CN103007907A - Preparation method of high-efficiency quantitative supported nano iron - Google Patents
Preparation method of high-efficiency quantitative supported nano iron Download PDFInfo
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- CN103007907A CN103007907A CN2012105641737A CN201210564173A CN103007907A CN 103007907 A CN103007907 A CN 103007907A CN 2012105641737 A CN2012105641737 A CN 2012105641737A CN 201210564173 A CN201210564173 A CN 201210564173A CN 103007907 A CN103007907 A CN 103007907A
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Abstract
The invention discloses a preparation method of high-efficiency quantitative supported nano iron. The method comprises the steps of placing a carrier into a crucible, dripping a ferric iron solution to the surface of the carrier to be colloid according to a required mass fraction of the nano iron, stopping dripping, baking, continuing to drip the ferric iron solution into a dried substance, baking after the carrier is mixed with the dripped ferric iron solution to be colloid, repeating until all the ferric iron solution for calculation is dripped into the carrier, placing a colloid substance obtained from the final step into an oven for drying, taking the carrier out, placing the carrier into a conical flask, dripping excessive sodium borohydride solution, conducting vacuum filtering on solid after quiescent sedimentation after reaction completion, and transferring the filtered solid (namely the supported nano iron) into an alcoholic solution or a closed container for preservation. The preparation method can control the mass fraction of nano iron in the final solid, can allow the nano iron to be dispersed better on the carrier, improves utilization efficiency of raw materials, facilitates subsequent application, and greatly increases a utilization ratio of nano iron.
Description
Technical field
The present invention relates to the preparation method that nano-functional material loads on the bulky grain carrier, can be applied to the fields such as environment, chemical industry, relate in particular to a kind of efficient quantitatively preparation method of loaded with nano-iron.
Background technology
Nanoscale Iron is to use in the last few years very extensively at environmental area, and it is with its higher specific area, more avtive spot, and stronger reproducibility becomes gradually and removes the focus that the environmental area pollutant is paid close attention to.In the last few years, people had carried out a large amount of research to Nanoscale Iron removal environmental area pollutant.Through studies show that Nanoscale Iron is for heavy metal contaminants, organic pollution, especially persistent organic pollutants have stronger removal ability.
The shortcomings such as although the nanometer body has lot of advantages, it also has some shortcomings, limits its application in reality, and for example Nanoscale Iron is reunited in storage process easily, and is easy oxidized.Nanoscale Iron form after reuniting is tending towards a micron attitude, has lost gradually Nanoscale Iron advantage originally so that the Nanoscale Iron after reuniting in actual applications effect greatly reduce.
In order to improve the practical application effect of Nanoscale Iron, Nanoscale Iron need to be loaded on the relevant carrier.There are some researches show that the Nanoscale Iron degree of scatter that loads on the carrier is better, improved to a certain extent service life and the efficient of Nanoscale Iron simultaneously.The method of conventional load Nanoscale Iron only simply is placed on carrier in the ferric iron solution and mixes, to be mixed evenly after, slowly splash into sodium borohydride solution, reaction generates Nanoscale Iron gradually, the Nanoscale Iron that generates simultaneously can automatic load to carrier.But this preparation method's shortcoming is a lot, content that for example can not the control load Nanoscale Iron, simultaneously before carrier longer with ferric iron solution incorporation time, a large amount of Nanoscale Irons that generate are wasted in the course of reaction, can not load on the carrier.Drawbacks limit the method application in practice that this is all.How quantitatively loaded with nano-iron shortens preparation time simultaneously, improves the Nanoscale Iron utilization ratio, is the difficult problem that needs to be resolved hurrily of preparation loaded with nano-iron.If can be efficient, and can quantitatively prepare the sorbing material of loaded with nano-iron, for the practical application of Nanoscale Iron at environmental area, even through engineering approaches is used very important effect is arranged.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of efficient quantitatively preparation method of loaded with nano-iron, can control nanometer iron content in the final solid, preparation technology is simple, and speed is fast.
In order to achieve the above object, the technical solution used in the present invention is:
A kind of efficient quantitatively preparation method of loaded with nano-iron comprises the steps:
Step 1, compound concentration is the ferric iron solution of 0.5mol/L, in crucible, place the 500mg carrier, Nanoscale Iron mass fraction according to demand, calculate the consumption that will splash into altogether ferric iron solution, ferric iron solution packed into drops to carrier surface in the dropper, splashes in the process and constantly stirs, and makes it even;
Step 2 after carrier and the ferric iron solution that is dripped are mixed to glue, stops to splash into, and colloid substance is put into 70 ℃ of baking ovens, baking 10 ~ 15min;
Step 3 continues to splash into ferric iron solution in the material after the oven dry, splashes in the process constantly and stirs, make it evenly, and after carrier and the ferric iron solution that is dripped are mixed to glue, repeating step two;
Step 4, repeating step three and step 2 all splash into carrier until calculate the ferric iron solution of consumption, and the colloid substance of final step is put into 70 ℃ of bakings of baking oven, 20 ~ 25min, make its drying;
Step 5 is taken out carrier, and carrier is put into the 200ml conical flask, splashes into the sodium borohydride solution that concentration is 1mol/L, and dripping speed is 30 droplets/minute, and whole process passes into nitrogen continuously in conical flask, and keeps stirring;
Step 6 adds excessive sodium borohydride solution, after question response finishes, and static 2 hours, the solid vacuum filtration after the quiescent setting, the suction filtration time is 12 hours;
Solid after the step 7, suction filtration is loaded with nano-iron, transfers them in alcoholic solution or the closed container and preserves.
Wherein, described ferric iron solution can be FeCl
3Solution or Fe
2(SO
4)
3Solution, also available ferrous iron solution preparation, for example FeCl
2Solution or FeSO
4Solution.
Described carrier can be active carbon, activated alumina, diatomite or molecular sieve.
Described loaded with nano-iron macroscopic view is Powdered, and microstructure is that Nanoscale Iron is spot distribution at carrier surface, and grain diameter is about 20nm, and described Nanoscale Iron mass fraction is 10%, and the total amount that need to splash into ferric iron solution is 2ml, divides to drip off for 2 times.
Described loaded with nano-iron macroscopic view is black powder, and microstructure is that Nanoscale Iron is spot distribution at carrier surface, and grain diameter is about 30 ~ 40nm, and described Nanoscale Iron mass fraction is 20%, and the total amount that need to splash into ferric iron solution is 4.5ml, divides to drip off for 3 ~ 4 times.
Described loaded with nano-iron macroscopic view is powder, microstructure be the chain solid supported on carrier, grain diameter is 80 ~ 100nm, described Nanoscale Iron mass fraction is 40%, the total amount that need to splash into ferric iron solution is 12ml, drips off minutes for 10 ~ 12 times.
Compared with prior art, the present invention has the following advantages:
1) the present invention can control nanometer iron content in the final solid, is convenient to follow-up application.
2) the present invention is high for the utilization rate of Nanoscale Iron, greatly alleviates wasting of resources phenomenon.
3) the present invention prepares the material cycle weak point of loaded with nano-iron, and speed is fast.
Description of drawings
Fig. 1 is activated carbon supported 20% Nanoscale Iron new material scanning electron microscope (SEM) photograph.
Fig. 2 is tripolite loading 20% Nanoscale Iron new material scanning electron microscope (SEM) photograph.
Fig. 3 is activated alumina load 20% Nanoscale Iron new material scanning electron microscope (SEM) photograph.
Fig. 4 is molecular sieve carried 20% Nanoscale Iron new material scanning electron microscope (SEM) photograph.
The specific embodiment
Below in conjunction with drawings and Examples the present invention is described in further details.
Embodiment 1: the preparation of activated carbon supported 20% Nanoscale Iron
Preparation 0.5mol/L ferric iron solution is placed the 500mg active carbon in crucible, ferric iron solution is packed in the dropper, uses dropper slowly solution to be dripped to carrier surface, in splashing into process, constantly stirs, and makes it even.
After carrier and solution are mixed to glue, no longer splash into solution, colloid substance is put into 70 ℃ of baking ovens, toasted 12 minutes, colloid substance is dried substantially (not dry especially).
Slowly splash into ferric iron solution in the carrier of continuation after the oven dry, splash in the process constantly and stir, make it even.After carrier and solution are mixed to glue, repeating step two.
Ferric iron solution total amount to be dripped is put into baking oven with colloid substance and is dried by the fire 20min after 4.5ml, makes its drying.
Take out carrier, carrier is put into the 200ml conical flask, preparation 1mol/L sodium borohydride solution constantly splashes in the conical flask, and dripping speed is 30 droplets/minute, and whole process passes into nitrogen continuously in conical flask, and keeps stirring.
Add excessive sodium borohydride solution, after question response finishes, static conical flask 2 hours.The rapid vacuum filtration of solid after the quiescent setting, the suction filtration time is 12 hours.
Solid transfer after the suction filtration is preserved to alcoholic solution.The product that obtains is activated carbon supported Nanoscale Iron sorbing material.
Embodiment 2: the preparation of tripolite loading 20% Nanoscale Iron
Preparation 0.5mol/L ferric iron solution is placed 500mg diatomite in crucible, ferric iron solution is packed in the dropper, uses dropper slowly solution to be dripped to carrier surface, in splashing into process, constantly stirs, and makes it even.
After carrier and solution are mixed to glue, no longer splash into solution, colloid substance is put into 70 ℃ of baking ovens, toasted 15 minutes, colloid substance is dried substantially (not dry especially).
Slowly splash into ferric iron solution in the carrier of continuation after the oven dry, splash in the process constantly and stir, make it even.After carrier and solution are mixed to glue, repeating step two.
Ferric iron solution total amount to be dripped is put into baking oven baking 20min with colloid substance and is made its drying after 4.5ml.
Take out carrier, carrier is put into the 200ml conical flask, preparation 1mol/L sodium borohydride solution constantly splashes in the conical flask, and dripping speed is 30 droplets/minute, and whole process passes into nitrogen continuously in conical flask, and keeps stirring.
Add excessive sodium borohydride solution, after question response finishes, static conical flask 2 hours.The rapid vacuum filtration of solid after the quiescent setting, the suction filtration time is 12 hours.
Solid transfer after the suction filtration is preserved to alcoholic solution.The product that obtains is tripolite loading nano iron sorbing material.
Embodiment 3: the preparation of activated alumina load 20% Nanoscale Iron
Preparation 0.5mol/L ferric iron solution is placed the 500mg activated alumina in crucible, ferric iron solution is packed in the dropper, uses dropper slowly solution to be dripped to carrier surface, in splashing into process, constantly stirs, and makes it even.
After carrier and solution are mixed to glue, no longer splash into solution, colloid substance is put into 70 ℃ of baking ovens, toasted 14 minutes, colloid substance is dried substantially (not dry especially).
Slowly splash into ferric iron solution in the carrier of continuation after the oven dry, splash in the process constantly and stir, make it even.After carrier and solution are mixed to glue, repeating step two.
Ferric iron solution total amount to be dripped is put into baking oven baking 20min with colloid substance and is made its drying after 4.5ml.
Take out carrier, carrier is put into the 200ml conical flask, preparation 1mol/L sodium borohydride solution constantly splashes in the conical flask, and dripping speed is 30 droplets/minute, and whole process passes into nitrogen continuously in conical flask, and keeps stirring.
Add excessive sodium borohydride solution, after question response finishes, static conical flask 2 hours.The rapid vacuum filtration of solid after the quiescent setting, the suction filtration time is 12 hours.
Solid transfer after the suction filtration is preserved to alcoholic solution.The product that obtains is activated alumina loaded with nano-iron sorbing material.
Embodiment 4: the preparation of molecular sieve carried 20% Nanoscale Iron
Preparation 0.5mol/L ferric iron solution is placed the 500mg molecular sieve in crucible, ferric iron solution is packed in the dropper, uses dropper slowly solution to be dripped to carrier surface, in splashing into process, constantly stirs, and makes it even.
After carrier and solution are mixed to glue, no longer splash into solution, colloid substance is put into 70 ℃ of baking ovens, toasted 10 minutes, colloid substance is dried substantially (not dry especially).
Slowly splash into ferric iron solution in the carrier of continuation after the oven dry, splash in the process constantly and stir, make it even.After carrier and solution are mixed to glue, repeating step two-step 3 3～4 times.
Ferric iron solution total amount to be dripped is put into baking oven baking 20min with colloid substance and is made its drying after 4.5ml.
Take out carrier, carrier is put into the 200ml conical flask, preparation 1mol/L sodium borohydride solution constantly splashes in the conical flask, and dripping speed is 30 droplets/minute, and whole process passes into nitrogen continuously in conical flask, and keeps stirring.
Add excessive sodium borohydride solution, after question response finishes, static conical flask 2 hours.The rapid vacuum filtration of solid after the quiescent setting, the suction filtration time is 12 hours.
Solid transfer after the suction filtration is preserved to alcoholic solution.The product that obtains is molecular sieve carried Nanoscale Iron sorbing material.
Gained loaded with nano-iron macroscopic view is black powder, and microstructure is that Nanoscale Iron is spot distribution at carrier surface, and grain diameter is about 30 ~ 40nm.
Among the embodiment 1 ~ 4, ferric iron solution can be selected FeCl3 solution or Fe2 (SO4) 3 solution.
Embodiment 5:
Difference from Example 4 is:
Prepare molecular sieve carried 10% Nanoscale Iron, the total amount that need to splash into ferric iron solution is 2ml, divides to drip off for 2 times.Preparation gained loaded with nano-iron macroscopic view is Powdered, and microstructure is that Nanoscale Iron is spot distribution at carrier surface, and grain diameter is about 20nm.
Embodiment 6:
Difference from Example 4 is:
Prepare molecular sieve carried 40% Nanoscale Iron, the total amount that need to splash into ferric iron solution is 12ml, divides to drip off for 10 ~ 12 times.Preparation gained loaded with nano-iron macroscopic view is powder, microstructure be the chain solid supported on carrier, grain diameter is 80 ~ 100nm.
Embodiment 7:
Difference from Example 4 is:
Prepare molecular sieve carried 20% Nanoscale Iron, the total amount that need to splash into ferrous iron solution is 4.5ml, divides to drip off for 3 ~ 4 times.Described loaded with nano-iron macroscopic view is black powder, and microstructure is that Nanoscale Iron is spot distribution at carrier surface, and grain diameter is about 30 ~ 40nm.
Ferrous iron solution among the embodiment 7 can be selected FeCl
2Solution or FeSO
4Solution.
Can find out from Fig. 1 ~ Fig. 4 don't work loads to Nanoscale Iron on which kind of carrier, nano iron particles distributes all very even, and nano iron particles does not have agglomeration simultaneously, and particle is all very little.
Claims (8)
1. the efficient quantitatively preparation method of loaded with nano-iron comprises the steps:
Step 1, compound concentration is the ferric iron solution of 0.5mol/L, in crucible, place the 500mg carrier, Nanoscale Iron mass fraction according to demand, calculate the consumption that will splash into altogether ferric iron solution, ferric iron solution packed into drops to carrier surface in the dropper, splashes in the process and constantly stirs, and makes it even;
Step 2 after carrier and the ferric iron solution that is dripped are mixed to glue, stops to splash into, and colloid substance is put into 70 ℃ of baking ovens, baking 10 ~ 15min;
Step 3 continues to splash into ferric iron solution in the material after the oven dry, splashes in the process constantly and stirs, make it evenly, and after carrier and the ferric iron solution that is dripped are mixed to glue, repeating step two;
Step 4, repeating step three and step 2 all splash into carrier until calculate the ferric iron solution of consumption, and the colloid substance of final step is put into 70 ℃ of bakings of baking oven, 20 ~ 25min, make its drying;
Step 5 is taken out carrier, and carrier is put into the 200ml conical flask, splashes into the sodium borohydride solution that concentration is 1mol/L, and dripping speed is 30 droplets/minute, and whole process passes into nitrogen continuously in conical flask, and keeps stirring;
Step 6 adds excessive sodium borohydride solution, after question response finishes, and static 2 hours, the solid vacuum filtration after the quiescent setting, the suction filtration time is 12 hours;
Solid after the step 7, suction filtration is loaded with nano-iron, transfers them in alcoholic solution or the closed container and preserves.
2. a kind of efficient quantitatively preparation method of loaded with nano-iron according to claim 1 is characterized in that the ferrous iron solution take concentration as 0.5mol/L substitutes described ferric iron solution.
3. a kind of efficient quantitatively preparation method of loaded with nano-iron according to claim 2 is characterized in that described ferrous iron solution is FeCl
2Solution or FeSO
4Solution.
4. a kind of efficient quantitatively preparation method of loaded with nano-iron according to claim 1 and 2 is characterized in that described ferric iron solution is FeCl
3Solution or Fe
2(SO
4)
3Solution.
5. a kind of efficient quantitatively preparation method of loaded with nano-iron according to claim 1 is characterized in that described carrier is active carbon, activated alumina, diatomite or molecular sieve.
6. a kind of efficient quantitatively preparation method of loaded with nano-iron according to claim 1, it is characterized in that, described loaded with nano-iron macroscopic view is Powdered, microstructure is that Nanoscale Iron is spot distribution at carrier surface, grain diameter is about 20nm, described Nanoscale Iron mass fraction is 10%, and the total amount that need to splash into ferric iron solution is 2ml, divides to drip off for 2 times.
7. a kind of efficient quantitatively preparation method of loaded with nano-iron according to claim 1, it is characterized in that, described loaded with nano-iron macroscopic view is black powder, microstructure is that Nanoscale Iron is spot distribution at carrier surface, grain diameter is about 30 ~ 40nm, described Nanoscale Iron mass fraction is 20%, and the total amount that need to splash into ferric iron solution is 4.5ml, divides to drip off for 3 ~ 4 times.
8. a kind of efficient quantitatively preparation method of loaded with nano-iron according to claim 1, it is characterized in that, described loaded with nano-iron macroscopic view is powder, microstructure is that the chain solid supported is on carrier, grain diameter is 80 ~ 100nm, described Nanoscale Iron mass fraction is 40%, and the total amount that need to splash into ferric iron solution is 12ml, divides to drip off for 10 ~ 12 times.
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| CN111252845A (en) * | 2020-02-24 | 2020-06-09 | 广东工业大学 | Novel catalysis-adsorption material and preparation method and application thereof |
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