CN103949203B - A kind of preparation method of novel compound sewage process adsorbent - Google Patents
A kind of preparation method of novel compound sewage process adsorbent Download PDFInfo
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Abstract
The invention provides a kind of preparation method of novel compound sewage process adsorbent, it comprises: the first step, and preparation adopts dendroid quaternary ammonium salt four to gather the Concave-convex clay rod powder that surfactant carries out surface modification; Second step, prepares nano manganese oxide suspension; 3rd step, prepares potassium ferrate; 4th step, prepares compound sewage inorganic agent by the product compound that the first step is prepared to the 3rd step.This compound sewage inorganic agent utilizes Concave-convex clay rod, nano manganese oxide and potassium ferrate decontamination feature separately, use in conjunction, and by mutually making up, synergy, substantially increases the dirt-removing power to trade effluent.
Description
Technical field
The present invention relates to technical field of sewage, particularly relate to the preparation method of a kind of novel modified attapulgite clay-nano manganese oxide-potassium ferrate compound sewage process adsorbent.
Background technology
Along with expanding economy, the chemical plant of various places gets more and more, and the focus being treated as all circles' concern of trade effluent, at present, Industrial Wastewater Treatment common technology has charcoal absorption, zeolite exchange etc.Active carbon, because of features such as it are expensive, regeneration is complicated, is difficult to extensive use.Natural attapulgite clay is a kind of silicate clay mineral that occurring in nature extensively exists, there is special octahedral structure and higher cation exchange and physical absorption ability, it has the micro-structural of layer chain, fiber is elongated, duct is many, and surface area is comparatively large, generally presents earthy, bulk, there is stronger water imbibition and lower rainwater dilatancy, there is after moistening certain viscosity and good plasticity.Concave-convex clay rod, due to its special geological environment, has a wide range of applications, is more and more concerned in recent years.
At present, the domestic development and application to Concave-convex clay rod, especially utilizes the performance of its excellence to improve modification aspect and imperfection.Utilizing Concave-convex clay rod to carry out Industrial Waste Water Treatments is the importance that Concave-convex clay rod is applied, the environmental pollution that sewage discharge causes more and more is worth self-examination, utilize Concave-convex clay rod to carry out sewage disposal and be not only economy and technical problem, environmental issue especially, the reserves of China's Concave-convex clay rod are large, of high grade, utilize Concave-convex clay rod process trade effluent to have important and far-reaching meaning concerning our country.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of Concave-convex clay rod-nano manganese oxide compound sewage process adsorbent of novel surface modification, utilize Concave-convex clay rod, nano manganese oxide and potassium ferrate decontamination feature separately, use in conjunction, by mutually making up, synergy, substantially increases the dirt-removing power to trade effluent.
For solving the problems of the technologies described above, the invention provides a kind of preparation method of novel compound sewage process adsorbent, by Concave-convex clay rod being carried out modification and other adsorption components of compound are prepared from.
Present invention also offers a kind of preparation method of novel compound sewage process adsorbent, it comprises:
The first step, preparation adopts dendroid quaternary ammonium salt four to gather the Concave-convex clay rod powder that surfactant carries out surface modification;
Second step, prepares nano manganese oxide suspension;
3rd step, prepares potassium ferrate;
4th step, prepares compound sewage inorganic agent by the product compound that the first step is prepared to the 3rd step.
Wherein, the preparation method that described dendroid quaternary ammonium salt four gathers surfactant is specially: in the 250ml there-necked flask that condenser pipe is housed, add absolute ethyl alcohol 40ml, ethylenediamine 4.5g, room temperature carries out magnetic agitation, add epoxychloropropane 34.7g with 10/min, dropwise rear back flow reaction 4h.Four poly-surfactant-intermediates are obtained after decompression distillation, for faint yellow translucent thick liquid, get this intermediate 20g, be that absolute ethyl alcohol and the deionized water mixed solution 40ml of 1:1 is solvent with volume ratio, then drip 7.9gN, N-dimethyl dodecyl base tertiary amine, be warming up to 80 DEG C, reaction 1h, decompression distillation, recrystallization, vacuum drying acquisition white powdery solids is dendroid quaternary ammonium salt four and gathers surfactant.
Wherein, the described first step is specially and joins in deionized water by Concave-convex clay rod, stir 30min ~ 1h, be warming up to 30 DEG C ~ 50 DEG C afterwards, the dendroid quaternary ammonium salt four adding described preparation gathers surfactant, stirring reaction 5 ~ 10h, filter, washing, dry, pulverizing, obtains the Concave-convex clay rod powder of modification.
Wherein, described second step is specially at the temperature of 25 DEG C, under hyperacoustic effect, be that the liquor potassic permanganate of 0.1ml/L is slowly added drop-wise to that 4ml concentration is housed is in the conical flask of 1.5mol/L manganese acetate solution by 40ml concentration, dropwise the ultrasonic 5 ~ 10min of rear continuation.By the brown color manganese dioxide suspension 8000r/min high speed centrifugation be obtained by reacting, abandoning supernatant, deionized water is washed till neutrality, adds 43.5mL deionized water and makes MnO
2suspension, mass concentration is about 20g/L, 0 ~ 4 DEG C of preservation, for subsequent use.
Wherein, described 3rd step is specially: take 6.0g Fe(NO3)39H2O (Fe (NO
3)
39H
2o), NaOH 3.0g, in ice bath, sodium hydrate solid is added in 20ml clorox (NaClO), be stirred to solid to dissolve completely, continue to add NaOH to saturated, continue to stir 0.5h, then add Fe(NO3)39H2O (Fe (NO several times, on a small quantity
3)
39H
2o), control reaction temperature at 25 DEG C, constantly stir 1.5h, solution gradually becomes royal purple, shows there is Na
2feO
4generate, under agitation, add solid sodium hydroxide and again reach capacity, then continue the thickness stirring the change of 0.5h solution, centrifugal, suction filtration, obtains Na
2feO
4solution;
Solution temperature is kept to be 25 DEG C, add saturated potassium hydroxide solution, stir 15min, have atropurpureus to precipitate to generate, suction filtration, obtains potassium ferrate crude product, is dissolved by the potassium hydroxide solution of crude product 3mol/L, add saturated potassium hydroxide solution, put into ice bath to cool, have solid to wash out, suction filtration, filter residue cyclohexane is except anhydrating, lixiviating is removed again with absolute ethanol washing, finally with ether removing second alcohol and water, 60 DEG C of vacuum drying, the vacuum desiccator being placed in silica gel water absorbing agent is dry, obtains potassium ferrate.
Wherein, the Concave-convex clay rod powder that described 4th step is specially the surface modification first step prepared mixes with the ratio of distilled water according to mass ratio 1:10, be configured to suspension, pour in there-necked flask, add nano manganese oxide suspension prepared by second step and potassium ferrate prepared by the 3rd step more in proportion, stir with the speed of 200r/min, after 85 DEG C of constant temperature stir 3h, product is through suction filtration, washing 3 times, after 110 DEG C of dry 1h, put into Muffle furnace 350 DEG C calcining 3h, obtain compound sewage inorganic agent.
Beneficial effect of the present invention:
Concave-convex clay rod, nano manganese oxide and potassium ferrate are prepared into compound formulation by compound sewage process adsorbent provided by the invention, utilize Concave-convex clay rod, nano manganese oxide and potassium ferrate decontamination feature separately, use in conjunction, by mutually making up, synergy, substantially increases the dirt-removing power to trade effluent.
Accompanying drawing explanation
Fig. 1 is the XRD figure of compound sewage inorganic agent prepared by Concave-convex clay rod after Concave-convex clay rod former state, surface modification and the present invention, in figure A represent Concave-convex clay rod former state, B represent surface modification after Concave-convex clay rod, C represent compound sewage inorganic agent prepared by the present invention;
Fig. 2 is the IR figure of compound sewage inorganic agent prepared by Concave-convex clay rod after Concave-convex clay rod former state, surface modification and the present invention, in figure A represent Concave-convex clay rod former state, B represent surface modification after Concave-convex clay rod, C represent compound sewage inorganic agent prepared by the present invention.
Detailed description of the invention
A kind of clay mineral that it is key component that Concave-convex clay rod refers to attapulgite (attapulgite).Attapulgite is a kind of crystalloid hydrous magnesium aluminium silicate mineral, has unique layer chain structure feature, in its structure, there is crystal lattice, the Na containing non-quantitative in side crystal
+, Ca
2+, Fe
3+, Al
3+, crystal is needle-like, threadiness or fiber collection shape.Attapulgite has unique dispersion, high temperature resistant, anti-good colloidal nature and the higher adsorption bleaching ability such as saline and alkaline.And there is certain plasticity and cohesive force, its desirable chemical molecular formula is: Mg
5si
8o
20(OH)
2(OH
2)
44H2O, has the intermediate structure between chain structure and layer structure.No matter be in adsorption process, or in sewage disposal, Concave-convex clay rod can regenerate, its power consumption is few, highly beneficial to environmental protection.
Because Concave-convex clay rod is natural, therefore more or less having some limitations property, organic substance is adopted to carry out these defects that modification can improve Concave-convex clay rod to a great extent, the present invention is the impurity in disposing of sewage, organic substance is adopted to carry out modification to Concave-convex clay rod, improve its alternately performance and absorption property, Concave-convex clay rod after process becomes a kind of organic-inorganic composition, the organic group that molecular weight is very large instead of the original cation of Concave-convex clay rod, simultaneously, the particle surface meeting adsorb organic compound matter of Concave-convex clay rod, crystal structure inside can embed organic matter, replace the original crystallization water, the hydrophobicity of Concave-convex clay rod is strengthened greatly, improve the performance being adsorbed with organic pollutants, reach the efficiency improving sewage disposal.
Organic surface modifying material provided by the invention is specially dendroid quaternary ammonium salt four and gathers surfactant, and its structure is specifically such as formula shown in I:
Formula I
The concrete preparation method of described organic surface modifying material is: in the 250ml there-necked flask that condenser pipe is housed, add absolute ethyl alcohol 40ml, ethylenediamine 4.5g, room temperature carries out magnetic agitation, add epoxychloropropane 34.7g with 10/min, dropwise rear back flow reaction 4h.Four poly-surfactant-intermediates are obtained after decompression distillation, for faint yellow translucent thick liquid, get this intermediate 20g, be that absolute ethyl alcohol and the deionized water mixed solution 40ml of 1:1 is solvent with volume ratio, then drip 7.9gN, N-dimethyl dodecyl base tertiary amine, be warming up to 80 DEG C, reaction 1h, decompression distillation, recrystallization, vacuum drying acquisition white powdery solids is dendroid quaternary ammonium salt four and gathers surfactant.
Synthetic route is as follows:
Present invention also offers a kind of Concave-convex clay rod adopting organic surface modifying substance modification, its raw material comprises Concave-convex clay rod and dendroid quaternary ammonium salt four gathers surfactant, relative to the Concave-convex clay rod of 100 weight portions, the addition that dendroid quaternary ammonium salt four gathers surfactant is 10 weight portion ~ 20 weight portions, further preferred 15 weight portions.
Present invention also offers the method for modifying of Concave-convex clay rod, be specially:
Concave-convex clay rod is joined in deionized water, stir 30min ~ 1h, be warming up to 30 DEG C ~ 50 DEG C afterwards, add the dendroid quaternary ammonium salt four prepared above and gather surfactant, stirring reaction 5 ~ 10h, filter, washing, dry, pulverizing, obtains the Concave-convex clay rod powder of modification.
Manganese oxide is a kind of amphoteric metal oxide, and nanoscale manganese has the features such as specific area is large, ion-exchange capacity is strong, not only to heavy metal ion in water as Pb
2+, Cd
2+, Cu
2+, Ni
2+there is good removal ability, and have very strong oxidation and adsorption capacity to As (III) and As (V).
The preparation method of nano manganese oxide is specially:
At the temperature of 25 DEG C, under hyperacoustic effect, be that the liquor potassic permanganate of 0.1ml/L is slowly added drop-wise to that 4ml concentration is housed is in the conical flask of 1.5mol/L manganese acetate solution by 40ml concentration, dropwise the ultrasonic 5 ~ 10min of rear continuation.By the brown color manganese dioxide suspension 8000r/min high speed centrifugation be obtained by reacting, abandoning supernatant, deionized water is washed till neutrality, adds 43.5mL deionized water and makes MnO
2suspension, mass concentration is about 20g/L, 0 ~ 4 DEG C of preservation, and for subsequent use, reaction equation is as follows:
2KMnO
4+3Mn(Ac)
2+2H
2O→5MnO
2+2KAc+4HAc。
Potassium ferrate can sterilizing, the reducing substanceses such as the ammonia nitrogen in oxidation removal water, sulphur class material, phenols, and can not form organic chloride, cause secondary pollution, security is reliably guaranteed, and meanwhile, decomposition soluble in water produces (Fe (OH)
3) suspension in water is had to the effect of flocculation, absorption and co-precipitation.
The preparation method of potassium ferrate is specially:
The first step, takes 6.0g Fe(NO3)39H2O (Fe (NO
3)
39H
2o), NaOH 3.0g, in ice bath, sodium hydrate solid is added in 20ml clorox (NaClO), be stirred to solid to dissolve completely, continue to add NaOH to saturated, continue to stir 0.5h, then add Fe(NO3)39H2O (Fe (NO several times, on a small quantity
3)
39H
2o), control reaction temperature at 25 DEG C, constantly stir 1.5h, solution gradually becomes royal purple, shows there is Na
2feO
4generate, under agitation, add solid sodium hydroxide and again reach capacity, then continue the thickness stirring the change of 0.5h solution, centrifugal, suction filtration, obtains Na
2feO
4solution;
Second step, solution temperature is kept to be 25 DEG C, add saturated potassium hydroxide solution, stir 15min, have atropurpureus to precipitate and generate, suction filtration, obtain potassium ferrate crude product, the potassium hydroxide solution of crude product 3mol/L is dissolved, adds saturated potassium hydroxide solution, put into ice bath and cool, solid is had to wash out, suction filtration, filter residue cyclohexane except anhydrating, then removes lixiviating with absolute ethanol washing, finally with ether removing second alcohol and water, 60 DEG C of vacuum drying, the vacuum desiccator being placed in silica gel water absorbing agent is dry, obtains potassium ferrate.
The present invention is by utilizing Concave-convex clay rod, nano manganese oxide and potassium ferrate decontamination feature separately by being prepared into compound formulation by the Concave-convex clay rod of organic surface modifying substance modification, potassium ferrate and nano manganese oxide, use in conjunction, by mutually making up, synergy, substantially increase the dirt-removing power to trade effluent, in this compound sewage absorbent, main component is Concave-convex clay rod, adopts it as carrier.
Present invention also offers a kind of modified attapulgite clay-nano manganese oxide-potassium ferrate compound sewage process adsorbent, its raw materials comprises the above-mentioned Concave-convex clay rod by organic surface modifying substance modification, above-mentioned nano manganese oxide and above-mentioned potassium ferrate.
Further, described compound sewage process adsorbent is prepared from by the above-mentioned Concave-convex clay rod by organic surface modifying substance modification, above-mentioned nano manganese oxide and above-mentioned potassium ferrate.
Relative to the Concave-convex clay rod of the modification of 100 weight portions, the addition of described nano manganese oxide is 8 weight portion ~ 12 weight portions, the addition of described potassium ferrate is 5 weight portion ~ 10 weight portions, the addition of further preferred described nano manganese oxide is 10 weight portions, and the addition of described potassium ferrate is 8 weight portions.
Its preparation method of the present invention is specially:
The first step, adopts dendroid quaternary ammonium salt four to gather the Concave-convex clay rod powder that surfactant carries out surface modification according to method preparation above;
Second step, prepares nano manganese oxide suspension according to method above;
3rd step, prepares potassium ferrate according to method above;
4th step, the Concave-convex clay rod powder of the surface modification first step prepared mixes with the ratio of distilled water according to mass ratio 1:10, be configured to suspension, pour in there-necked flask, then add nano manganese oxide suspension prepared by second step and potassium ferrate prepared by the 3rd step in proportion, stir with the speed of 200r/min, after 85 DEG C of constant temperature stir 3h, product through suction filtration, washing 3 times, after 110 DEG C of dry 1h, put into Muffle furnace 350 DEG C calcining 3h, obtain compound sewage inorganic agent.
Below adopt embodiment to describe embodiments of the present invention in detail, to the present invention, how application technology means solve technical problem whereby, and the implementation procedure reaching technique effect can fully understand and implement according to this.
Embodiment 1 dendroid quaternary ammonium salt four gathers the preparation of surfactant
Be equipped with in the 250ml there-necked flask of condenser pipe, add absolute ethyl alcohol 40ml, ethylenediamine 4.5g, room temperature carries out magnetic agitation, adds epoxychloropropane 34.7g with 10/min, dropwises rear back flow reaction 4h.Four poly-surfactant-intermediates are obtained after decompression distillation, for faint yellow translucent thick liquid, get this intermediate 20g, be that absolute ethyl alcohol and the deionized water mixed solution 40ml of 1:1 is solvent with volume ratio, then drip 7.9gN, N-dimethyl dodecyl base tertiary amine, be warming up to 80 DEG C, reaction 1h, decompression distillation, recrystallization, vacuum drying acquisition white powdery solids is dendroid quaternary ammonium salt four and gathers surfactant.
Embodiment 2 dendroid quaternary ammonium salt four gathers surfactant-modified Concave-convex clay rod
100g Concave-convex clay rod is joined in deionized water, stirs 1h, be warming up to 40 DEG C afterwards, the dendroid quaternary ammonium salt four adding embodiment 1 preparation gathers surfactant 15g, stirring reaction 7h, filters, washing, dry, pulverizing, obtains the Concave-convex clay rod powder of modification.
The preparation of embodiment 3 nano-manganese dioxide
At the temperature of 25 DEG C, under hyperacoustic effect, be that the liquor potassic permanganate of 0.1ml/L is slowly added drop-wise to that 4ml concentration is housed is in the conical flask of 1.5mol/L manganese acetate solution by 40ml concentration, dropwise the ultrasonic 5 ~ 10min of rear continuation.By the brown color manganese dioxide suspension 8000r/min high speed centrifugation be obtained by reacting, abandoning supernatant, deionized water is washed till neutrality, and add 43.5mL deionized water and make nano-manganese dioxide suspension, mass concentration is about 20g/L.
The preparation of embodiment 4 potassium ferrate
Take 6.0g Fe(NO3)39H2O (Fe (NO
3)
39H
2o), NaOH 3.0g, in ice bath, sodium hydrate solid is added in 20ml clorox (NaClO), be stirred to solid to dissolve completely, continue to add NaOH to saturated, continue to stir 0.5h, then add Fe(NO3)39H2O (Fe (NO several times, on a small quantity
3)
39H
2o), control reaction temperature at 25 DEG C, constantly stir 1.5h, solution gradually becomes royal purple, shows there is Na
2feO
4generate, under agitation, add solid sodium hydroxide and again reach capacity, then continue the thickness stirring the change of 0.5h solution, centrifugal, suction filtration, obtains Na
2feO
4solution; Solution temperature is kept to be 25 DEG C, add saturated potassium hydroxide solution, stir 15min, have atropurpureus to precipitate to generate, suction filtration, obtains potassium ferrate crude product, is dissolved by the potassium hydroxide solution of crude product 3mol/L, add saturated potassium hydroxide solution, put into ice bath to cool, have solid to wash out, suction filtration, filter residue cyclohexane is except anhydrating, lixiviating is removed again with absolute ethanol washing, finally with ether removing second alcohol and water, 60 DEG C of vacuum drying, the vacuum desiccator being placed in silica gel water absorbing agent is dry, obtains potassium ferrate.
The preparation of embodiment 5 compound sewage inorganic agent 1
The Concave-convex clay rod powder 100g of surface modification embodiment 2 prepared mixes with 1L distilled water, be configured to suspension, pour in there-necked flask, add the nano manganese oxide suspension 500ml of embodiment 3 preparation and the potassium ferrate 8g of embodiment 4 preparation again, stir with the speed of 200r/min, after 85 DEG C of constant temperature stir 3h, product is through suction filtration, washing 3 times, after 110 DEG C of dry 1h, put into Muffle furnace 350 DEG C calcining 3h, obtain compound sewage inorganic agent 1.
Comparative example 1 compound sewage inorganic agent 2
Preparation method is identical with embodiment 5, and difference is that the surface modification of Concave-convex clay rod adopts softex kw to replace dendroid quaternary ammonium salt four to gather surfactant, and the method for surface modification is identical with embodiment 2.
Comparative example 2 compound sewage inorganic agent 3
Preparation method is identical with embodiment 5, and difference is that Concave-convex clay rod does not adopt any surface modifier to carry out modification.
Experiment
Experiment material:
Be divided into into 7 groups to test, first group of compound sewage inorganic agent 1 adopting the embodiment of the present invention 5 to prepare, second group of compound sewage inorganic agent 2 adopting comparative example 1 to prepare, the 3rd group of compound sewage inorganic agent 3 adopting comparative example 2 to prepare, nano-manganese dioxide prepared by the 4th group of the modified attapulgite clay powder directly embodiment 2 prepared, embodiment 3 and potassium ferrate prepared by embodiment 4 put into pending sewage in the ratio of embodiment 5, the 5th group of Concave-convex clay rod powder adopting embodiment 2 to prepare, the addition of each group inorganic agent is all identical.
Process waste water
Coal is selected to turn the sewage produced in oily industry.
Processing method
Add in trade effluent by above-mentioned inorganic agent, stir 1h ~ 2h, measure COD, ammonia nitrogen, basicity, BOD, SS and oil index, the indices of waste water carries out monitoring analysis according to " water and waste water detection method " the 4th edition.
Result
1 is the results are shown in Table before and after process.
The every result of table 1
As can be seen from Table 1, the obvious to the clean effect of industrial wastewater of the compound sewage inorganic agent of the embodiment of the present invention 1 preparation is adopted.
All above-mentioned this intellectual properties of primary enforcement, not setting restriction this new product of other forms of enforcement and/or new method.Those skilled in the art will utilize this important information, and foregoing is revised, to realize similar implementation status.But all modifications or transformation belong to the right of reservation based on new product of the present invention.
The above is only preferred embodiment of the present invention, and be not restriction the present invention being made to other form, any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the Equivalent embodiments of equivalent variations.But everyly do not depart from technical solution of the present invention content, any simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (5)
1. a preparation method for compound sewage process adsorbent, by Concave-convex clay rod being carried out modification and other adsorption components of compound are prepared from, is characterized in that comprising the steps:
The first step, preparation adopts dendroid quaternary ammonium salt four to gather the Concave-convex clay rod powder that surfactant carries out surface modification;
Second step, prepares nano manganese oxide suspension;
3rd step, prepares potassium ferrate;
4th step, prepares compound sewage inorganic agent by the product compound that the first step is prepared to the 3rd step;
The preparation method that described dendroid quaternary ammonium salt four gathers surfactant is specially: in the 250ml there-necked flask that condenser pipe is housed, add absolute ethyl alcohol 40ml, ethylenediamine 4.5g, room temperature carries out magnetic agitation, epoxychloropropane 34.7g is added with 10/min, dropwise rear back flow reaction 4h, four poly-surfactant-intermediates are obtained after decompression distillation, for faint yellow translucent thick liquid, get this intermediate 20g, take volume ratio as absolute ethyl alcohol and the deionized water mixed solution 40ml of 1:1 be solvent, drip 7.9gN again, N-dimethyl dodecyl base tertiary amine, be warming up to 80 DEG C, reaction 1h, decompression distillation, recrystallization, vacuum drying acquisition white powdery solids is dendroid quaternary ammonium salt four and gathers surfactant.
2. the preparation method of compound sewage process adsorbent as claimed in claim 1, it is characterized in that: the described first step is specially and joins in deionized water by Concave-convex clay rod, stir 30min ~ 1h, be warming up to 30 DEG C ~ 50 DEG C afterwards, the dendroid quaternary ammonium salt four adding described preparation gathers surfactant, stirring reaction 5 ~ 10h, filter, washing, dry, pulverizing, obtains the Concave-convex clay rod powder of modification.
3. the preparation method of compound sewage process adsorbent as claimed in claim 1, it is characterized in that: described second step is specially at the temperature of 25 DEG C, under hyperacoustic effect, be that the liquor potassic permanganate of 0.1ml/L is slowly added drop-wise to that 4ml concentration is housed is in the conical flask of 1.5mol/L manganese acetate solution by 40ml concentration, dropwise the ultrasonic 5 ~ 10min of rear continuation, by the brown color manganese dioxide suspension 8000r/min high speed centrifugation be obtained by reacting, abandoning supernatant, deionized water is washed till neutrality, adds 43.5mL deionized water and makes MnO
2suspension, mass concentration is about 20g/L, 0 ~ 4 DEG C of preservation, for subsequent use.
4. the preparation method of compound sewage process adsorbent as claimed in claim 1, is characterized in that: described 3rd step is specially, and takes 6.0g Fe(NO3)39H2O (Fe (NO
3)
39H
2o), NaOH 3.0g, in ice bath, sodium hydrate solid is added in 20ml clorox (NaClO), be stirred to solid to dissolve completely, continue to add NaOH to saturated, continue to stir 0.5h, then add Fe(NO3)39H2O (Fe (NO several times, on a small quantity
3)
39H
2o), control reaction temperature at 25 DEG C, constantly stir 1.5h, solution gradually becomes royal purple, shows there is Na
2feO
4generate, under agitation, add solid sodium hydroxide and again reach capacity, then continue the thickness stirring the change of 0.5h solution, centrifugal, suction filtration, obtains Na
2feO
4solution; Solution temperature is kept to be 25 DEG C, add saturated potassium hydroxide solution, stir 15min, have atropurpureus to precipitate to generate, suction filtration, obtains potassium ferrate crude product, is dissolved by the potassium hydroxide solution of crude product 3mol/L, add saturated potassium hydroxide solution, put into ice bath to cool, have solid to wash out, suction filtration, filter residue cyclohexane is except anhydrating, lixiviating is removed again with absolute ethanol washing, finally with ether removing second alcohol and water, 60 DEG C of vacuum drying, the vacuum desiccator being placed in silica gel water absorbing agent is dry, obtains potassium ferrate.
5. the preparation method of compound sewage process adsorbent as claimed in claim 1, it is characterized in that: the Concave-convex clay rod powder that described 4th step is specially the surface modification first step prepared mixes with the ratio of distilled water according to mass ratio 1:10, be configured to suspension, pour in there-necked flask, add nano manganese oxide suspension prepared by second step and potassium ferrate prepared by the 3rd step more in proportion, stir with the speed of 200r/min, after 85 DEG C of constant temperature stir 3h, product is through suction filtration, wash 3 times, after 110 DEG C of dry 1h, put into Muffle furnace 350 DEG C calcining 3h, obtain compound sewage inorganic agent.
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| CN110143624A (en) * | 2019-05-31 | 2019-08-20 | 中国石油大学(华东) | A kind of support type stabilizes the preparation method of potassium ferrate |
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| CN102371145A (en) * | 2010-08-18 | 2012-03-14 | 周济元 | Composite efficient cyanobacteria-eutrophication water treatment agent |
| CN103241793A (en) * | 2013-05-17 | 2013-08-14 | 杭州一清环保工程有限公司 | Multifunctional water treatment agent used for treating refractory wastewater |
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