CN110066004A - Improve the preparation method and application of the solid oxidizer of permanganate stability and oxidisability - Google Patents
Improve the preparation method and application of the solid oxidizer of permanganate stability and oxidisability Download PDFInfo
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
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Abstract
The invention discloses the preparation method and applications of a kind of raising permanganate stability and the solid oxidizer of oxidisability, and the mixed solution of divalent metal salt and trivalent metal salt is prepared by certain proportion；Mixed solution is added in aqueous slkali, keeps pH value in particular range and to be stirred, emulsion is obtained after standing；Liquor potassic permanganate is added to again after being stirred in emulsion and obtains subsequent emulsion, obtains the permanganate solid oxidizer product with layer structure after centrifugation, cleaning, drying.Solid product of the present invention is put into organic wastewater, stirring is reacted, and under the conditions of same, solid product shows oxidation efficiency more better than permanganate, and the product after reaction is still absorbed by its own, without secondary pollution.The method of the present invention is applied to the bisphenol-A waste water that processing is 4~12 containing pH, has higher removal efficiency, without secondary pollution, process costs are low, and water treatment efficiency is good.
Description
Technical field
The present invention relates to a kind of water treatment agent preparation method and applications, more particularly to a kind of based on permanganate
Solid oxidizer material preparation method and its application are applied to technical field for the treatment of of organic waste.
Background technique
The waste water handling problem of organic pollution has been a hot spot of research, and potassium permanganate is with cheap, source is wide
General, easy storage does not generate the advantages that poisonous and hazardous oxidized byproduct, and can control microorganism in the growth and water of algae
Breeding, be common green medicament in water treatment procedure.
As the potassium permanganate of conventional oxidation agent, although strong oxidizer, compared with hydroxyl radical free radical, to organic matter
Oxidability it is weak, it is therefore desirable to improve the oxidation susceptibility of potassium permanganate.Potassium permanganate can pass through transition metal ions, complexing
The activation of the medicaments such as agent, manganese dioxide, but be all restricted in actual application process, such as transition metal ions Ru (III) price
It is difficult to recycle after expensive, Fe (II) and Fe (III) use；For the oxidisability for significantly improving potassium permanganate, complexing agent will increase
Usage amount, but the excess of complexing agent adds and can cause secondary pollution to water body；Manganese dioxide is only in slightly acidic water environment
Catalysis or oxidation can just be shown.Meanwhile the efficiency of potassium permanganate oxidation organic matter depends primarily on the structure of organic matter
With property, and to different oxidation operations when is affected by pH value, and the process of potassium permanganate oxidation organic matter is to natural oxygen
The requirement for changing environment is high, needs to improve oxidisability and the stability of potassium permanganate to be applicable in the water body environment of different pH value, this is limited
Application of the potassium permanganate in water process has been made, technical problem urgently to be resolved is become.
Summary of the invention
In order to solve prior art problem, it is an object of the present invention to overcome the deficiencies of the prior art, and to provide one kind
The preparation method and application for improving the solid oxidizer of permanganate stability and oxidisability, the height prepared using the method for the present invention
The oxidisability and stability of manganate solid material oxidant potassium permanganate obtain harness and improve, and can be applicable in the water body of different pH value
The water treatment procedure of environment carries out fast degradation to different pH value Organic Pollutants In Waters, improves the efficiency of water process, reduces
The cost of water process.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of preparation method for the solid oxidizer improving permanganate stability and oxidisability, includes the following steps:
A. a certain amount of divalent metal salt, trivalent metal salt, potassium permanganate and suitable water soluble alkali are weighed, it is spare；Institute
The molar ratio for stating divalent metal salt and trivalent metal salt is 2:1~3:1, and potassium permanganate and trivalent metal salt molar ratio are 1:1；Institute
It states divalent metal salt and preferably uses at least one of villaumite and nitrate of magnesium；Trivalent metal salt preferably use aluminium villaumite and
At least one of nitrate, the villaumite of iron and nitrate；Water soluble alkali preferably use sodium hydroxide, in potassium hydroxide at least
It is a kind of；
B. the divalent metal salt and trivalent metal salt in the step a are utilized, divalent metal salt and trivalent metal are prepared
The mixing salt solution of salt；Using the water soluble alkali in the step a, alkali liquid medicine is prepared；The mixing salt solution is added
Enter and be stirred mixing into the alkali liquid medicine, and maintains the mixing salt solution pH value of alkalinity in 9~12 ranges, and
Stir at room temperature and stand 16 after at least 2h~for 24 hours, obtain the first emulsion；
C. the first cream prepared in the step b will be added to after potassium permanganate weighed in step a dissolution
In turbid, is continuously stirred at least for 24 hours under conditions of being not higher than 70 DEG C, obtain the second emulsion；
D. the second emulsion prepared in the step c is centrifuged, washed, collect solid content, and be not higher than
Solid content is dried at 70 DEG C, to obtain permanganate solid material oxidant.It is preferred that prepared permanganate is solid
Body material oxidation agent has laminated metal compound structure, forms the value Mn composite material based on sexavalence manganese and septivalency manganese.
A kind of preparation method preparation for the solid oxidizer improving permanganate stability and oxidisability using the present invention
The application of permanganate solid material oxidant, for implement degrade organic pollutants method during, by the height
Manganate solid material oxidant is added in the waste water to be processed that pH value is 4~12, and according to permanganate solid material oxygen
The dosage that the quality of agent and the volume of waste water to be processed calculate is 0.5~1.0g/L ratio, carries out permanganate solid material
Expect that oxidant is launched, while waste water to be processed is stirred to react, makes the sexavalence manganese in permanganate solid material oxidant
It is reacted with septivalency manganese with useless Organic substance in water and is converted to manganese dioxide, and be attached to permanganate solid material oxidant surface.
As a kind of currently preferred technical solution, during the method for organic pollutants of degrading, when described
When the concentration of target contaminant bisphenol-A in waste water to be processed is 20~50mg/L or when being greater than 10mg/L, the processing time is not
Greater than 30min.
Work as institute during the method for organic pollutants of degrading as currently preferred another technical solution
When stating the concentration of the target contaminant bisphenol-A in waste water to be processed no more than 10mg/L, the processing time is not more than 5min.
The present invention compared with prior art, has following obvious prominent substantive distinguishing features and remarkable advantage:
1. the present invention is prepared for NEW TYPE OF COMPOSITE solid material, the stability and oxidation susceptibility of permanganate are improved, is solved
The problem of being affected when potassium permanganate of having determined degradation bisphenol-A by pH value；
2. the permanganate solid material oxidant of the method for the present invention preparation is higher than traditional medicine to the degradation effect of organic matter
Agent or common potassium permanganate, when the permanganate solid material oxidant prepared using the method for the present invention carries out wastewater degradation,
Reaction rate obviously increases compared with prior art, and the manganese dioxide generated after reacting is still inhaled by stratiform metallic compound
It receives and fixed, secondary pollution will not be generated to subsequent processing；
3. the method for the present invention uses common metal salt medicament, raw material is cheap and easily-available, and preparation process is simple, no higher to set
It is standby to require, can practical application it is strong.
Detailed description of the invention
Fig. 1 uses general for the potassium permanganate solid material oxidant and the prior art of the preparation of one method of the embodiment of the present invention
Logical potassium permanganate is under different ph values to the removal rate of bisphenol-A.
Fig. 2 is the permanganate solid material oxidant of one method of embodiment of the present invention preparation to various concentration bisphenol-A
Removal ability experimental results curve comparison figure.
Fig. 3 uses general for the potassium permanganate solid material oxidant and the prior art of the preparation of two method of the embodiment of the present invention
Logical potassium permanganate is under different ph values to the removal rate of bisphenol-A.
Fig. 4 is the permanganate solid material oxidant of two method of embodiment of the present invention preparation to various concentration bisphenol-A
Removal ability experimental results curve comparison figure.
Specific embodiment
Above scheme is described further below in conjunction with specific implementation example, the preferred embodiment of the present invention is described in detail such as
Under:
Embodiment one:
In the present embodiment, a kind of preparation method for the solid oxidizer improving permanganate stability and oxidisability, packet
Include following steps:
A. a certain amount of magnesium nitrate, aluminum nitrate, potassium permanganate and suitable water soluble alkali sodium hydroxide are weighed, it is spare；Nitre
The molar ratio of sour magnesium and aluminum nitrate is 3:1, and the molar ratio of potassium permanganate and aluminum nitrate is 1:1；
B. the magnesium nitrate and aluminum nitrate in the step a are utilized, the mixing salt solution of magnesium nitrate and aluminum nitrate is prepared；It adopts
Sodium hydroxide in the step a prepares the alkali liquid medicine that 100mL naoh concentration is 40g/L；By the mixing
Salting liquid is added in the alkali liquid medicine and is stirred mixing, and maintaining the mixing salt solution pH value of alkalinity is 10, and
It is stood for 24 hours after stirring 2h at room temperature, obtains the first emulsion；
C. it will be added to after the weighed equimolar potassium permanganate dissolution with aluminum nitrate in the step in the step a
In the first emulsion prepared in b, is continuously stirred for 24 hours under conditions of 70 DEG C, obtain the second emulsion；
D. the second emulsion prepared in the step c is centrifuged, washed, collect solid content, and at 70 DEG C
Solid content is dried, to obtain permanganate solid material oxidant.
The height of the preparation method preparation of the solid oxidizer of permanganate stability and oxidisability is improved using the present embodiment
The application of manganate solid material oxidant, for implement degrade organic pollutants method during, by the Gao Meng
Hydrochlorate solid material oxidant is added in the wastewater sample to be processed that pH value is 4~12, and according to permanganate solid material
The dosage that the quality of oxidant and the volume of waste water to be processed calculate is 1.0g/L ratio, carries out permanganate solid material oxygen
Agent is launched, while being stirred to react to waste water to be processed, and the sexavalence manganese and seven in permanganate solid material oxidant is made
Valence manganese is reacted with useless Organic substance in water is converted to manganese dioxide, and is attached to permanganate solid material oxidant surface.
Experimental test and analysis:
The Gao Meng of the preparation method preparation of the solid oxidizer of permanganate stability and oxidisability is improved to the present embodiment
Hydrochlorate solid material oxidant carries out XRD structural analysis, it is seen that prepared permanganate solid material oxidant has stratiform
Metallic compound structure forms the value Mn composite material based on sexavalence manganese and septivalency manganese, is improved using the present embodiment high
The permanganate solid material oxidant of the preparation method of mangaic acid salt-stable and the solid oxidizer of oxidisability preparation, for real
During the method for applying degradation organic pollutants, sexavalence manganese and septivalency manganese in permanganate solid material oxidant and useless
Organic substance in water reaction is converted to manganese dioxide, and is attached to permanganate solid material oxidant surface.It can be seen that the present embodiment
The stability of the permanganate solid material oxidant of method preparation is greatly improved, and the manganese dioxide generated after reaction is still
It is absorbed and is fixed by stratiform metallic compound, secondary pollution, the water process that can be significantly improved will not be generated to subsequent processing
The rate of recovery of agent.
To the system of the solid oxidizer manufactured in the present embodiment for improving permanganate stability and oxidisability to the present embodiment
The permanganate solid material oxidant of Preparation Method preparation is used to implement to degrade during the method for organic pollutants, with double
Phenol A is target contaminant, under conditions of concentration is 50mg/L, with the permanganate solid material oxygen of one method of embodiment preparation
Agent is added to pH value to measure in 4,5,6,7,8,9,10,11,12 water sample
93.39%, 90.58%, 91.57%, 99.68%, 99.73%, 99.93%, 99.89%, 100%, 100%.And identical manganese
The water sample of the potassium permanganate of amount, different pH changes greatly the removal rate of bisphenol-A, from 70% to 95% etc., as shown in Figure 1.
It can be seen that the oxidisability of the permanganate solid material oxidant of the present embodiment method preparation is greatly improved.This implementation
Example is prepared for NEW TYPE OF COMPOSITE solid material oxidant, improves the stability and oxidation susceptibility of permanganate, and solve height
The problem of being affected when potassium manganate degradation bisphenol-A by pH value.
It is additionally carried out experimental analysis, in the bisphenol-A solution that pH value is 7, by the permanganate of one method of embodiment preparation
Solid material oxidant is added in the bisphenol-A solution of 10mg/L, 20mg/L, 30mg/L, 50mg/L, reaction 5min,
The concentration of bisphenol-A is measured at 15min, 30min, 45min and 60min, every group of experiment is respectively provided with two parallel control groups, in 5min
Within the bisphenol-A of 10mg/L can be completely removed, the bisphenol-A of other concentration can be completely removed within 30min, such as scheme
Shown in 2.It follows that the permanganate solid material oxidant of the present embodiment method preparation is higher than the degradation effect of organic matter
Traditional medicament or common potassium permanganate, when the permanganate solid material oxidant prepared using the present embodiment method carries out waste water
When degradation, reaction rate is obviously increased compared with prior art.
Embodiment two:
The present embodiment is basically the same as the first embodiment, and is particular in that:
In the present embodiment, a kind of preparation method for the solid oxidizer improving permanganate stability and oxidisability, packet
Include following steps:
A. a certain amount of magnesium nitrate, ferric nitrate, potassium permanganate and suitable water soluble alkali sodium hydroxide are weighed, it is spare；Nitre
The molar ratio of sour magnesium and ferric nitrate is 2:1, and the molar ratio of potassium permanganate and ferric nitrate is 1:1；
B. the magnesium nitrate and ferric nitrate in the step a are utilized, the mixing salt solution of magnesium nitrate and ferric nitrate is prepared；It adopts
Sodium hydroxide in the step a prepares the alkali liquid medicine that 100mL naoh concentration is 40g/L；By the mixing
Salting liquid is added in the alkali liquid medicine and is stirred mixing, and maintaining the mixing salt solution pH value of alkalinity is 10, and
It is stood for 24 hours after stirring 2h at room temperature, obtains the first emulsion；
C. it will be added to after the weighed equimolar potassium permanganate dissolution with ferric nitrate in the step in the step a
In the first emulsion prepared in b, is continuously stirred for 24 hours under conditions of 70 DEG C, obtain the second emulsion；
D. the second emulsion prepared in the step c is centrifuged, washed, collect solid content, and at 70 DEG C
Solid content is dried, to obtain permanganate solid material oxidant.
The height of the preparation method preparation of the solid oxidizer of permanganate stability and oxidisability is improved using the present embodiment
The application of manganate solid material oxidant, for implement degrade organic pollutants method during, by the Gao Meng
Hydrochlorate solid material oxidant is added in the wastewater sample to be processed that pH value is 4~12, and according to permanganate solid material
The dosage that the quality of oxidant and the volume of waste water to be processed calculate is 1.0g/L ratio, carries out permanganate solid material oxygen
Agent is launched, while being stirred to react to waste water to be processed, and the sexavalence manganese and seven in permanganate solid material oxidant is made
Valence manganese is reacted with useless Organic substance in water is converted to manganese dioxide, and is attached to permanganate solid material oxidant surface.
Experimental test and analysis:
The Gao Meng of the preparation method preparation of the solid oxidizer of permanganate stability and oxidisability is improved to the present embodiment
Hydrochlorate solid material oxidant carries out XRD structural analysis, it is seen that prepared permanganate solid material oxidant has stratiform
Metallic compound structure forms the value Mn composite material based on the value Mn of sexavalence manganese and septivalency manganese, utilizes the present embodiment
The permanganate solid material oxidant of the preparation method preparation of the solid oxidizer of permanganate stability and oxidisability is improved,
During method for implementing degradation organic pollutants, value Mn and waste water in permanganate solid material oxidant
Middle organic matter reaction is converted to manganese dioxide, and is attached to permanganate solid material oxidant surface.It can be seen that the present embodiment side
The stability of permanganate solid material oxidant of method preparation is greatly improved, the manganese dioxide generated after reaction still by
Laminated metal compound is absorbed and is fixed, and will not generate secondary pollution, the water treatment agent that can be significantly improved to subsequent processing
The rate of recovery.
To the system of the solid oxidizer manufactured in the present embodiment for improving permanganate stability and oxidisability to the present embodiment
The permanganate solid material oxidant of Preparation Method preparation is used to implement to degrade during the method for organic pollutants, with double
Phenol A is target contaminant, under conditions of concentration is 50mg/L, with the permanganate solid material oxygen of two method of embodiment preparation
Agent is added to pH value to measure in 4,5,6,7,8,9,10,11,12 water sample
99.80%, 99.67%, 100%, 99.95%, 100%, 100%, 99.91%, 99.91%, 95.54%.And identical manganese amount
Potassium permanganate, the water sample of different pH changes greatly the removal rate of bisphenol-A, from 70% to 95% etc., sees Fig. 3.Thus may be used
See, the oxidisability of the permanganate solid material oxidant of the present embodiment method preparation is greatly improved.The present embodiment preparation
NEW TYPE OF COMPOSITE solid material oxidant, improves the stability and oxidation susceptibility of permanganate, and solve potassium permanganate
The problem of being affected when degradation bisphenol-A by pH value.
It is additionally carried out experimental analysis, in the bisphenol-A solution that pH value is 7, permanganate solid prepared by embodiment two
Material oxidation agent is added in the bisphenol-A solution of 10mg/L, 20mg/L, 30mg/L, 50mg/L, reaction 5min, 15min,
The concentration of bisphenol-A is measured at 30min, 45min and 60min, every group of experiment is respectively provided with two parallel control groups, within 5min
The bisphenol-A of 10mg/L can be completely removed, the bisphenol-A of other concentration can be completely removed within 15min, see Fig. 4.Thus
It is found that the permanganate solid material oxidant of the present embodiment method preparation to the degradation effect of organic matter be higher than traditional medicament or
Common potassium permanganate, when the permanganate solid material oxidant prepared using the present embodiment method carries out wastewater degradation, with
The prior art is obviously increased compared to reaction rate.
Combination attached drawing of the embodiment of the present invention is illustrated above, but the present invention is not limited to the above embodiments, it can be with
The purpose of innovation and creation according to the present invention makes a variety of variations, under the Spirit Essence and principle of all technical solutions according to the present invention
Change, modification, substitution, combination or the simplification made, should be equivalent substitute mode, as long as meeting goal of the invention of the invention,
The technology of the preparation method and application of the solid oxidizer of permanganate stability and oxidisability is improved without departing from the present invention
Principle and inventive concept, belong to protection scope of the present invention.
Claims (8)
1. a kind of preparation method for the solid oxidizer for improving permanganate stability and oxidisability, which is characterized in that including such as
Lower step:
A. a certain amount of divalent metal salt, trivalent metal salt, potassium permanganate and suitable water soluble alkali are weighed, it is spare；Described two
The molar ratio of valence metal salt and trivalent metal salt is 2:1~3:1, and potassium permanganate and trivalent metal salt molar ratio are 1:1；
B. it utilizes the divalent metal salt and trivalent metal salt in the step a, prepares divalent metal salt and trivalent metal salt
Mixing salt solution；Using the water soluble alkali in the step a, alkali liquid medicine is prepared；The mixing salt solution is added to
It is stirred mixing in the alkali liquid medicine, and maintains the mixing salt solution pH value of alkalinity in 9~12 ranges, and in room temperature
After lower stirring at least 2h stand 16~for 24 hours, obtain the first emulsion；
C. the first emulsion prepared in the step b will be added to after potassium permanganate weighed in step a dissolution
In, it is continuously stirred at least for 24 hours under conditions of being not higher than 70 DEG C, obtains the second emulsion；
D. the second emulsion prepared in the step c is centrifuged, washed, collect solid content, and be not higher than 70 DEG C
Under solid content is dried, to obtain permanganate solid material oxidant.
2. the preparation method of the solid oxidizer of permanganate stability and oxidisability is improved according to claim 1, it is special
Sign is: the divalent metal salt is at least one of villaumite and nitrate of magnesium.
3. the preparation method of the solid oxidizer of permanganate stability and oxidisability is improved according to claim 1, it is special
Sign is: trivalent metal salt is at least one of villaumite and nitrate, the villaumite of iron and nitrate of aluminium.
4. the preparation method of the solid oxidizer of permanganate stability and oxidisability is improved according to claim 1, it is special
Sign is: water soluble alkali is at least one of sodium hydroxide, potassium hydroxide.
5. the preparation method of the solid oxidizer of permanganate stability and oxidisability is improved according to claim 1, it is special
Sign is: the permanganate solid material oxidant prepared in the step d have laminated metal compound structure, formed with
Value Mn composite material based on the value Mn of sexavalence manganese and septivalency manganese.
6. a kind of preparation method system using raising permanganate stability and the solid oxidizer of oxidisability described in claim 1
The application of standby permanganate solid material oxidant, it is characterised in that: the method for implementing degradation organic pollutants
In the process, the permanganate solid material oxidant is added in the waste water to be processed that pH value is 4~12, and according to Gao Meng
The dosage that the quality of hydrochlorate solid material oxidant and the volume of waste water to be processed calculate is 0.5~1.0g/L ratio, is carried out
Permanganate solid material oxidant is launched, while being stirred to react to waste water to be processed, and permanganate solid material oxygen is made
Sexavalence manganese and septivalency manganese in agent are reacted with useless Organic substance in water is converted to manganese dioxide, and is attached to permanganate solid material
Expect oxidant surface.
7. applying according to claim 6, it is characterised in that: during the method for organic pollutants of degrading, work as institute
When the concentration for stating the target contaminant bisphenol-A in waste water to be processed is 20~50mg/L or when being greater than 10mg/L, the time is handled
No more than 30min.
8. applying according to claim 6, it is characterised in that: during the method for organic pollutants of degrading, work as institute
When stating the concentration of the target contaminant bisphenol-A in waste water to be processed no more than 10mg/L, the processing time is not more than 5min.
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| JP2005046763A (en) * | 2003-07-30 | 2005-02-24 | Nippon Chem Ind Co Ltd | Method of treating environmental contaminant |
| CN102049258A (en) * | 2010-11-04 | 2011-05-11 | 哈尔滨工业大学 | Method for preparing composite type solid oxide catalyst |
| CN105314728A (en) * | 2015-11-25 | 2016-02-10 | 上海大学 | Method for degrading organic pollutant in water through activated persulfate |
| CN108423794A (en) * | 2018-04-02 | 2018-08-21 | 上海大学 | A kind of method of sulphite composite drug activation potassium permanganate degradation of organic substances |
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2019
- 2019-04-09 CN CN201910278210.XA patent/CN110066004A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005046763A (en) * | 2003-07-30 | 2005-02-24 | Nippon Chem Ind Co Ltd | Method of treating environmental contaminant |
| CN102049258A (en) * | 2010-11-04 | 2011-05-11 | 哈尔滨工业大学 | Method for preparing composite type solid oxide catalyst |
| CN105314728A (en) * | 2015-11-25 | 2016-02-10 | 上海大学 | Method for degrading organic pollutant in water through activated persulfate |
| CN108423794A (en) * | 2018-04-02 | 2018-08-21 | 上海大学 | A kind of method of sulphite composite drug activation potassium permanganate degradation of organic substances |
Non-Patent Citations (1)
| Title |
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| JINGJING YANG等: "Oxidationof bisphenol A by permanganate: reaction kinetics and removal of estrogenic activity", 《WATER SCIENCE & TECHNOLOGY》 * |
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Application publication date: 20190730 |