CN110498471A - A kind of sewage-treating agent and preparation method thereof - Google Patents
A kind of sewage-treating agent and preparation method thereof Download PDFInfo
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- CN110498471A CN110498471A CN201910803144.3A CN201910803144A CN110498471A CN 110498471 A CN110498471 A CN 110498471A CN 201910803144 A CN201910803144 A CN 201910803144A CN 110498471 A CN110498471 A CN 110498471A
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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Abstract
The present invention relates to technical field of sewage, a kind of sewage-treating agent and preparation method thereof is proposed.The preparation method of above-mentioned sewage-treating agent includes: that magnesium hydroxide powder and aluminium-hydroxide powder that mass ratio is 2.13~2.35:1 are uniformly mixed to prepare magnalium mixture；Deionized water and ethyl alcohol that volume ratio is 4~5:1 are mixedly configured into mixed solvent, odium stearate is dissolved in the mixed solvent and is configured to the clear solution that concentration is 0.03~0.05mol/L；Magnalium mixture is added in clear solution under stirring and suspension is made；Odium stearate intercalation Mg is made after a hydro-thermal, freezing processing, secondary hydro-thermal, centrifugation and drying in suspension3Al-OH LDHs.Odium stearate intercalation Mg obtained above3Al-OH LDHs improves Mg3Adsorptivity of the Al-OH LDHs material to hydrophobic organic pollutant.
Description
Technical field
The present invention relates to technical field of sewage, and in particular to a kind of sewage-treating agent and preparation method thereof.
Background technique
Water is the lifeblood place of all things on earth in the important component and the earth of the earth.In recent years, with social economy
It rapidly develops, China's water pollution phenomenon is also got worse, and causes the highest attention appointed.Water pollutant includes inorganic pollution
And organic pollutant.Wherein, inorganic pollution mainly includes the heavy metal ion such as lead, cadmium, mercury, copper.These heavy metal elements exist
Have the characteristics that difficult to degrade, easy accumulation, irreversible, toxicity is big, metabolism is slow and is easily bioaccumulation in environment.A long-term drinking huge sum of money
The water for belonging to pollution can make one that acute and chronic poisoning occurs or lead to body canceration, and harm is serious.Organic pollutant category is various, and
And with the high speed development of petro chemical industry, many artificial synthesized organic pollutants are produced, such as organo-chlorine pesticide, macromolecule
Polymer, dyestuff, food additives etc..Wherein bad organic pollutant is teratogenesis, mutagenesis, carcinogen.
Currently, adsorbent is exactly a kind of common reagent there are many kinds of sewage-treating agents.Wherein, layered bi-metal hydrogen-oxygen
Compound (abbreviation LDHs), also known as houghite are a kind of novel adsorbents, are made of two or more skill element
Hydroxide with hydrotalcite layered crystal structure, chemical general formula are as follows: [MII 1-xMIII x(OH)2]x+An- x/n·mH2O, wherein
Mg3(chemical structural formula is [Mg to Al-OH LDHs3/4Al1/4(OH)2](OH)1/4Houghite) be adsorption effect preferable one
Kind.Some researches show that it can effectively remove some hydrophilic pollutants, but for hydrophobic organic pollutant removal
Effect is undesirable.How being modified enhancing to LDHs, it requires study for the removal effect of hydrophobic organic compound.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of sewage-treating agent, the above method is added cold using hydro-thermal twice
The technique for freezing processing, makes odium stearate to Mg3Al-OH LDHs material is modified, odium stearate intercalation Mg obtained3Al-
OH LDHs is good to the adsorption effect of hydrophobic organic pollutant.
Another object of the present invention is to provide a kind of sewage-treating agents, this sewage-treating agent odium stearate is to Mg3Al-
OH LDHs material is modified, and improves Mg3Al-OH LDHs material is obtained to the adsorptivity of hydrophobic organic pollutant
Odium stearate intercalation Mg3Al-OH LDHs is good to the adsorption effect of hydrophobic organic pollutant.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention proposes a kind of preparation method of sewage-treating agent comprising following steps:
S1 step: magnesium hydroxide powder and aluminium-hydroxide powder that mass ratio is 2.13~2.35:1 are uniformly mixed to prepare
Magnalium mixture；
S2 step: deionized water and ethyl alcohol that volume ratio is 4~5:1 are mixedly configured into mixed solvent, by odium stearate
It is dissolved in the mixed solvent and is configured to the clear solution that concentration is 0.03~0.05mol/L；
S3 step: magnalium mixture is added in clear solution under stirring and suspension is made；
S4 step: odium stearate is made after a hydro-thermal, freezing processing, secondary hydro-thermal, centrifugation and drying in suspension
Intercalation Mg3Al-OH LDHs。
Preferably, in S4 step, a hydro-thermal and secondary hydro-thermal carry out under stiring, and mixing speed is 120~240r/
min。
Preferably, in S4 step, a hydro-thermal are as follows: protected after being warming up to 90~100 DEG C with the heating rate of 1~3 DEG C/min
24~36h of temperature.
Preferably, in S4 step, freezing processing are as follows: the suspension obtained after hydro-thermal is placed in subzero 15 DEG C, and
Keep 30min.
Preferably, in S4 step, secondary hydro-thermal are as follows: protected after being warming up to 100~120 DEG C with the heating rate of 1~3 DEG C/min
2~4h of temperature, is then cooled to 30 DEG C with the rate of temperature fall of 2~4 DEG C/min.
Preferably, in S1 step, magnesium hydroxide powder and aluminium-hydroxide powder are mechanical under the revolving speed of 100~300r/min
1~3h of ball milling.
Preferably, in S3 step, the amount ratio of magnalium mixture and clear solution is 8~12g:150mL.
A kind of sewage-treating agent is made using the preparation method of above-mentioned sewage-treating agent.
The beneficial effect of the sewage-treating agent of the embodiment of the present invention and preparation method thereof is: a kind of preparation of sewage-treating agent
Method, using odium stearate, and using the method for a hydro-thermal, freezing processing and secondary hydro-thermal to traditional wastewater inorganic agent
Mg3Al-OH LDHs is modified.Traditional wastewater inorganic agent Mg3Adsorption effect of the Al-OH LDHs to hydrophily organic pollutant
Preferably, but it is very poor to the adsorption effect of hydrophobic organic pollutant.The hydrophobic group of odium stearate is alkyl, and hydrophilic group is carboxylic
Base.Under hydro-thermal reaction, sulfonic group can be inserted into Mg by electrostatic attraction and hydrogen bond action3Al-OH LDHs interlayer, makes it
Interlayer forms hydrophobic region, substantially increases the adsorption capacity to hydrophobic organic pollutant.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Layered double hydroxide (abbreviation LDHs), also known as houghite are a kind of novel adsorbents, by two kinds or
The hydroxide with hydrotalcite layered crystal structure of two or more skill element compositions, chemical general formula are as follows: [MII 1-xMIII x
(OH)2]x+An- x/n·mH2O, wherein Mg3(chemical structural formula is [Mg to Al-OH LDHs3/4Al1/4(OH)2](OH)1/4Class neatly
Stone) it is that adsorption effect is preferably a kind of.Some researches show that LDHs can effectively remove some hydrophilic organic pollutants, still
It is undesirable for hydrophobic organic pollutant removal effect.
Odium stearate also known as sodium stearate are interacted by octadecanoid acid and sodium hydroxide and are made, be soluble in hot water or
Hot alcohol.For aqueous solution because hydrolysis is in alkalinity, alcoholic solution is neutrality.Odium stearate has hydrophobic group and hydrophilic group, and hydrophobic group is hydrocarbon
Base, hydrophilic group are carboxyl.
Sewage-treating agent of the embodiment of the present invention and preparation method thereof is specifically described below.
A kind of preparation method of sewage-treating agent provided in an embodiment of the present invention, comprising the following steps:
S1 step: magnesium hydroxide powder and aluminium-hydroxide powder that mass ratio is 2.13~2.35:1 are uniformly mixed to prepare
Magnalium mixture；According to generation product odium stearate intercalation Mg3The molar ratio of magnesium and aluminium is 3:1 in Al-OH LDHs, corresponding
The optimum quality of magnesium hydroxide powder and aluminium-hydroxide powder ratio is 2.24:1.In ingredient, ratio floating range is within 5%
When, the result of final product is influenced smaller.
Further, above-mentioned magnesium hydroxide powder and the aluminium-hydroxide powder mechanical ball under the revolving speed of 100~300r/min
Grind 1~3h.Magnesium hydroxide powder and aluminium-hydroxide powder is not soluble in water and ethyl alcohol, can be effective under mechanical ball mill state
Magnesium hydroxide powder and aluminium-hydroxide powder powder are ground tiny.Also, prolonged mechanical ball mill can by magnesium atom and
Aluminium atom is adequately mixed on atomic level, for later period hydro-thermal reaction sufficiently carry out sound assurance is provided.
S2 step: deionized water and ethyl alcohol that volume ratio is 4~5:1 are mixedly configured into mixed solvent, by odium stearate
It is dissolved in the mixed solvent and is configured to the clear solution that concentration is 0.03~0.05mol/L；
It should be noted that using the mixed solvent that deionized water and ethyl alcohol are configured as raw material, it is water-soluble with traditional deionization
Agent, which is compared, has more special property, tends to make the growth of nucleus special, and material obtained is also more loose.It generates
Odium stearate intercalation Mg3Al-OH LDHs is loosely organized, can have many channels that sewage is allowed to enter, and improves the whole of material
Body utilization rate improves its adsorption effect.
S3 step: magnalium mixture is added in clear solution under stirring and suspension is made；Magnesium hydroxide powder
End and aluminium-hydroxide powder is not soluble in water and ethyl alcohol, is added under stirring, enables to magnalium mixture and clear solution
There is relatively good mixing.
Further, the amount ratio of above-mentioned magnalium mixture and above-mentioned clear solution is 8~12g:150mL.
S4 step: odium stearate is made after a hydro-thermal, freezing processing, secondary hydro-thermal, centrifugation and drying in suspension
Intercalation Mg3Al-OH LDHs。
Further, a hydro-thermal and secondary hydro-thermal carry out under stiring, and mixing speed is 120~240r/min.Hydrogen
Magnesium oxide powder and aluminium-hydroxide powder is not soluble in water and ethyl alcohol, hydro-thermal carry out under stirring enables to magnalium mixed
Closing object and clear solution has relatively good mixing, convenient for odium stearate is adequately intercalation into Mg3Al-OH LDHs。
Further, a hydro-thermal are as follows: after being warming up to 90~100 DEG C with the heating rate of 1~3 DEG C/min keep the temperature 24~
36h.Configure mixed solvent with deionized water and ethyl alcohol, obtained solvent than simple deionized water solution boiling point point, thus
In same reaction, the hydrothermal temperature needed is relatively low.It can make odium stearate with the heating of slow heating rate
Slowly be inserted into Mg3The interlayer of Al-OH LDHs.Prolonged heat preservation operation enables to odium stearate and Mg3Al-OH
Power and key between LDHs is more stable.
Further, freezing processing are as follows: the suspension obtained after a hydro-thermal is placed in subzero 15 DEG C, and is kept
30min.Freezing processing makes the suspension fast cooling obtained after a hydro-thermal to zubzero temperature, this process makes odium stearate
And Mg3The combination of Al-OH LDHs is more firm.
Further, secondary hydro-thermal are as follows: after being warming up to 100~120 DEG C with the heating rate of 1~3 DEG C/min keep the temperature 2~
Then 4h is cooled to 30 DEG C with the rate of temperature fall of 2~4 DEG C/min.In secondary water-heat process, Mg3Al-OH LDHs is not inserted
The interlayer for entering odium stearate can more be inserted into odium stearate, further increase Mg3The hydrophobic region of Al-OH LDHs.
The present invention also provides a kind of sewage-treating agents, are made using a kind of preparation method of above-mentioned sewage-treating agent.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of preparation method of sewage-treating agent provided in this embodiment comprising following steps:
S1 step: the aluminium-hydroxide powder powder of the magnesium hydroxide powder powder and 7.80g that weigh 17.50g is placed in ball
In grinding jar, keeping ratio of grinding media to material is 40, ball mill ball milling 2 hours obtained magnalium mixtures under the revolving speed of 200r/min；
S2 step: being mixed to prepare mixed solvent with 100mL ethyl alcohol for 450mL deionized water and it is standby to be heated to 50 DEG C of heat preservations
With weighing 6.12g odium stearate, and dissolve odium stearate using above-mentioned mixed dissolution and be settled in 500mL volumetric flask
500mL, the concentration that odium stearate is made is the clear solution of 0.04mol/L；
S3 step: the clear solution 379mL in S2 step, and the magnalium mixture that above-mentioned S1 step is uniformly mixed are measured
It is added under stirring in 379mL clear solution and suspension is made；
S4 step: suspension made from S3 step is put into the water heating kettle that volume is 1L and carries out a hydro-thermal, specific water
Thermal process are as follows: be warming up to after 95 DEG C with the heating rate of 2 DEG C/min and keep the temperature 30h, and carry out constantly being stirred in water-heat process
It mixes, mixing speed is set as 180r/min.
Suspension is put into low temperature refrigerator rapidly after the completion of hydro-thermal and carries out freezing processing 30min, sets deep freezer
Temperature be subzero 15 DEG C.
Suspension is put into the water heating kettle of 1L after the completion of freezing processing and carries out secondary hydro-thermal, specific hydrothermal process are as follows: with 2
DEG C/heating rate of min keeps the temperature 3h after being warming up to 110 DEG C, then 30 DEG C are cooled to the rate of temperature fall of 3 DEG C/min.Water
It is constantly stirred in thermal process, mixing speed is set as 180r/min.
Suspension by secondary hydro-thermal is by centrifuge solid-liquor separation, by obtained precipitating in a vacuum drying oven 120
Odium stearate intercalation Mg is made in DEG C dry 10h3Al-OH LDHs。
A kind of sewage-treating agent is made using the above method.
Embodiment 2
A kind of preparation method of sewage-treating agent provided in this embodiment comprising following steps:
S1 step: the aluminium-hydroxide powder powder of the magnesium hydroxide powder powder and 7.80g that weigh 18.33g is placed in ball
In grinding jar, keeping ratio of grinding media to material is 40, ball mill ball milling 3 hours obtained magnalium mixtures under the revolving speed of 100r/min；
S2 step: being mixed to prepare mixed solvent with 100mL ethyl alcohol for 500mL deionized water and it is standby to be heated to 50 DEG C of heat preservations
With weighing 7.65g odium stearate, and dissolve odium stearate and the constant volume in 500mL volumetric flask using above-mentioned mixed dissolution, system
The concentration for obtaining odium stearate is the clear solution of 0.05mol/L；
S3 step: the clear solution 344mL in S2 step, and the magnalium mixture that above-mentioned S1 step is uniformly mixed are measured
It is added under stirring in 344mL clear solution and suspension is made；
S4 step: suspension made from S3 step is put into the water heating kettle that volume is 1L and carries out a hydro-thermal, specific water
Thermal process are as follows: be warming up to after 100 DEG C and kept the temperature for 24 hours with the heating rate of 1 DEG C/min, and carry out in a water-heat process constantly into
Row stirring, mixing speed are set as 120r/min.
Suspension is put into low temperature refrigerator rapidly after the completion of hydro-thermal and carries out freezing processing 30min, sets deep freezer
Temperature be subzero 15 DEG C.
Suspension is put into the water heating kettle of 1L after the completion of freezing processing and carries out secondary hydro-thermal, specific hydrothermal process are as follows: with 3
DEG C/heating rate of min keeps the temperature 4h after being warming up to 100 DEG C, then 30 DEG C are cooled to the rate of temperature fall of 2 DEG C/min.Secondary
It is constantly stirred in water-heat process, mixing speed is set as 120r/min.
Suspension by secondary hydro-thermal is by centrifuge solid-liquor separation, by obtained precipitating in a vacuum drying oven 120
Odium stearate intercalation Mg is made in DEG C dry 10h3Al-OH LDHs。
A kind of sewage-treating agent is made using the above method.
Embodiment 3
A kind of preparation method of sewage-treating agent provided in this embodiment comprising following steps:
S1 step: the aluminium-hydroxide powder powder of the magnesium hydroxide powder powder and 7.80g that weigh 16.61g is placed in ball
In grinding jar, keeping ratio of grinding media to material is 40, ball mill ball milling 1 hour obtained magnalium mixture under the revolving speed of 300r/min；
S2 step: being mixed to prepare mixed solvent with 100mL ethyl alcohol for 400mL deionized water and it is standby to be heated to 50 DEG C of heat preservations
With weighing 2.30g odium stearate, and dissolve odium stearate and the constant volume in 250mL volumetric flask using above-mentioned mixed dissolution, system
The concentration for obtaining odium stearate is the clear solution of 0.03mol/L；
S3 step: the clear solution 207mL in S2 step, and the magnalium mixture that above-mentioned S1 step is uniformly mixed are measured
It is added under stirring in 207mL clear solution and suspension is made；
S4 step: suspension made from S3 step is put into the water heating kettle that volume is 0.5L and carries out a hydro-thermal, specifically
Hydrothermal process are as follows: be warming up to after 90 DEG C with the heating rate of 3 DEG C/min and keep the temperature 36h, and carried out constantly in a water-heat process
It is stirred, mixing speed is set as 240r/min.
Suspension is put into low temperature refrigerator rapidly after the completion of hydro-thermal and carries out freezing processing 30min, sets deep freezer
Temperature be subzero 15 DEG C.
Suspension is put into the water heating kettle of 0.5L after the completion of freezing processing and carries out secondary hydro-thermal, specific hydrothermal process are as follows:
It is warming up to after 120 DEG C with the heating rate of 1 DEG C/min and keeps the temperature 2h, be then cooled to 30 DEG C with the rate of temperature fall of 4 DEG C/min.Two
It is constantly stirred in secondary water-heat process, mixing speed is set as 240r/min.
Suspension by secondary hydro-thermal is by centrifuge solid-liquor separation, by obtained precipitating in a vacuum drying oven 120
Odium stearate intercalation Mg is made in DEG C dry 10h3Al-OH LDHs。
A kind of sewage-treating agent is made using the above method.
Embodiment 4
A kind of preparation method of sewage-treating agent provided in this embodiment comprising following steps:
S1 step: the aluminium-hydroxide powder powder of the magnesium hydroxide powder powder and 7.80g that weigh 17.47g is placed in ball
In grinding jar, keeping ratio of grinding media to material is 40, ball mill ball milling 1 hour obtained magnalium mixture under the revolving speed of 100r/min；
S2 step: being mixed to prepare mixed solvent with 100mL ethyl alcohol for 450mL deionized water and it is standby to be heated to 50 DEG C of heat preservations
With weighing 6.12g odium stearate, and dissolve odium stearate and the constant volume in 500mL volumetric flask using above-mentioned mixed dissolution, system
The concentration for obtaining odium stearate is the clear solution of 0.04mol/L；
S3 step: the clear solution 474mL in S2 step, and the magnalium mixture that above-mentioned S1 step is uniformly mixed are measured
It is added under stirring in 474mL clear solution and suspension is made；
S4 step: suspension made from S3 step is put into the water heating kettle that volume is 1L and carries out a hydro-thermal, specific water
Thermal process are as follows: be warming up to after 100 DEG C with the heating rate of 2 DEG C/min and keep the temperature 36h, and carry out in a water-heat process constantly into
Row stirring, mixing speed are set as 120r/min.
Suspension is put into low temperature refrigerator rapidly after the completion of hydro-thermal and carries out freezing processing 30min, sets deep freezer
Temperature be subzero 15 DEG C.
Suspension is put into the water heating kettle of 1L after the completion of freezing processing and carries out secondary hydro-thermal, specific hydrothermal process are as follows: with 3
DEG C/heating rate of min keeps the temperature 4h after being warming up to 100 DEG C, then 30 DEG C are cooled to the rate of temperature fall of 3 DEG C/min.Secondary
It is constantly stirred in water-heat process, mixing speed is set as 180r/min.
Suspension by secondary hydro-thermal is by centrifuge solid-liquor separation, by obtained precipitating in a vacuum drying oven 120
Odium stearate intercalation Mg is made in DEG C dry 10h3Al-OH LDHs。
A kind of sewage-treating agent is made using the above method.
Embodiment 5
A kind of preparation method of sewage-treating agent provided in this embodiment comprising following steps:
S1 step: the aluminium-hydroxide powder powder of the magnesium hydroxide powder powder and 7.80g that weigh 17.47g is placed in ball
In grinding jar, keeping ratio of grinding media to material is 40, ball mill ball milling 3 hours obtained magnalium mixtures under the revolving speed of 300r/min；
S2 step: being mixed to prepare mixed solvent with 100mL ethyl alcohol for 400mL deionized water and it is standby to be heated to 50 DEG C of heat preservations
With weighing 4.60g odium stearate, and dissolve odium stearate and the constant volume in 500mL volumetric flask using above-mentioned mixed dissolution, system
The concentration for obtaining odium stearate is the clear solution of 0.03mol/L；
S3 step: the clear solution 316mL in S2 step, and the magnalium mixture that above-mentioned S1 step is uniformly mixed are measured
It is added under stirring in 316mL clear solution and suspension is made；
S4 step: suspension made from S3 step is put into the water heating kettle that volume is 1L and carries out a hydro-thermal, specific water
Thermal process are as follows: be warming up to after 95 DEG C with the heating rate of 3 DEG C/min and keep the temperature 30h, and carry out in a water-heat process constantly into
Row stirring, mixing speed are set as 240r/min.
Suspension is put into low temperature refrigerator rapidly after the completion of hydro-thermal and carries out freezing processing 30min, sets deep freezer
Temperature be subzero 15 DEG C.
Suspension is put into the water heating kettle of 1L after the completion of freezing processing and carries out secondary hydro-thermal, specific hydrothermal process are as follows: with 2
DEG C/heating rate of min keeps the temperature 3h after being warming up to 110 DEG C, then 30 DEG C are cooled to the rate of temperature fall of 2 DEG C/min.Secondary
It is constantly stirred in water-heat process, mixing speed is set as 120r/min.
Suspension by secondary hydro-thermal is by centrifuge solid-liquor separation, by obtained precipitating in a vacuum drying oven 120
Odium stearate intercalation Mg is made in DEG C dry 10h3Al-OH LDHs。
A kind of sewage-treating agent is made using the above method.
Comparative example 1
This comparative example 1 is with the main distinction in embodiment 1:
In the preparation method of sewage-treating agent, after a hydro-thermal, 30 are cooled to the rate of temperature fall of 3 DEG C/min
℃.Then secondary hydro-thermal is carried out, is warming up to after 110 DEG C with the heating rate of 2 DEG C/min and keeps the temperature 3h, then with the drop of 3 DEG C/min
Warm rate is cooled to 30 DEG C.It is constantly stirred in water-heat process, mixing speed is set as 180r/min.Secondary water
The suspension obtained after heat is by centrifuge solid-liquor separation, and by obtained precipitating, 120 DEG C of dry 10h are made in a vacuum drying oven
Odium stearate intercalation Mg3Al-OH LDHs。
Comparative example 2
This comparative example 2 is with the main distinction in embodiment 1:
In the preparation method of sewage-treating agent, after a hydro-thermal, 30 are cooled to the rate of temperature fall of 3 DEG C/min
℃.Directly to obtained suspension by centrifuge solid-liquor separation, by the 120 DEG C of dryings in a vacuum drying oven of obtained precipitating
Odium stearate intercalation Mg is made in 10h3Al-OH LDHs。
Comparative example 3
This comparative example 3 and the main distinction of embodiment 1 are:
In S2 step, without dissolution odium stearate in clear solution, above-mentioned clear solution and mixed solvent at split-phase
Together.
Test example 1
The odium stearate intercalation Mg prepared using Examples 1 to 5 and comparative example 1~33At Al-OH LDHs sewage-treating agent
Wastewater Sample is managed, the amount of nitrobenzene compounds in sewage before and after the processing is measured, said determination uses gas chromatography.
Use instrument: 6890 gas chromatograph of Agilent, cooperation shunting/without stream capillary sample inlet mouth and micro- pond electron capture detection
Device.
Specific steps:
(1), standard curve is drawn
Nitrobenzene compounds Standard Stock solutions are used to be configured to molten for the standard series of 5~1000 μ g/L using concentration
Liquid.Take each 1 μ L of above-mentioned standard serial solution to be analyzed, gas chromatographic analysis using DB-5 quartz capillary chromatographic column (30m ×
0.25 250 μm of μ m), analysis condition are as follows: 60 DEG C of chromatographic column initial temperature, 220 DEG C of reservation 12min, column are raised to 10 DEG C/min
Flow velocity is 1.6mL/min；220 DEG C of injector temperature, Splitless injecting-Sample speed is 20mL/min；From sample introduction to unlatching flow divider
Time is 0.75min；Detector temperature is 310 DEG C, make-up gas 60mL/min.Above-mentioned each concentration replication twice, with two
Secondary average value draws standard curve.
(2), sample preparation and measurement are carried out using distillation-Toluene Extraction
Water sample is shaken up, the accurate 200mL that measures is placed in separatory funnel, and 10mL toluene is added, shakes 3min, stands 10min,
Two phase stratification abandons water phase.It is collected in 250mL boiling flask after extract liquor is dried column by anhydrous sodium sulfate, then with 5mL
Toluene extraction is primary, combining extraction liquid；Extract liquor is concentrated by evaporation to 2mL, and toluene is added and is settled to 250mL.
Outer mark method can be used in the quantitative analysis of nitrobenzene compounds, calculates according to following formula: C=(Ai-Ao/As)
×Cs×V1/V2,
C in formula: the concentration of nitrobenzene compounds each component, mg/L in water sample；
Ai: component response is detected in water sample；
Ao: component response is detected in blank sample；
As: component response is detected in standard sample；
Cs: concentration of component, mg/L are detected in standard sample；
V1: sample constant volume volume, mL；
V2: water sample constant volume volume, mL.
By the concentration summation of nitrobenzene compounds each component in the water sample measured.
Test example 2
The odium stearate intercalation Mg prepared using Examples 1 to 5 and comparative example 1~33At Al-OH LDHs sewage-treating agent
Wastewater Sample is managed, the amount of polycyclic aromatic hydrocarbon compounds in sewage before and after the processing is measured, said determination uses gas chromatography.
Use instrument: 6890 gas chromatograph of Agilent, cooperation shunting/without stream capillary sample inlet mouth and micro- pond electron capture detection
Device, extraction shaker, Rotary Evaporators, silicagel column 1000mg/6.0mL.
Specific steps:
(1), standard curve is drawn
The standard for the use of concentration being 1~1000 μ g/mL is configured to using polycyclic aromatic hydrocarbon Standard Stock solutions, and with n-hexane
Serial solution.Each 1 μ L of above-mentioned standard serial solution is taken to be analyzed, gas chromatographic analysis uses DB-5 quartz capillary chromatographic column
(320 μm of the μ m of 30m × 0.25), analysis condition are as follows: 60 DEG C of chromatographic column initial temperature, 300 DEG C of reservations are raised to 12 DEG C/min
12min, column flow rate 1.0mL/min；Carrier gas hydrogen flow rate 1.8mL/min；300 DEG C of holding 5min of injector temperature, no shunting
Sample introduction speed is 20mL/min；310 DEG C of temperature, hydrogen flow rate 40mL/min of 200 detector of hydrogen flameionization (FID), air
350mL/min.Above-mentioned each concentration replication draws standard curve twice, with average value twice.
(2), sample preparation and measurement
It takes 1000mL water sample to be measured in separatory funnel, 50mL methylene chloride is added, adds 30g sodium chloride, vibrates, puts
After gas sodium dissolution to be chlorinated, it is placed in and extracts oscillation extraction 20min on shaker, after stratification, extract liquor is through anhydrous sodium sulfate
Dry column is collected in 250mL boiling flask, then primary, combining extraction liquid is extracted with 50mL methylene chloride；Extract liquor is through evaporating
After being concentrated into 2mL, n-hexane is added and is settled to 5mL.
Outer mark method can be used in the quantitative analysis of polycyclic aromatic hydrocarbon compounds, calculates according to following formula: C=(Ai-Ao/As)
×Cs×V1/V2,
C in formula: the concentration of cycloaromatics each component, mg/L are crossed in water sample；
Ai: component response is detected in water sample；
Ao: component response is detected in blank sample；
As: component response is detected in standard sample；
Cs: concentration of component, mg/L are detected in standard sample；
V1: sample constant volume volume, mL；
V2: water sample constant volume volume, mL.
By the concentration summation of polycyclic aromatic hydrocarbon compounds each component in the water sample measured.
The polycyclic aromatic hydrocarbon that the total concentration for the nitrobenzene compounds each component that test example 1 measures and test example 2 are measured
The total concentration for closing object each component is recorded in table 1.
Nitrobenzene in the sewage-treating agent of 1. raw sewage of table, Examples 1 to 5 and comparative example 1~3 treated sewage
The total concentration of compound each component and the total concentration of polycyclic aromatic hydrocarbon compounds each component
According to the experimental result of table 1 it can be seen that 8 sewage treatments prepared by (1) Examples 1 to 5 and comparative example 1~3
In agent, using sewage-treating agent-odium stearate intercalation Mg of the preparation of embodiment 13Al-OH LDHs has optimal organic contamination
Object handles adsorption capacity, can effectively adsorb to the organic pollutant in sewage, achievees the purpose that purify sewage.(2)
When comparative example 3 prepares sewage-treating agent, other than not adding odium stearate, other processes and embodiment 1 are consistent, but prepare
Adsorption energy of the sewage-treating agent to above two hydrophobic organic pollutant (nitrobenzene compounds and polycyclic aromatic hydrocarbon compounds)
Power is very low, but the embodiment 1 that odium stearate is added is fine to above two hydrophobic organic pollutant effect, illustrates hard
Resin acid sodium is modified to have obviously effect.(3) although sewage-treating agent prepared by comparative example 1 also has good organic contamination
The adsorption effect of object, but compared with sewage-treating agent prepared by embodiment 1, effect or far short of what is expected.The reason is that 1 He of comparative example
Embodiment 1 illustrates that freezing processing is preferably inserted into Mg to odium stearate compared to not having freezing processing process3Al-OH LDHs interlayer
Favorably.(4) comparative example 2 is compared with comparative example 3, has lacked sewage-treating agent made of the comparative example 2 of secondary hydrothermal step to above-mentioned
The treatment effect of hydrophobic organic pollutant is weaker, illustrates that secondary hydro-thermal is inserted into Mg to odium stearate3Al-OH LDHs interlayer has
It helps.
In conclusion the sewage-treating agent of the embodiment of the present invention and the preparation method of sewage-treating agent, using odium stearate,
And using the method for a hydro-thermal, freezing processing and secondary hydro-thermal to traditional wastewater inorganic agent Mg3Al-OH LDHs is modified.
Traditional wastewater inorganic agent Mg3Al-OH LDHs is preferable to the adsorption effect of hydrophily organic pollutant, but organic to hydrophobicity
The adsorption effect of pollutant is very poor.The hydrophobic group of odium stearate is alkyl, and hydrophilic group is carboxyl.Under hydro-thermal reaction, sulfonic group
Mg can be inserted by electrostatic attraction and hydrogen bond action3Al-OH LDHs interlayer makes its interlayer form hydrophobic region, greatly improves
To the adsorption capacity of hydrophobic organic pollutant.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (8)
1. a kind of preparation method of sewage-treating agent, characterized in that it comprises:
S1 step: magnesium hydroxide powder and aluminium-hydroxide powder that mass ratio is 2.13~2.35:1 are uniformly mixed to prepare magnalium
Mixture；
S2 step: deionized water and ethyl alcohol that volume ratio is 4~5:1 are mixedly configured into mixed solvent, odium stearate is dissolved
The clear solution that concentration is 0.03~0.05mol/L is configured in the in the mixed solvent；
S3 step: the magnalium mixture is added in the clear solution under stirring, suspension is made；
S4 step: odium stearate is made after a hydro-thermal, freezing processing, secondary hydro-thermal, centrifugation and drying in the suspension
Intercalation Mg3Al-OH LDHs。
2. a kind of preparation method of sewage-treating agent according to claim 1, which is characterized in that in S4 step, described one
Secondary hydro-thermal and the secondary hydro-thermal carry out under stiring, and mixing speed is 120~240r/min.
3. a kind of preparation method of sewage-treating agent according to claim 1, which is characterized in that in S4 step, described one
Secondary hydro-thermal are as follows: 24~36h is kept the temperature after being warming up to 90~100 DEG C with the heating rate of 1~3 DEG C/min.
4. a kind of preparation method of sewage-treating agent according to claim 1, which is characterized in that described cold in S4 step
Jelly processing are as follows: the suspension obtained after a hydro-thermal is placed in subzero 15 DEG C, and keeps 30min.
5. a kind of preparation method of sewage-treating agent according to claim 1, which is characterized in that in S4 step, described two
Secondary hydro-thermal are as follows: 2~4h is kept the temperature after being warming up to 100~120 DEG C with the heating rate of 1~3 DEG C/min, then with 2~4 DEG C/min's
Rate of temperature fall is cooled to 30 DEG C.
6. a kind of preparation method of sewage-treating agent according to claim 1, which is characterized in that in S1 step, the hydrogen
Magnesium oxide powder and the aluminium-hydroxide powder 1~3h of mechanical ball mill under the revolving speed of 100~300r/min.
7. a kind of preparation method of sewage-treating agent according to claim 1, which is characterized in that in S3 step, the magnesium
The amount ratio of aluminium mixture and the clear solution is 8~12g:150mL.
8. a kind of sewage-treating agent, which is characterized in that utilize a kind of described in any item sewage-treating agents of claim 1~7
Preparation method is made.
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