CN101935101A - Method for preparing absorptive reducing material - Google Patents
Method for preparing absorptive reducing material Download PDFInfo
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- CN101935101A CN101935101A CN 201010262289 CN201010262289A CN101935101A CN 101935101 A CN101935101 A CN 101935101A CN 201010262289 CN201010262289 CN 201010262289 CN 201010262289 A CN201010262289 A CN 201010262289A CN 101935101 A CN101935101 A CN 101935101A
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Abstract
The invention discloses a method for preparing an absorptive reducing material, which comprises the following steps of: dropwise adding 0.3-0.4mol of Na2CO3 solution into an FeCl3 solution with the volume of 1L and the concentration of 0.6-0.8mol/L at room temperature for preparing iron carbonyl pillared liquid; dropwise adding 50-100mL of iron carbonyl pillared liquid into suspension containing 10g of bentonite in a water bath at 60-65 DEG C for preparing inorganic pillared bentonite; and finally, carrying out mixing reaction on the obtained inorganic pillared bentonite with 60-100mL of organic solvent and 5-20mmol of silylating reagent. With the bentonite used as a matrix, nano zero-valent iron is prepared among bentonite nano layers, which can be used for controlling water pollution, and the like; by introducing the silylating reagent among the bentonite layers, on one hand, the drainage performance of bentonite and the absorptive capability of organic matter are improved, on the other hand, the distance of the bentonite layers can be expanded; the nano zero-valent iron fully plays a role in fully touching adsorbed pollutants and performs the nano effect of rapidly converting the pollutants, and a converted organic product is beneficial to microbiological degradation.
Description
Technical field
The present invention relates to environmental pollution control and repair, relate in particular to a kind of pollutent absorption and reductive preparation methods of can be used for.
Background technology
Nano metal particles has characteristics such as size is little, specific surface area is big, all shows numerous characteristics at aspects such as catalysis, optics and electromagnetism, and therefore, its preparation and applied research become the focus that countries in the world are paid close attention to.Because the specific surface energy of nanoparticle is very high, very easily is agglomerated into macrobead in preparation process, thus vertical many excellent specific properties of forfeiture nanoparticle.Utilize the confinement effect of nano-reactor to prepare the metal nanoparticle compound catalyze material of polymolecularity, can overcome the reunion of nanoparticle, and facilitate dispersion of particles.And the silicate minerals of laminate structure such as wilkinite have big internal surface and nanometer sheet sheaf space, and it as nano-reactor, can effectively be avoided the generation of reuniting, and are particularly useful for making the nanoparticle with narrow particle diameter and polymolecularity.
Zero-valent Iron can be applied to the improvement and the reparation of multiple polluted water, has treatment effect preferably, and have easy to use, energy consumption is low, can improve advantages such as wastewater biodegradability, has been used to handle halo organic waste water, agricultural chemicals waste water, waste water from dyestuff etc.Nano iron particles is little because of particle diameter, and particulate specific surface area and surface energy are big, thereby has excellent adsorption performance and reducing activity.Utilize nanometer iron to handle all kinds of vattability waste water and have bigger potentiality.But also there are problems such as easy oxidation and particle agglomeration in actual applications in nanometer iron.Document (petrochemical complex 2004 33 volume supplementary issue 123 pages) has been introduced a kind of being nano-reactor between cheating engaging layer, KBH
4Be reductive agent, prepare nanometer iron/montmorillonite Composite catalytic material at normal temperatures, iron particle high dispersing that makes and particle diameter are narrow respectively; This material is in actual application: because the iron particle particle radius is little, the bentonite lamella spacing that is strutted has only 1.29nm, and lamella is because the fixed action of iron particle loses swelling property, therefore, when organic pollutant is handled in being applied to waste water, pollutent can't be adsorbed also contact, lose the effect that it should be brought into play with nano zero valence iron.
Summary of the invention
The objective of the invention is for overcoming the deficiencies in the prior art, a kind of pollutent absorption and reductive preparation methods of can be used for is provided, the applying silicon oxide structure supports in this method, the bentonite bed spacing is increased, make prepared material can be effective to reduction and be difficult to biodegradable organic substance, improve the biodegradability of waste water.
The technical solution used in the present invention is in turn include the following steps:
1) under the room temperature, be that 1L, concentration are the FeCl of 0.6～0.8mol/L to volume
3Dripping total amount in the solution is the Na of 0.3～0.4mol
2CO
3Solution continues in the dropping process to stir, and is added dropwise to complete the back and continues to stir 2～2.5h, and aging then 24h obtains the pillared liquid of iron carbonyl;
2) in 60～65 ℃ of water-baths, the pillared liquid of Dropwise 5 0～100mL iron carbonyl in containing the bentonitic suspension liquid of 10g, continuously stirring in the dropping process, dropwise the back and stir 2.0～3.0h down in 60～65 ℃ of the same terms, aging 24h under 60 ℃ of constant temperature, centrifugation is used deionized water wash 4-5 time earlier with resulting solids, dry 12～36h down at 95 ℃～125 ℃ then, obtain inorganic pillared bentonite;
3) the inorganic pillared bentonite of gained is mixed with 60mL～100mL organic solvent and 5mmol～20mmol silylating reagent, reacted 12～36 hours, filter, the gained solid product is used acetone rinsing 3～5 times earlier, again 90 ℃～120 ℃ following vacuum-dryings 12～36 hours;
4) the vacuum-drying after product is added 50～60ml deionized water, feed N
2Stirring into solution after the protection, is the KBH of 1mol/L with 50～80ml concentration
4Solution adds in the above-mentioned solution that stirs into, and continues to stir 120～240min again;
5) the step 4) product is carried out centrifugation, use washed with de-ionized water, 60～70 ℃ of freeze-day with constant temperature 5～6h promptly get the absorbing and reducing material in vacuum drying oven.
Described wilkinite is sodium bentonite or calcium-base bentonite, and organic solvent is toluene, benzene, acetone or pyridine.Silylating reagent is that chemical structure of general formula is R
N-Si-X
4-NOrganosilane, wherein, N=1～3, R comprises that carbonatoms is that 1～18 alkyl, phenyl and carbonatoms are the organic group of 1～18 amino, cyano group, sulfydryl, chlorine substituted alkyl, X is the hydrolyzable part that comprises halogen, amino, methoxyl group, oxyethyl group.
The invention has the beneficial effects as follows:
1, the present invention as matrix, gives full play to bentonitic confinement effect with wilkinite, makes nano zero valence iron at the bentonite nano interlayer, can be used for the reparation of water pollution etc.
2, between bentonite bed, introduce silylating reagent, improved bentonitic hydrophobic performance on the one hand, improve organic adsorptive power, can strut the bentonite bed spacing on the other hand, nano zero valence iron is played one's part to the full, the pollutent after the absorption is fully contacted, bring into play its nano effect again, rapidly pollutent is transformed, transform the back organic product and help microbiological deterioration.
Embodiment 1
Under the room temperature, be 1L to volume, concentration is the FeCl of 0.8mol/L
3Dripping total amount in the solution is the Na of 0.4mol
2CO
3Solution continues in the dropping process to stir, and is added dropwise to complete the back and continues to stir 2.5h, and aging then 24h obtains the pillared liquid of iron carbonyl; In 65 ℃ of water-baths, in the suspension liquid that contains the 10g calcium-base bentonite, drip the pillared liquid of 100mL iron carbonyl, continuously stirring in the dropping process, dropwise the back and stir 2.0h down in 65 ℃ of the same terms, aging 24h under 60 ℃ of constant temperature, centrifugation is with solids deionized water wash 5 times that obtain, the solid that obtains is dried 12h down at 125 ℃, obtains inorganic pillared bentonite; With the inorganic pillared bentonite of gained and 60mL toluene, 20mmol octadecyl trichlorosilane (Cl
3Si (CH
2)
17CH
3), reacted 36 hours, filter, with acetone rinsing 5 times of gained solid product, remove unreacted silylating reagent and organic solvent, the gained solid was 90 ℃ of following vacuum-dryings 12 hours; Add the 50ml deionized water again, feed N
2Stir the protection back, is the KBH of 1mol/L again with 50ml concentration
4Solution adds in the above-mentioned solution, continues to stir 120min; Washed with de-ionized water is used in centrifugation, and 70 ℃ of dry 5h of constant temperature in vacuum drying oven promptly obtain can be used for pollutent absorption and reductive material.The products therefrom interlamellar spacing is 1.95nm.
The 500mL concentration of packing in Brown Glass Brown glass bottles and jars only is the 40mg/L nitrobenzene solution, adds the repair materials for preparing with aforesaid method of 8g again, 25 ℃ of constant temperature vibration 20min, and precipitate and separate is measured the concentration of oil of mirbane in the solution, and clearance is 96.4%.
Embodiment 2
Under the room temperature, be 1L to volume, concentration is the FeCl of 0.6mol/L
3Dripping total amount in the solution is the Na of 0.3mol
2CO
3Solution continues in the dropping process to stir, and is added dropwise to complete the back and continues to stir 2h, and aging then 24h obtains the pillared liquid of iron carbonyl; In 60 ℃ of water-baths, the pillared liquid of Dropwise 5 0mL iron carbonyl in the suspension liquid that contains the 10g calcium-base bentonite, continuously stirring in the dropping process, dropwise the back and stir 3.0h down in 65 ℃ of the same terms, aging 24h under 60 ℃ of constant temperature, centrifugation is with solids deionized water wash 4 times that obtain, the solid that obtains is dried 36h down at 95 ℃, obtains inorganic pillared bentonite; With the inorganic pillared bentonite of gained and 60mL benzene, 20mmol trimethylchlorosilane (Cl
3Si (CH
3)
3) mix, reacted 12 hours, filter, solid product acetone rinsing 3 times, the gained solid was 120 ℃ of vacuum-dryings 36 hours; Add the 50ml deionized water again, feed N
2Stir the protection back, is the KBH of 1mol/L again with 80ml concentration
4Solution adds in the above-mentioned solution, continues to stir 120min; Washed with de-ionized water is used in centrifugation, and 70 ℃ of dry 5h of constant temperature in vacuum drying oven promptly obtain can be used for pollutent absorption and reductive material.The products therefrom interlamellar spacing is 1.45nm.
The 500mL concentration of packing in Brown Glass Brown glass bottles and jars only is the 40mg/L nitrobenzene solution, adds the repair materials for preparing with aforesaid method of 10g again, 25 ℃ of constant temperature vibration 20min, and precipitate and separate is measured the concentration of oil of mirbane in the solution, and clearance is 90.4%.
Embodiment 3
Under the room temperature, be 1L to volume, concentration is the FeCl of 0.6mol/L
3Dripping total amount in the solution is the Na of 0.3mol
2CO
3Solution continues in the dropping process to stir, and is added dropwise to complete the back and continues to stir 2.5h, and aging then 24h obtains the pillared liquid of iron carbonyl; In 60 ℃ of water-baths, the pillared liquid of Dropwise 5 0mL iron carbonyl in the suspension liquid that contains the 10g sodium bentonite, continuously stirring in the dropping process, dropwise the back and stir 2.0h down in 60 ℃ of the same terms, aging 24h under 60 ℃ of constant temperature, centrifugation is with solids deionized water wash 4 times that obtain, the solid that obtains is dried 36h down at 95 ℃, obtains inorganic pillared bentonite; With the inorganic pillared bentonite of gained and 100mL acetone, 20mmol3 aminopropyl-triethoxyl silane ((CH
3CH
2O)
3CH
2SiCH
2CH
2CH
2NH
2) mix, reacted 36 hours, to filter, unreacted silylating reagent and organic solvent are removed in solid product acetone rinsing 3 times, and the gained solid was 90 ℃ of vacuum-dryings 12 hours; Add the 50ml deionized water again, feed N
2Stir the protection back, is the KBH of 1mol/L again with 80ml concentration
4Solution adds in the above-mentioned solution, continues to stir 120min; Washed with de-ionized water is used in centrifugation, and 60 ℃ of dry 5h of constant temperature in vacuum drying oven promptly obtain can be used for pollutent absorption and reductive material.The products therefrom interlamellar spacing is 1.75nm.
The 500mL concentration of packing in Brown Glass Brown glass bottles and jars only is the 40mg/L nitrobenzene solution, adds the repair materials for preparing with aforesaid method of 10g again, 25 ℃ of constant temperature vibration 20min, and precipitate and separate is measured the concentration of oil of mirbane in the solution, and clearance is 94.3%.
Embodiment 4
Under the room temperature, be 1L to volume, concentration is the FeCl of 0.8mol/L
3Dripping total amount in the solution is the Na of 0.4mol
2CO
3Solution continues in the dropping process to stir, and is added dropwise to complete the back and continues to stir 2h, and aging then 24h obtains the pillared liquid of iron carbonyl; In 60 ℃ of water-baths, in the suspension liquid that contains the 10g sodium bentonite, drip the pillared liquid of 100mL iron carbonyl, continuously stirring in the dropping process, dropwise the back and stir 2.0h down in 60 ℃ of the same terms, aging 24h under 60 ℃ of constant temperature, centrifugation is with solids deionized water wash 4 times that obtain, the solid that obtains is dried 36h down at 125 ℃, obtains inorganic pillared bentonite; With the inorganic pillared bentonite of gained and 100mL pyridine, 20mmol benzyl-triethoxyl silane ((CH
3CH
2O)
3SiC
6H
5) mix, reacted 36 hours, filter, solid product acetone rinsing 3 times, the gained solid was 90 ℃ of vacuum-dryings 12 hours; Add the 60ml deionized water again, feed N
2Stir the protection back, is the KBH of 1mol/L again with 80ml concentration
4Solution adds in the above-mentioned solution, continues to stir 120min; Washed with de-ionized water is used in centrifugation, and 70 ℃ of dry 6h of constant temperature in vacuum drying oven promptly obtain can be used for pollutent absorption and reductive material.The products therefrom interlamellar spacing is 1.72nm.
The 500mL concentration of packing in Brown Glass Brown glass bottles and jars only is the 40mg/L nitrobenzene solution, adds the repair materials for preparing with aforesaid method of 8g again, 25 ℃ of constant temperature vibration 20min, and precipitate and separate is measured the concentration of oil of mirbane in the solution, and clearance is 93.4%.
Embodiment 5
Under the room temperature, be 1L to volume, concentration is the FeCl of 0.8mol/L
3Dripping total amount in the solution is the Na of 0.4mol
2CO
3Solution continues in the dropping process to stir, and is added dropwise to complete the back and continues to stir 2.5h, and aging then 24h obtains the pillared liquid of iron carbonyl; In 65 ℃ of water-baths, in the suspension liquid that contains the 10g calcium-base bentonite, drip the pillared liquid of 100mL iron carbonyl, continuously stirring in the dropping process, dropwise the back and stir 2.0h down in 65 ℃ of the same terms, aging 24h under 60 ℃ of constant temperature, centrifugation is with solids deionized water wash 5 times that obtain, the solid that obtains is dried 12h down at 125 ℃, obtains inorganic pillared bentonite; With the inorganic pillared bentonite of gained and 60mL toluene, 20mmol 3-cyanogen propyl group-triethoxyl silane ((CH
3CH
2O)
3SiCH
2CH
2CH
2CN) mix, reacted 36 hours, filter, solid product acetone rinsing 5 times, the gained solid was 120 ℃ of vacuum-dryings 36 hours; Add the 50ml deionized water again, feed N
2Stir the protection back, is the KBH of 1mol/L again with 50～80ml concentration
4Solution adds in the above-mentioned solution, continues to stir 120～240min; Washed with de-ionized water is used in centrifugation, and 60～70 ℃ of drying 5～6h of constant temperature in vacuum drying oven promptly obtain can be used for pollutent absorption and reductive material.The products therefrom interlamellar spacing is 1.75nm.
The 500mL concentration of packing in Brown Glass Brown glass bottles and jars only is the 20mg/L nitrobenzene solution, adds the repair materials for preparing with aforesaid method of 8g again, 25 ℃ of constant temperature vibration 20min, and precipitate and separate is measured the concentration of oil of mirbane in the solution, and clearance is 92.9%.
Embodiment 6
Under the room temperature, be 1L to volume, concentration is the FeCl of 0.8mol/L
3Dripping total amount in the solution is the Na of 0.4mol
2CO
3Solution continues in the dropping process to stir, and is added dropwise to complete the back and continues to stir 2.5h, and aging then 24h obtains the pillared liquid of iron carbonyl; In 65 ℃ of water-baths, in the suspension liquid that contains the 10g calcium-base bentonite, drip the pillared liquid of 100mL iron carbonyl, continuously stirring in the dropping process, dropwise the back and stir 2.0h down in 65 ℃ of the same terms, aging 24h under 60 ℃ of constant temperature, centrifugation is with solids deionized water wash 5 times that obtain, the solid that obtains is dried 12h down at 125 ℃, obtains inorganic pillared bentonite; With the inorganic pillared bentonite of gained and 60mL acetone, 20mmol 3-mercapto propyl group-triethoxyl silane ((CH
3CH
2O)
3SiCH
2CH
2CH
2SH) mix, reacted 36 hours, filter, solid product acetone rinsing 5 times, the gained solid was 120 ℃ of vacuum-dryings 36 hours; Add the 50ml deionized water again, feed N
2Stir the protection back, is the KBH of 1mol/L again with 50～80ml concentration
4Solution adds in the above-mentioned solution, continues to stir 120～240min; Washed with de-ionized water is used in centrifugation, and 60～70 ℃ of drying 5～6h of constant temperature in vacuum drying oven promptly obtain can be used for pollutent absorption and reductive material.The products therefrom interlamellar spacing is 1.77nm.
The 500mL concentration of packing in Brown Glass Brown glass bottles and jars only is the 40mg/L nitrobenzene solution, adds the repair materials for preparing with aforesaid method of 10g again, 25 ℃ of constant temperature vibration 20min, and precipitate and separate is measured the concentration of oil of mirbane in the solution, and clearance is 96.4%.
Claims (3)
1. absorbing and reducing preparation methods is characterized in that in turn including the following steps:
1) under the room temperature, be that 1L, concentration are the FeCl of 0.6～0.8mol/L to volume
3Dripping total amount in the solution is the Na of 0.3～0.4mol
2CO
3Solution continues in the dropping process to stir, and is added dropwise to complete the back and continues to stir 2～2.5h, and aging then 24h obtains the pillared liquid of iron carbonyl;
2) in 60～65 ℃ of water-baths, the pillared liquid of Dropwise 5 0～100mL iron carbonyl in containing the bentonitic suspension liquid of 10g, continuously stirring in the dropping process, dropwise the back and stir 2.0～3.0h down in 60～65 ℃ of the same terms, aging 24h under 60 ℃ of constant temperature, centrifugation is used deionized water wash 4-5 time earlier with resulting solids, dry 12～36h down at 95 ℃～125 ℃ then, obtain inorganic pillared bentonite;
3) the inorganic pillared bentonite of gained is mixed with 60mL～100mL organic solvent and 5mmol～20mmol silylating reagent, reacted 12～36 hours, filter, the gained solid product is used acetone rinsing 3～5 times earlier, again 90 ℃～120 ℃ following vacuum-dryings 12～36 hours;
4) the vacuum-drying after product is added 50～60ml deionized water, feed N
2Stirring into solution after the protection, is the KBH of 1mol/L with 50～80ml concentration
4Solution adds in the above-mentioned solution that stirs into, and continues to stir 120～240min again;
5) the step 4) product is carried out centrifugation, use washed with de-ionized water, 60～70 ℃ of freeze-day with constant temperature 5～6h promptly get the absorbing and reducing material in vacuum drying oven.
2. a kind of absorbing and reducing preparation methods according to claim 1 is characterized in that: the described organic solvent of step 3) is toluene, benzene, acetone or pyridine, and described silylating reagent is that chemical structure of general formula is R
N-Si-X
4-NOrganosilane, wherein, N=1～3; R comprises that carbonatoms is that 1～18 alkyl, phenyl and carbonatoms are the organic group of 1～18 amino, cyano group, sulfydryl, chlorine substituted alkyl; X is the hydrolyzable part that comprises halogen, amino, methoxyl group, oxyethyl group.
3. a kind of absorbing and reducing preparation methods according to claim 1 is characterized in that: step 2) described wilkinite is sodium bentonite or calcium-base bentonite.
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|---|---|---|---|
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ID=43388708
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102895942A (en) * | 2012-09-07 | 2013-01-30 | 常州大学 | Method for synthesizing iron modified bentonite |
| CN103785855A (en) * | 2014-02-10 | 2014-05-14 | 上海市环境科学研究院 | Method for preparing multi-component organically-modified bentonite-embedded nanoscale zero-valent iron |
| CN105110424A (en) * | 2015-08-18 | 2015-12-02 | 昆明理工大学 | Preparation method for floatable nano mesoporous zero-valent iron carbon material |
| CN105290099A (en) * | 2014-11-07 | 2016-02-03 | 上海市环境科学研究院 | Preparing method and use method of chlorinated organic compound polluted soil repairing agent |
| CN106076321A (en) * | 2016-06-12 | 2016-11-09 | 常州大学 | A kind of combined oxidation manganese preparation method for processing organic exhaust gas |
| CN106076310A (en) * | 2016-06-12 | 2016-11-09 | 常州大学 | A kind of preparation method of the load-type zirconium oxide for processing waste gas |
Citations (1)
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|---|---|---|---|---|
| CN100429146C (en) * | 2006-11-27 | 2008-10-29 | 浙江大学 | Method for synthesizing composite material of organic - inorganic bentonite |
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2010
- 2010-08-25 CN CN 201010262289 patent/CN101935101A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100429146C (en) * | 2006-11-27 | 2008-10-29 | 浙江大学 | Method for synthesizing composite material of organic - inorganic bentonite |
Non-Patent Citations (2)
| Title |
|---|
| 《北京化工大学学报（自然科学版）》 20091231 张莉等 纳米铁/粘土杂化材料的制备与表征 1-3 第36卷, 2 * |
| 《矿物岩石地球化学通报》 20070430 袁鹏等 铁盐水解法制备铁层柱蒙脱石及其结构特性研究 1-3 第26卷, 第2期 2 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102895942A (en) * | 2012-09-07 | 2013-01-30 | 常州大学 | Method for synthesizing iron modified bentonite |
| CN102895942B (en) * | 2012-09-07 | 2014-10-29 | 常州大学 | Method for synthesizing iron modified bentonite |
| CN103785855A (en) * | 2014-02-10 | 2014-05-14 | 上海市环境科学研究院 | Method for preparing multi-component organically-modified bentonite-embedded nanoscale zero-valent iron |
| CN105290099A (en) * | 2014-11-07 | 2016-02-03 | 上海市环境科学研究院 | Preparing method and use method of chlorinated organic compound polluted soil repairing agent |
| CN105110424A (en) * | 2015-08-18 | 2015-12-02 | 昆明理工大学 | Preparation method for floatable nano mesoporous zero-valent iron carbon material |
| CN106076321A (en) * | 2016-06-12 | 2016-11-09 | 常州大学 | A kind of combined oxidation manganese preparation method for processing organic exhaust gas |
| CN106076310A (en) * | 2016-06-12 | 2016-11-09 | 常州大学 | A kind of preparation method of the load-type zirconium oxide for processing waste gas |
| CN106076310B (en) * | 2016-06-12 | 2019-01-25 | 常州大学 | It is a kind of for handling the preparation method of the load-type zirconium oxide of exhaust gas |
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