CN101993868A - Embedded nano iron/microbe microspheres and preparation method thereof - Google Patents
Embedded nano iron/microbe microspheres and preparation method thereof Download PDFInfo
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- CN101993868A CN101993868A CN2010102974715A CN201010297471A CN101993868A CN 101993868 A CN101993868 A CN 101993868A CN 2010102974715 A CN2010102974715 A CN 2010102974715A CN 201010297471 A CN201010297471 A CN 201010297471A CN 101993868 A CN101993868 A CN 101993868A
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Abstract
The invention relates to embedded nano iron/microbe microspheres and a preparation method thereof. The embedded nano iron/microbe microspheres are formed under the gelation action of calcium alginate. An embedding method is adopted in the prepared nano iron/microbial microspheres; nano iron and microbe are immobilized in the microspheres together by using the cross-linking and curing effects of a sodium alginate embedding agent and a calcium chloride cross linker; and the prepared microspheres have uniform particle size distribution, small average particle size and large specific surface area, and can be widely applied in the fields of environmental pollution treatment and environmental remediation.
Description
Technical field
The present invention relates to field of nanometer technology, especially a kind of embedding type nanometer iron/microbe microsphere and preparation method thereof.
Background technology
Microorganism has been widely used in the groundwater pollutant reparation at present.According to its electron donor difference, mainly be divided into heterotrophic microorganism and autotrophic microorganism, wherein heterotrophic microorganism has been limited its application in underground water is repaired for organic dependence, and autotrophic microorganism utilizes H usually
2As electron donor, but H
2Inflammable and explosive characteristic has also been brought difficulty to practical application.Therefore by adding the intensive treatment measure, molten iron corrosion product hydrogen can be autotrophic microorganism provides enough electron donors, under both synergies, accelerates contaminant degradation.In recent years, nanometer iron relies on its higher specific surface area and reactive behavior, has shown great application prospect in the groundwater pollutant reparation.
But existing state of the art only rests on nanometer iron and microorganism are carried out the simple physical mix stages, although also obtaining some achievements aspect the removal pollutent, but the synergy of nanometer iron and microorganism and not obvious in the whole process, cause finally occur microbially stable poor, easily run off, easily inactivation and microorganism and the effective contact rate of nanometer iron are not high, problems such as reaction efficiency is lower are difficult to be applied in the original position reparation of actual pollutent.
At above problem, the present invention utilizes chemical means, nanometer iron and microorganism are carried out the processing of embedding vesiculation, microorganism and nanometer iron are embedded in the same microballoon environment, make that their synergistic effects in contaminant removal process are more obvious, also can guarantee the stable and active of microorganism simultaneously; Adhere to because the nanometer iron stability after the finishing strengthens and is easy to contact with microorganism, improved their contact rate, accelerated the speed of its Synergistic degradation pollutent.These microballoons of Xing Chenging are fit to the original position reparation more in view of freely being suspended in the polluted-water in addition, also easily by filtering or utilizing its magnetic to reclaim, reduce secondary pollution from water surrounding.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of embedding type nanometer iron/microbe microsphere and preparation method thereof is provided, this method required equipment is simple, easy to operate, and prepared product performance are superior.
The present invention is achieved through the following technical solutions:
A kind of embedding type nanometer iron/microbe microsphere, this embedding type nanometer iron/microbe microsphere is the crosslinking curing effect by sodium alginate and calcium chloride, makes nanometer iron and microorganism fixing jointly in microballoon.
The preparation method of embedding type nanometer iron/microbe microsphere may further comprise the steps:
(1) preparation of embedding medium sodium alginate soln
With the sodium alginate particle vitreous state that is heated to soluble in water, obtain the sodium alginate soln that the quality percentage composition is 1-6%;
(2) preparation of linking agent calcium chloride solution
The calcium chloride powder is soluble in water, obtain the calcium chloride solution that volumetric molar concentration is 0.1-1mol/L;
(3) preparation of nanometer ferrous solution
Adopt liquid phase reduction, strong reductant KBH
4Reduction FeSO
47H
2O obtains Fe
0, use Fe
0The preparation volumetric molar concentration is the nanometer ferrous solution of 0.1-0.6g/L;
(4) preparation of reaction solution A
Add bacterium liquid and sodium alginate soln in the nanometer ferrous solution, volume ratio is 2: 3: 5, and mechanical stirring 8-15min obtains reaction solution A so that mix fully then;
(5) preparation of reaction solution B
Add sodium alginate soln in calcium chloride solution, its volume ratio is 1: 3-5: 1;
(6) preparation of reaction system
Reaction solution A slowly is directed among the reaction solution B by vacuum line, and the continuous stirred solution B of whole process makes its sufficient reacting, the volume ratio of reaction solution A and reaction solution B is 1: 1-1: 4, after importing end, continue ageing 30-60min, obtain embedding type nanometer iron/microbe microsphere;
(7) after reaction finishes,, preserve with deoxidation deionized water repetitive scrubbing embedding type nanometer iron/microbe microsphere.
And described embedding type nanometer iron/microbe microsphere store method is meant in stroke-physiological saline solution and soaks and place in the refrigerator 4 ℃ and preserve down.
Advantage of the present invention and beneficial effect are:
1. the selected embedding medium sodium alginate of the present invention is that a kind of natural biological macromolecular material is not only cheap and easy to get, and nontoxic, has excellent biological compatibility, can be widely used in environmental pollution treatment and environment remediation field.
2. the present invention is by the crosslinking curing effect of sodium alginate and calcium chloride, can realize that the immobilization in the lump of nanometer iron and microorganism handles, and obtained microspherulite diameter is evenly distributed, median size is little, specific surface area is big, can be widely used in environmental pollution treatment and environment remediation field.
3. equipment required for the present invention is simple, easy to operate, and reaction is finished at normal temperatures and pressures, and product is a solid phase, and reaction system is a liquid phase, and therefore the product separate easily, is applicable to large-scale commercial production.
Description of drawings
Fig. 1 is preparation flow figure of the present invention;
Fig. 2 is the pictorial diagram of the embedding type nanometer iron/microbe microsphere of the present invention's preparation.
Embodiment
The present invention is described in further detail in conjunction with the accompanying drawings by following examples, but the technology contents that present embodiment is narrated is illustrative, rather than determinate, should not limit to protection scope of the present invention according to this.
A kind of embedding type nanometer iron/microbe microsphere, this embedding type nanometer iron/microbe microsphere is the crosslinking curing effect by sodium alginate and calcium chloride, makes nanometer iron and microorganism fix (as shown in Figure 2) jointly in microballoon; The selected microorganism of present embodiment is alcaligenes eutrophus (Alcaligenes eutrophus), its OD
420=0.0229.Kind of selected microorganism and concrete concentration also can carry out specifically determining according to target contaminant in addition.
Preparation method's (as shown in Figure 1) embodiment that states specific as follows of this embedding type nanometer iron/microbe microsphere:
Embodiment 1:
(1) preparation of embedding medium sodium alginate soln
With the sodium alginate particle vitreous state that is heated to soluble in water, obtain the quality percentage composition and be 2% sodium alginate soln;
(2) preparation of linking agent calcium chloride solution
The calcium chloride powder is soluble in water, obtain the calcium chloride solution that volumetric molar concentration is 0.2mol/L;
(3) preparation of nanometer ferrous solution
Adopt liquid phase reduction, strong reductant KBH
4Reduction FeSO
47H
2O obtains Fe
0, use Fe
0The preparation volumetric molar concentration is the nanometer ferrous solution of 0.1g/L;
(4) preparation of reaction solution A
Add bacterium liquid and sodium alginate soln in the nanometer ferrous solution, volume ratio is 2: 3: 5, and mechanical stirring 10min obtains reaction solution A so that mix fully then;
(5) preparation of reaction solution B
Add sodium alginate soln in calcium chloride solution, its volume ratio is 2: 1;
(6) preparation of reaction system
Reaction solution A slowly is directed among the reaction solution B by vacuum line, the continuous stirred solution B of whole process, make its sufficient reacting, the volume ratio of reaction solution A and reaction solution B is 1: 1, after importing end, continue ageing 40min, obtain embedding type nanometer iron/microbe microsphere, this microballoon can be used for the original position reparation of nitrate nitrogen, perchlorate contaminated water body;
(7) after the reaction end, with deoxidation deionized water repetitive scrubbing embedding type nanometer iron/microbe microsphere, 4 ℃ of preservations down in immersion and the placement refrigerator in stroke-physiological saline solution.
Embodiment 2:
(1) preparation of embedding medium sodium alginate soln
With the sodium alginate particle vitreous state that is heated to soluble in water, obtain the quality percentage composition and be 3.5% sodium alginate soln;
(2) preparation of linking agent calcium chloride solution
The calcium chloride powder is soluble in water, obtain the calcium chloride solution that volumetric molar concentration is 0.15mol/L;
(3) preparation of nanometer ferrous solution
Adopt liquid phase reduction, strong reductant KBH
4Reduction FeSO
47H
2O obtains Fe
0, use Fe
0The preparation volumetric molar concentration is the nanometer ferrous solution of 0.3g/L;
(4) preparation of reaction solution A
Add bacterium liquid and sodium alginate soln in the nanometer ferrous solution, volume ratio is 2: 3: 5, and mechanical stirring 15min obtains reaction solution A so that mix fully then;
(5) preparation of reaction solution B
Add sodium alginate soln in calcium chloride solution, its volume ratio is 4: 1;
(6) preparation of reaction system
Reaction solution A slowly is directed among the reaction solution B by vacuum line, the continuous stirred solution B of whole process, make its sufficient reacting, the volume ratio of reaction solution A and reaction solution B is 1: 2, after importing end, continue ageing 50min, obtain embedding type nanometer iron/microbe microsphere, this microballoon can be used for the original position reparation of nitrate nitrogen, perchlorate contaminated water body;
(7) after the reaction end, with deoxidation deionized water repetitive scrubbing embedding type nanometer iron/microbe microsphere, 4 ℃ of preservations down in immersion and the placement refrigerator in stroke-physiological saline solution.
Embodiment 3:
(1) preparation of embedding medium sodium alginate soln
With the sodium alginate particle vitreous state that is heated to soluble in water, obtain the quality percentage composition and be 1.5% sodium alginate soln;
(2) preparation of linking agent calcium chloride solution
The calcium chloride powder is soluble in water, obtain the calcium chloride solution that volumetric molar concentration is 0.3mol/L;
(3) preparation of nanometer ferrous solution
Adopt liquid phase reduction, strong reductant KBH
4Reduction FeSO
47H
2O obtains Fe
0, use Fe
0The preparation volumetric molar concentration is the nanometer ferrous solution of 0.1g/L;
(4) preparation of reaction solution A
Add bacterium liquid and sodium alginate soln in the nanometer ferrous solution, volume ratio is 2: 3: 5, and mechanical stirring 8min obtains reaction solution A so that mix fully then;
(5) preparation of reaction solution B
Add sodium alginate soln in calcium chloride solution, its volume ratio is 1: 1;
(6) preparation of reaction system
Reaction solution A slowly is directed among the reaction solution B by vacuum line, the continuous stirred solution B of whole process, make its sufficient reacting, the volume ratio of reaction solution A and reaction solution B is 1: 3, after importing end, continue ageing 30min, obtain embedding type nanometer iron/microbe microsphere, this microballoon can be used for the original position reparation of nitrate nitrogen, perchlorate contaminated water body;
(7) after the reaction end, with deoxidation deionized water repetitive scrubbing embedding type nanometer iron/microbe microsphere, 4 ℃ of preservations down in immersion and the placement refrigerator in stroke-physiological saline solution.
Embodiment 4:
(1) preparation of embedding medium sodium alginate soln
With the sodium alginate particle vitreous state that is heated to soluble in water, obtain the quality percentage composition and be 6% sodium alginate soln;
(2) preparation of linking agent calcium chloride solution
The calcium chloride powder is soluble in water, obtain the calcium chloride solution that volumetric molar concentration is 1mol/L;
(3) preparation of nanometer ferrous solution
Adopt liquid phase reduction, strong reductant KBH
4Reduction FeSO
47H
2O obtains Fe
0, use Fe
0The preparation volumetric molar concentration is the nanometer ferrous solution of 0.6g/L;
(4) preparation of reaction solution A
Add bacterium liquid and sodium alginate soln in the nanometer ferrous solution, volume ratio is 2: 3: 5, and mechanical stirring 12min obtains reaction solution A so that mix fully then;
(5) preparation of reaction solution B
Add sodium alginate soln in calcium chloride solution, its volume ratio is 5: 1;
(6) preparation of reaction system
Reaction solution A slowly is directed among the reaction solution B by vacuum line, the continuous stirred solution B of whole process, make its sufficient reacting, the volume ratio of reaction solution A and reaction solution B is 1: 4, after importing end, continue ageing 60min, obtain embedding type nanometer iron/microbe microsphere, this microballoon can be used for the original position reparation of nitrate nitrogen, perchlorate contaminated water body;
(7) after the reaction end, with deoxidation deionized water repetitive scrubbing embedding type nanometer iron/microbe microsphere, 4 ℃ of preservations down in immersion and the placement refrigerator in stroke-physiological saline solution.
Claims (3)
1. embedding type nanometer iron/microbe microsphere, it is characterized in that: this embedding type nanometer iron/microbe microsphere is the crosslinking curing effect by sodium alginate and calcium chloride, makes nanometer iron and microorganism fixing jointly in microballoon.
2. the preparation method of an embedding type nanometer iron/microbe microsphere as claimed in claim 1, it is characterized in that: this preparation method may further comprise the steps:
(1) preparation of embedding medium sodium alginate soln
With the sodium alginate particle vitreous state that is heated to soluble in water, obtain the sodium alginate soln that the quality percentage composition is 1-6%;
(2) preparation of linking agent calcium chloride solution
The calcium chloride powder is soluble in water, obtain the calcium chloride solution that volumetric molar concentration is 0.1-1mol/L;
(3) preparation of nanometer ferrous solution
Adopt liquid phase reduction, strong reductant KBH
4Reduction FeSO
47H
2O obtains Fe
0, use Fe
0The preparation volumetric molar concentration is the nanometer ferrous solution of 0.1-0.6g/L;
(4) preparation of reaction solution A
Add bacterium liquid and sodium alginate soln in the nanometer ferrous solution, volume ratio is 2: 3: 5, and mechanical stirring 8-15min obtains reaction solution A so that mix fully then;
(5) preparation of reaction solution B
Add sodium alginate soln in calcium chloride solution, its volume ratio is 1: 3-5: 1;
(6) preparation of reaction system
Reaction solution A slowly is directed among the reaction solution B by vacuum line, and the continuous stirred solution B of whole process makes its sufficient reacting, the volume ratio of reaction solution A and reaction solution B is 1: 1-1: 4, after importing end, continue ageing 30-60min, obtain embedding type nanometer iron/microbe microsphere;
(7) after reaction finishes,, preserve with deoxidation deionized water repetitive scrubbing embedding type nanometer iron/microbe microsphere.
3. the preparation method of embedding type nanometer iron/microbe microsphere according to claim 2 is characterized in that: described embedding type nanometer iron/microbe microsphere store method is meant in stroke-physiological saline solution and soaks and place in the refrigerator 4 ℃ and preserve down.
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| CN103157413A (en) * | 2013-03-28 | 2013-06-19 | 湖南农业大学 | Method for preparing sodium alginate microcapsule-supported nanoscale zero-valent iron particles |
| CN103803704A (en) * | 2014-03-03 | 2014-05-21 | 中国环境科学研究院 | Permeable reaction medium material for nitrate pollution of underground water |
| CN104439270A (en) * | 2014-09-04 | 2015-03-25 | 河南城建学院 | Method for preparing sodium alginate/beta-cyclodextrin collaborative immobilized nanometer zero-valent iron |
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| CN103157413A (en) * | 2013-03-28 | 2013-06-19 | 湖南农业大学 | Method for preparing sodium alginate microcapsule-supported nanoscale zero-valent iron particles |
| CN103803704A (en) * | 2014-03-03 | 2014-05-21 | 中国环境科学研究院 | Permeable reaction medium material for nitrate pollution of underground water |
| CN103803704B (en) * | 2014-03-03 | 2015-05-27 | 中国环境科学研究院 | Permeable reaction medium material for nitrate pollution of underground water |
| CN104439270A (en) * | 2014-09-04 | 2015-03-25 | 河南城建学院 | Method for preparing sodium alginate/beta-cyclodextrin collaborative immobilized nanometer zero-valent iron |
| CN104475749A (en) * | 2014-09-04 | 2015-04-01 | 河南城建学院 | Preparation method of beta-cyclodextrin stabilized embedded nanoscale zero-valent iron |
| CN106699322A (en) * | 2015-09-25 | 2017-05-24 | 北京菲迪威尔科技有限公司 | Nitrogen-supplementing embedded growth-promoting agent, and preparation method and application thereof |
| CN106754855A (en) * | 2016-06-29 | 2017-05-31 | 华南理工大学 | Embedding type Nanoscale Iron/complex micro organism fungicide and preparation method thereof |
| CN105969760A (en) * | 2016-06-29 | 2016-09-28 | 华南理工大学 | Embedded nano-iron/single-microorganism composite microbial agent and preparation method thereof |
| CN105925560A (en) * | 2016-06-29 | 2016-09-07 | 华南理工大学 | Embedded nano iron/two microbial agents and preparation method thereof |
| CN105969760B (en) * | 2016-06-29 | 2020-02-18 | 华南理工大学 | Embedded nano iron/single microorganism composite microbial agent and preparation method thereof |
| CN105925560B (en) * | 2016-06-29 | 2020-06-19 | 华南理工大学 | Embedded nano-iron/two microbial agents and preparation method thereof |
| CN106754855B (en) * | 2016-06-29 | 2020-07-28 | 华南理工大学 | Embedded nano-iron/compound microbial agent and preparation method thereof |
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Application publication date: 20110330 |