid generated when producing active carbon.
Compared with prior art, the present invention can efficiently remove the Fe in graphene oxide waste liquid3+、Mn2+Equal heavy metals from
Son and SO4 2-And CO3 2-, while KNO can have been recycled3And KCl；Can the treatment of wastes with processes of wastes against one another saved cost, and method letter
Just.
Detailed description of the invention
By the description carried out with reference to the accompanying drawing, above and other purpose of the invention and feature will become more clear
Chu, in which:
Fig. 1 shows the flow diagram of graphene oxide method for treating waste liquid in an illustrative embodiment of the invention.
Fig. 2 shows the process signals of graphene oxide method for treating waste liquid in another exemplary embodiment of the invention
Figure.
Specific embodiment
Hereinafter, the place of graphene oxide waste liquid of the invention will be described in detail in conjunction with attached drawing and exemplary embodiment
Reason method.
The waste water discharged in graphene oxide industrial production especially prepares graphene oxide discharge in oxidation graft process
Waste water, which includes nitrate ion (NO3 -) and chloride ion (Cl-) at least one of and manganese ion (Mn2+), iron from
Son (Fe3+), sulfate ion (SO4 2-) and potassium ion (K+) etc., it is therefore desirable to waste liquid is handled, is not intended to deposit to remove
Element and recycling, and processed waste water is made to reach industrial wastewater discharge standard.
In an exemplary embodiment of the present invention, as shown in Figure 1, the processing method of shown graphene oxide waste liquid can
The following steps are included:
It will include K2CO3Activated Carbon Production waste liquid mixed with graphene oxide waste liquid, to precipitate graphene oxide waste liquid
In Mn2+And Fe3+And obtain the first intermediate solution, step S01 as shown in figure 1.Wherein, active carbon waste liquid and graphene oxide
After waste liquid mixing, CO3 2-With Mn2+In conjunction with generation MnCO3Precipitating, CO3 2-Also with H2O、Fe3+Reaction production Fe (OH)3Precipitating removes
It may include having NO in obtained the first intermediate solution after precipitating (such as filtering)3 -And Cl-At least one of and K+、
SO4 2-, or even in Activated Carbon Production waste liquid excess, the first intermediate solution also may include having CO3 2-；The pH of first intermediate solution can
It is 9~12, further can is 11 ± 0.5, can make solution that basic character be presented, in this way to ensure Fe3+It is completely removed.Institute
State Mn in graphene oxide waste liquid2+Concentration can be 0.01~2mol/L, Fe3+Concentration can be 10-5~10-7Mol/L, SO4 2-
Concentration can be 0.01~2mol/L, Cl-Concentration can be 0~0.1mol/L, NO3 -Concentration can be 0~1mol/L.The work
Property charcoal production waste liquid pH can be 10~14, K in the active carbon waste liquid2CO3Concentration can be 0.01~1mol/L.If active
Charcoal waste liquid direct emission, since alkalinity is presented in it and contains K2CO3, can cause environmental pollution.The Activated Carbon Production waste liquid
The waste liquid generated when may include activation of potassium hydroxide active carbon.
Contain SO in the first intermediate solution4 2-In the case of, precipitating removal SO4 2-, contain SO in the first intermediate solution4 2-
And CO3 2-In the case where, precipitating removal SO4 2-And CO3 2-, then obtaining includes KNO3And/or the second intermediate solution of KCl；Such as
Step S02 in Fig. 1.Wherein, the SO in the first intermediate solution can be removed by solution for precipitating or substance4 2-Or
SO4 2-And CO3 2-.The anion of the solution or substance includes NO3 -And Cl-At least one of, cation includes can be with SO4 2-
And CO3 2-It is combined into the cation of precipitating, such as the substance can be CaCl2With Ca (NO3)2At least one of or the solution
It can be CaCl2With Ca (NO3)2At least one of solution.
Second intermediate solution is separated into KNO3And/or KCl and water body, step S03 as shown in figure 1, it can obtain
Two substances, one kind are KNO3And/or KCl, another kind of is water body.Wherein, the water body obtained is to meet industrial discharge standard
Waste water.It include KNO in the highly concentrated solution3In the case where KCl, described the step of separating the second intermediate solution, can
Include: that second intermediate solution is concentrated, obtains the KNO of high concentration3With KCl solution and water body, such as can pass through
Reverse osmosis or evaporation is to handle；The solute in the highly concentrated solution is precipitated, to obtain KNO3And KCl, such as weight can be passed through
Crystallization is to handle.It include KNO in the highly concentrated solution3Or in the case where KCl, it is described by the second intermediate solution separation
Step includes: the KNO made in the second intermediate solution by evaporating3Or KCl is separated with water body.
In the present embodiment, the method may further comprise the step of: before by second intermediate solution separation, to described
Second intermediate solution is purified, and removes the sulfate and carbonate deposition that generate with further.Wherein, purification can pass through activity
Charcoal adsorbs to carry out.
In the present embodiment, graphene oxide waste liquid may include that oxidation graft process is prepared and produced in graphene oxide production process
Raw waste liquid is also adapted to other waste liquids for producing graphene oxides, for example, by using other Hummers methods or improved
Hummers method prepares the waste liquid generated when graphene oxide, and other Hummers methods or improved Hummers method generate waste liquid
All contain Mn2+、Fe3+、SO4 2-、K+、NO3 -And Cl—Deng.
It in the present embodiment, include NO in graphene oxide waste liquid3 -、K+、Mn2+、Fe3+And SO4 2-In the case where, it obtains
It include NO in the first intermediate solution obtained3 -And K+、SO4 2-, in active carbon waste liquid excess, the first intermediate solution can also be wrapped
Contain CO3 2-；Ca (NO can be used in precipitating reagent3)2Or Ca (NO3)2Solution, then the second intermediate solution includes KNO3；Pass through active carbon
Second intermediate solution is purified, then isolates KNO from purified second intermediate solution3And water body.
It include Cl in graphene oxide waste liquid-、K+、Mn2+、Fe3+And SO4 2-In the case where, the first centre of acquisition is molten
It include Cl in liquid-And K+、SO4 2-, in active carbon waste liquid excess, the first intermediate solution also may include having CO3 2-；Precipitating reagent
CaCl can be used2Or CaCl2Solution, then the second intermediate solution includes KCl；The second intermediate solution is carried out by active carbon net
Change, then isolates KCl and water body from purified second intermediate solution.
It include NO in graphene oxide waste liquid3 -、Cl-、K+、Mn2+、Fe3+And SO4 2-In the case where, acquisition first in
Between include NO in solution3 -、Cl-And K+、SO4 2-, in active carbon waste liquid excess, the first intermediate solution also may include having
CO3 2-；Ca (NO can be used in precipitating reagent3)2And CaCl2At least one of, then the second intermediate solution includes KNO3And KCl；It is logical
It crosses active carbon to purify the second intermediate solution, then purified second intermediate solution is concentrated, obtains high concentration
Contain KNO3With the solution of KCl and meet the water body of discharge standard；Highly concentrated solution is recrystallized at different temperature,
Respectively obtain KNO3And KCl.
In another exemplary embodiment of the invention, graphene oxide method for treating waste liquid can include: first with
The industrial wastes (in alkalinity) of Activated Carbon Production adjusts pH value, precipitating iron ion and the manganese ion of filtrate, and precipitating reagent is then added
Calcium chloride (CaCl2), remove CO3 2-And SO4 2-Ion finally removes potassium ion, chloride ion and nitrate anion using reverse osmosis unit
Ion.Wherein,
(1) waste liquid in Activated Carbon Production workshop is mainly potassium carbonate (K2CO3), the waste liquid of graphene oxide is adjusted using it,
To pH to 9~12, iron ion and manganese ion are precipitated completely；
(2) appropriate calcium chloride is added, removes CO3 2-And SO4 2-；
(3) filtering precipitated；
(4) it is further purified water by active carbon；
(5) reverse osmosis unit concentration obtains KNO3With KCl solution；
(6) KNO is isolated using the method for recrystallization3And KCl.
The above exemplary embodiments for a better understanding of the present invention carry out further it below with reference to specific example
Explanation.
Proper amount of active carbon waste liquid is first added in graphene oxide waste water, adjusting pH value is 10, completely precipitating Fe3+(Fe
(OH)3Precipitation form removes) and Mn2+(MnCO3Precipitation form removes), then add suitable CaCl2Solution removes SO4 2-
(CaSO4Precipitation form removes) and CO3 2-(CaCO3Precipitation form removes)；After precipitating filtering, then filtrate is made to pass through activated carbon adsorption
Pond；Then waste liquid is made to reach the discharge standard of industrial wastewater by reverse osmosis pond again；The KCl and KNO being finally enriched with3Solution is logical
The method for crossing recrystallization is recycled.
In further exemplary embodiment of the invention, graphene oxide waste liquid includes nitrate ion (NO3 -), manganese from
Son (Mn2+), iron ion (Fe3+), chloride ion (Cl-), sulfate ion (SO4 2-) and potassium ion (K+).Graphene oxide waste liquid
Processing method can comprise the following steps that
Graphene oxide waste liquid and active carbon waste liquid are added in pH value conditioning tank, pH value of solution is adjusted, by adjusting pH
Value, efficiently eliminates Fe3+, Mn2+Etc. heavy metal ion, then obtain the first intermediate solution.
By the first intermediate solution and precipitating reagent (such as CaCl2) be added to and sink to the bottom in pond, utilize the method that precipitating reagent is added
So that SO4 2-And CO3 2-Precipitating is generated, the second intermediate solution is obtained.
Second intermediate solution is placed in activated carbon adsorption tank, to purify the second intermediate solution.
Purified second intermediate solution is placed in reverse osmosis pond, is concentrated using reverse osmosis unit and obtains high concentration
KNO3With KCl solution, and meet the waste water of industrial discharge standard, and obtained waste water is placed in industrial standard discharge of wastewater pond
In.
To the KNO of high concentration3Recrystallization is carried out with KCl solution to separate, and respectively obtains KNO3And KCl.
In conclusion the advantages of graphene oxide producing wastewater treatment of the invention, has: (1) utilizing active carbon workshop
Waste liquid, by adjust pH value, efficiently eliminate Fe3+, Mn2+Etc. heavy metal ion；(2) high using the method that precipitating reagent is added
Effect eliminates SO4 2-And CO3 2-, while KNO has been recycled using recrystallization3And KCl；(3) treatment of wastes with processes of wastes against one another is (raw using active carbon
The industrial wastes of production), cost is saved, and method is easy, it is easily operated.
Although those skilled in the art should be clear above by combining exemplary embodiment to describe the present invention
Chu can carry out exemplary embodiment of the present invention each without departing from the spirit and scope defined by the claims
Kind modifications and changes.
Claims (10)
1. a kind of processing method of graphene oxide waste liquid, which is characterized in that graphene oxide waste liquid includes NO3 -And Cl-In
At least one and K+、Mn2+、Fe3+And SO4 2-, it the treating method comprises following steps:
It will include K2CO3Activated Carbon Production waste liquid mixed with graphene oxide waste liquid, to precipitate in graphene oxide waste liquid
Mn2+And Fe3+And obtain the first intermediate solution；
The SO in the first intermediate solution is removed by precipitating reagent4 2-And it is existing when the active carbon waste liquid excess
CO3 2-, and obtaining includes KNO3And/or the second intermediate solution of KCl, the precipitating reagent include anion N O3 -And/or Cl-；
Second intermediate solution is separated into KNO3And/or KCl and water body.
2. graphene oxide method for treating waste liquid according to claim 1, which is characterized in that the method also includes steps
It is rapid: before by second intermediate solution separation, second intermediate solution being purified.
3. graphene oxide method for treating waste liquid according to claim 1, which is characterized in that described by the second intermediate solution
The step of being separated include:
Second intermediate solution is concentrated, the KNO of high concentration is obtained3And/or KCl solution and water body；
The solute in the highly concentrated solution is precipitated, to obtain KNO3And/or KCl.
4. graphene oxide method for treating waste liquid according to claim 3, which is characterized in that described to make in highly concentrated solution
Solute be precipitated the step of include:
It include KNO in the highly concentrated solution3Or in the case where KCl, described the step of separating the second intermediate solution, is wrapped
It includes: making the KNO in the second intermediate solution by evaporating3Or KCl is separated with water body.
5. graphene oxide method for treating waste liquid according to claim 3, which is characterized in that in the highly concentrated solution
It include KNO3It is described that the step of solute is precipitated in highly concentrated solution is made to include: according to KNO in the case where KCl3With KCl in water
In solubility and temperature relationship, make KNO3It is precipitated from solution at different temperature with KCl, and then obtains KNO respectively3
And KCl.
6. graphene oxide method for treating waste liquid according to claim 1, which is characterized in that the precipitating reagent includes CaCl2
Solution and Ca (NO3)2At least one of solution.
7. graphene oxide method for treating waste liquid according to claim 1, which is characterized in that the graphene oxide waste liquid
Middle Mn2+Concentration be 0.01~2mol/L, Fe3+Concentration be 10-5~10-7Mol/L, SO4 2-Concentration be 0.01~2mol/L,
NO3 -Concentration be 0~1mol/L, Cl-Concentration be 0~0.1mol/L.
8. graphene oxide method for treating waste liquid according to claim 1, which is characterized in that the graphene oxide waste liquid
The waste liquid generated in graphene oxide production process is prepared including oxidation graft process.
9. graphene oxide method for treating waste liquid according to claim 1, which is characterized in that the Activated Carbon Production waste liquid
PH be 10~14, CO in the active carbon waste liquid3 2-Concentration be 0.01~1mol/L.
10. graphene oxide method for treating waste liquid according to claim 1, which is characterized in that the Activated Carbon Production is useless
The waste liquid that liquid generates when including activation of potassium hydroxide method production active carbon.
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| DE102012216828A1 (en) * | 2012-09-19 | 2014-03-20 | Sgl Carbon Se | Producing modified graphene oxide useful in a composite material used as e.g. electrical insulation material for electrical and combustion components in e.g. computer, comprises mixing graphene oxide and surfactant |
| CN103382028A (en) * | 2013-08-17 | 2013-11-06 | 青岛中科昊泰新材料科技有限公司 | Preparation of graphene oxide and post-processing method for waste liquor |
| CN105923628A (en) * | 2016-06-13 | 2016-09-07 | 南京工业大学 | Wastewater treatment method in graphene preparation process |
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