CN106396131A - Novel composite nano-biomaterial and application thereof - Google Patents
Novel composite nano-biomaterial and application thereof Download PDFInfo
- Publication number
- CN106396131A CN106396131A CN201611045749.3A CN201611045749A CN106396131A CN 106396131 A CN106396131 A CN 106396131A CN 201611045749 A CN201611045749 A CN 201611045749A CN 106396131 A CN106396131 A CN 106396131A
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- China
- Prior art keywords
- composite nano
- phosphate rock
- lanthana
- ground phosphate
- biomaterial
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a preparation method of a novel composite nano-biomaterial used for removing heavy metal from waste water. The composite nano-biomaterial is prepared by modification measures such as high pressure steam and magnetic stirring from the materials of phosphate rock powder, lanthanum oxide, glacial acetic acid, amino three acetate and the like.
Description
Technical field
The present invention relates to a kind of novel composite nano biomaterial is used for removing the preparation method of the heavy metal in waste water, belong to
In water-treatment technology field.
Background technology
With the fast development of workers and peasants' industry, discharge heavy metal garbage quantity and exceed the self-purification ability of enviroment, make ecological landscape
See deterioration, aquatic organism loss of life, mankind's drink pollution of waterhead, surrounding Quality Down and affect health etc., this is
The frequent appearance of row problem of environmental pollution, gives people to have beaten alarm bell, reminds people's environmental pollution to be to be solved complete of current assistant officer
A ball difficult problem.Heavy metal has a stiff stability, difficult collect and the features such as toxicity is big, not only deteriorate composition of the soil, structure and work(
Can be moreover it is possible to pass through different channel serious harm healths.Therefore, process heavy metal pollution work and be subject to domestic and international logists
Great attention, become the important research content of field of scientific study.Shown, heavy metal flows into water body and soil, Yi Jihui
It is sent in atmosphere, take in human body followed by channels such as respiratory tract, plant and foods, be detrimental to health.I have invented
A kind of novel composite nano biomaterial is used for processing is had good effect by heavy metal polluted waste water.
Content of the invention
The problem existing for above-mentioned prior art, the present invention provides a kind of novel composite nano biomaterial to be used for removing
The preparation method of the heavy metal in waste water.
To achieve these goals, the technical solution used in the present invention is：A kind of novel composite nano biomaterial, its system
Preparation Method comprises the following steps：
Step 1, weigh a certain amount of ground phosphate rock first in beaker, be subsequently adding dehydrated alcohol, deionized water and glacial acetic acid,
After unlatching magnetic agitation is completely dissolved to ground phosphate rock, obtain final product A liquid；
Step 2, lanthana is taken to be added in the beaker filling dehydrated alcohol, magnetic agitation mix homogeneously, obtain final product B liquid；
Step 3, under magnetic stirring, with syringe drop by drop A liquid is slowly dropped in B liquid, after completion of dropping
Obtain the colloidal sol of homogeneous transparent, be then placed in the air ageing 24h and obtain final product gel；
Step 4 and then under nitrogen atmosphere ultrasonic wave concussion process 5h；
Step 5, gel is placed in air dry oven, 110 DEG C of drying, obtains xerogel；
Step 6, xerogel is ground into powder, is placed in Muffle furnace under 30% nitrogen+70% oxygen atmosphere, when
Between be 180 minutes, 600 DEG C of temperature, 0.5MPa, obtain phosphorus modification nano lanthanum oxide；
Step 7, the preparation of the culture medium of composite Nano biomaterial, its formula is (L-1)：11.5g glucose, 0.23g
Ammonium tartrate, 1.8g anhydrous sodium propionate, 0.5gNaH2PO4,0.06gMgSO4 7H2O, 0.08gCaCl2,0.002g biotin,
0.002g Folic Acid；
The calcium chloride solution of step 8, the sodium alginate soln of preparation a certain amount of 5% and 3%, then to sodium alginate soln
The middle nano lanthanum oxide adding phosphorus to modify, heats and stirs, bind up with gauze；
Step 9, by culture fluid, sodium alginate soln, calcium chloride solution, cotton swab, pipette tips etc. are placed in autoclave at 115 DEG C
Penicillium chrysogenum flat board is placed in activation 30min in shaking table simultaneously, and opens clean bench surface sterilizing by high pressure steam sterilization 90min
30min；
Step 10, first prepare a certain amount of Penicillium chrysogenum bacteria suspension, then by itself and the nano lanthanum oxide that adds phosphorus modification
Sodium alginate soln by volume 1: 2 mixing, stir；With 5ml syringe, by it, instillation calcium chloride drop by drop is molten
In liquid, that is, generate calcium alginate embedded bead, the embedding obtaining bead is continued to be placed in hardening 4h in calcium chloride solution, to improve
Its hardness, then filters and takes out simultaneously deionized water flushing several times.Finally by clean embedding bead equivalent be dispensed into equipped with
In the conical flask of culture fluid；
Step 11, the triangular pyramidal bottle being loaded into embedding bead are placed in 50 DEG C of constant-temperature table in 360r/min, shake
Swing culture 108 hours, filter, that is, obtain nanoscale composite biological material, then sample preparation is sieved 30-40 mesh.
Beneficial effect：A kind of present invention novel composite nano biomaterial is used for removing the heavy metal by waste water, this
Bright composite Nano biomaterial has bigger specific surface area than general nano material, inorganic nano material more organic than single
There are more excellent physicochemical properties, can preferably adsorb the heavy metal ion in water by synergism, acceptable
Heavy metal ion in water is changed into precipitate get off, then pass through ultrasound wave, the operation such as magnetic agitation can make compound receiving
The mechanical strength of the skeleton nano lanthanum oxide of rice biomaterial increases, and duct is more regular, and catalytic effect is more preferable.Pass through difference again
Calcine under atmosphere, so that the physico-chemical property of composite Nano biomaterial is improved further and can adapt it to varying environment, also can be by
Impurity in duct more thoroughly calcines removing.Wherein lanthana and the HUANGQING bacterium of ground phosphate rock mass ratio 1: 20,20 turbidity are hanged
The sample of liquid.Lanthana 1g, zeolite powder 20g, the HUANGQING bacteria suspension of 20 turbidity, dehydrated alcohol 20ml, deionized water 140ml, ice vinegar
Sour 30ml, the solution of preparation is prepared according to step；And produce the HUANGQING bacterium of lanthana and zeolite powder mass ratio 2: 24,40 turbidity
The sample of suspension.Lanthana 2g, ground phosphate rock 24g, the HUANGQING bacterium of 40 turbidity is hanged, liquid dehydrated alcohol 24ml, deionized water 168ml, ice
Acetic acid 36ml, the solution of preparation is prepared according to step.The composite Nano biomaterial being obtained under both ratios is subject to for removal
Heavy metal effect in waste water is best.
Specific embodiment
Embodiment 1 produces the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 1: 20,20 turbidity.Lanthana 1g,
Zeolite powder 20g, the HUANGQING bacteria suspension of 20 turbidity, dehydrated alcohol 20ml, deionized water 140ml, glacial acetic acid 30ml, the solution of preparation
Prepared according to step.
Step 1, weigh a certain amount of ground phosphate rock first in beaker, be subsequently adding dehydrated alcohol, deionized water and glacial acetic acid,
After unlatching magnetic agitation is completely dissolved to ground phosphate rock, obtain final product A liquid；
Step 2, lanthana is taken to be added in the beaker filling dehydrated alcohol, magnetic agitation mix homogeneously, obtain final product B liquid；
Step 3, under magnetic stirring, with syringe drop by drop A liquid is slowly dropped in B liquid, after completion of dropping
Obtain the colloidal sol of homogeneous transparent, be then placed in the air ageing 24h and obtain final product gel；
Step 4 and then under nitrogen atmosphere ultrasonic wave concussion process 5h；
Step 5, gel is placed in air dry oven, 110 DEG C of drying, obtains xerogel；
Step 6, xerogel is ground into powder, is placed in Muffle furnace under 30% nitrogen+70% oxygen atmosphere, when
Between be 180 minutes, 600 DEG C of temperature, 0.5MPa, obtain phosphorus modification nano lanthanum oxide；
Step 7, the preparation of the culture medium of composite Nano biomaterial, its formula is (L-1)：11.5g glucose, 0.23g
Ammonium tartrate, 1.8g anhydrous sodium propionate, 0.5gNaH2PO4,0.06gMgSO4 7H2O, 0.08gCaCl2,0.002g biotin,
0.002g Folic Acid；
The calcium chloride solution of step 8, the sodium alginate soln of preparation a certain amount of 5% and 3%, then to sodium alginate soln
The middle nano lanthanum oxide adding phosphorus to modify, heats and stirs, bind up with gauze；
Step 9, by culture fluid, sodium alginate soln, calcium chloride solution, cotton swab, pipette tips etc. are placed in autoclave at 115 DEG C
Penicillium chrysogenum flat board is placed in activation 30min in shaking table simultaneously, and opens clean bench surface sterilizing by high pressure steam sterilization 90min
30min；
Step 10, first prepare the HUANGQING bacteria suspension of a certain amount of turbidity, then by itself and the nano oxygen that adds phosphorus modification
Change sodium alginate soln 1: 2 mixing by volume of lanthanum, stir；With the instillation chlorination drop by drop by it of 5ml syringe
In calcium solution, that is, generate calcium alginate embedded bead, the embedding obtaining bead is continued to be placed in hardening 4h in calcium chloride solution, with
Improve its hardness, then filter taking-up and deionized water is rinsed several times, finally the embedding bead equivalent cleaned is dispensed into
Equipped with the conical flask of culture fluid；
Step 11, the triangular pyramidal bottle being loaded into embedding bead are placed in 50 DEG C of constant-temperature table in 360r/min, shake
Swing culture 108 hours, filter, that is, obtain nanoscale composite biological material, then sample preparation is sieved 30-40 mesh.
Embodiment 2 produces the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 2: 24,40 turbidity.Lanthana 2g,
Ground phosphate rock 24g, the HUANGQING bacteria suspension of 40 turbidity, dehydrated alcohol 24ml, deionized water 168ml, glacial acetic acid 36ml, other raw materials are used
Amount, operating procedure is as embodiment 1.
Embodiment 3 produces the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 2: 20,20 turbidity.Lanthana 2g,
Ground phosphate rock 20g, the HUANGQING bacteria suspension of 20 turbidity, other raw material dosage, operating procedure is as embodiment 1.
Embodiment 4 produces the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 4: 20,20 turbidity.Lanthana 4g,
Ground phosphate rock 20g, the HUANGQING bacteria suspension of 20 turbidity, other raw material dosage, operating procedure is as embodiment 1.
Embodiment 5 produces the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 6: 20,20 turbidity.Lanthana 6g,
Ground phosphate rock 20g, the HUANGQING bacteria suspension of 20 turbidity, other raw material dosage, operating procedure is as embodiment 1.
Embodiment 6 produces the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 1: 22,20 turbidity.Lanthana 1g,
Ground phosphate rock 22g, the HUANGQING bacteria suspension of 20 turbidity, other raw materials of dehydrated alcohol 22ml, deionized water 154ml, glacial acetic acid 33ml are used
Amount, operating procedure is as embodiment 1.
Embodiment 7 produces the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 1: 24,20 turbidity.Lanthana 1g,
Ground phosphate rock 24g, the HUANGQING bacteria suspension of 20 turbidity, other raw materials of dehydrated alcohol 24ml, deionized water 168ml, glacial acetic acid 36ml are used
Amount, operating procedure is as embodiment 1.
Embodiment 8 produces the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 2: 24,30 turbidity.Lanthana 2g,
Ground phosphate rock 24g, the HUANGQING bacteria suspension of 30 turbidity, other raw materials of dehydrated alcohol 24ml, deionized water 168ml, glacial acetic acid 36ml are used
Amount, operating procedure is as embodiment 1.
Embodiment 9 produces the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 2: 24,50 turbidity.Lanthana 2g, 2
Ground phosphate rock 4g, the HUANGQING bacteria suspension of 50 turbidity, other raw materials of dehydrated alcohol 24ml, deionized water 168ml, glacial acetic acid 36ml are used
Amount, operating procedure is as embodiment 1.
Embodiment 10 produces the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 2: 24,60 turbidity.Lanthana 1g,
Ground phosphate rock 24g, the HUANGQING bacteria suspension of 60 turbidity, dehydrated alcohol 24ml, deionized water 168ml, glacial acetic acid 36ml, other raw materials are used
Amount, operating procedure is as embodiment 1.
Embodiment 11 produces the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 1: 20,30 turbidity.Lanthana 1g,
2 ground phosphate rock 0g, the HUANGQING bacteria suspension of 30 turbidity, dehydrated alcohol 20ml, deionized water 140ml, glacial acetic acid 30ml, other raw materials are used
Amount, operating procedure is as embodiment 1.
Embodiment 12 produces the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 1: 20,40 turbidity.Lanthana 1g,
Ground phosphate rock 20g, the HUANGQING bacteria suspension of 40 turbidity, other raw material dosage, operating procedure is as embodiment 1.
Embodiment 13 produces the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 1: 20,50 turbidity.Lanthana 1g,
Ground phosphate rock 20g, the HUANGQING bacteria suspension of 50 turbidity, other raw material dosage, operating procedure is as embodiment 1.
Embodiment 14 produces the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 1: 20,60 turbidity.Lanthana 1g,
Ground phosphate rock 20g, the HUANGQING bacteria suspension of 60 turbidity, other raw material dosage, operating procedure is as embodiment 1.
Reference examples 1 produce the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 1: 20,20 turbidity.Lanthana 1g,
Ground phosphate rock 20g, the HUANGQING bacteria suspension of 20 turbidity, using mechanical agitation without magnetic agitation, other raw material dosage, operating procedure with
As embodiment 1.
Reference examples 2 produce the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 1: 20,20 turbidity.Lanthana 1g,
Ground phosphate rock 20g, the HUANGQING bacteria suspension of 20 turbidity, process without ultrasonic wave concussion, other raw material dosage, operating procedure is with implementing
As example 1.
Reference examples 3 produce the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 1: 20,20 turbidity.Lanthana 1g,
Ground phosphate rock 20g, the HUANGQING bacteria suspension of 20 turbidity, without gaseous mixture calcining, using the calcining of single air atmosphere, other raw materials are used
Amount, operating procedure is as embodiment 1.
Reference examples 4 produce the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 1: 20,20 turbidity.Lanthana 1g,
Ground phosphate rock 20g, the HUANGQING bacteria suspension of 20 turbidity, do not carry out embedding bead and be placed in cure operations in calcium chloride solution, other raw materials
Consumption, operating procedure is as embodiment 1.
Reference examples 5 are produced and are added without ground phosphate rock sample.Lanthana 1g, the HUANGQING bacteria suspension of 20 turbidity, other raw material dosage, behaviour
Make step as embodiment 1.
Reference examples 6 produce the biomass combined sample of discord.Lanthana 1g, ground phosphate rock 20g, remove and biomass combined one
Sequence of maneuvers, other raw material dosage, operating procedure is as embodiment 1.
Test method
By 1L by the water of heavy metal pollution my composite Nano level biomaterial of preparing of addition 0.05g, also one group empty
White group is added without the composite Nano level biomaterial of my preparation.
After table one 12h, detection adds the content of beary metal in composite Nano level biomaterial contaminant water
Test result indicate that：It can be found that the composite Nano biomaterial of embodiment 1,2 preparation is used for removing by waste water
Weight
Metal effect preferably, illustrates the sample of lanthana and the HUANGQING bacteria suspension of ground phosphate rock mass ratio 1: 20,20 turbidity, and
The sample of the HUANGQING bacteria suspension of lanthana and ground phosphate rock mass ratio 2: 24,40 turbidity, the synergism between internal each several part is best
To the heavy metal best results removing in contaminant water.The composite Nano biomaterial being obtained under other ratios is used for removing in waste water
Heavy metal effect general.Comparative example 1, comparative example 1,2, and 3,4 can be found that.Do not carry out magnetic agitation, ultrasound wave, difference
Calcine under atmosphere, do not carry out embedding bead and be placed in the composite Nano biomaterial that cure operations in calcium chloride solution are obtained and be used for
Except the heavy metal effect in waste water is bad.Comparative example 1, comparative example 5, and 6 it can be found that be added without ground phosphate rock, or not with life
It is bad for the heavy metal effect that removes in waste water that material is combined prepared nano material.
Claims (6)
1. a kind of novel composite nano biomaterial is it is characterised in that respectively with ground phosphate rock, lanthana, glacial acetic acid, amino three second
Acid esters passes through high steam, and the modified method such as magnetic agitation prepares composite Nano biomaterial.
2. novel composite nano biomaterial according to claim 1 is it is characterised in that its preparation method is specific as follows：
Step 1, weigh a certain amount of ground phosphate rock first in beaker, be subsequently adding dehydrated alcohol, deionized water and glacial acetic acid, open
Stir after being completely dissolved to ground phosphate rock, obtain final product A liquid；
Step 2, take lanthana to be added in the beaker filling dehydrated alcohol, be uniformly mixed, obtain final product B liquid；
Step 3, under magnetic stirring, with syringe drop by drop A liquid is slowly dropped in B liquid, after completion of dropping
To the colloidal sol of homogeneous transparent, then it is placed in the air ageing and obtains final product gel；
Step 4 and then under nitrogen atmosphere ultrasonic wave concussion are processed;
Step 5, gel is placed in air dry oven, 110 DEG C of drying, obtains xerogel；
Step 6, xerogel is ground into powder, is placed in Muffle furnace, the time is 180 minutes, 600 DEG C of temperature, 0.5MPa,
Obtain the nano lanthanum oxide of phosphorus modification；
Step 7, the preparation of the culture medium of composite Nano biomaterial；
The calcium chloride solution of step 8, the sodium alginate soln of preparation a certain amount of 5% and 3%, then adds in sodium alginate soln
Enter the nano lanthanum oxide of phosphorus modification, heat and stir, bind up with gauze；
Step 9, by culture fluid, sodium alginate soln, calcium chloride solution, cotton swab, pipette tips etc. are placed in autoclave high pressure at 115 DEG C
Penicillium chrysogenum flat board is placed in activation 30min in shaking table simultaneously, and opens clean bench surface sterilizing by steam sterilization 90min
30min；
Step 10, first prepare a certain amount of Penicillium chrysogenum bacteria suspension, then by the sea of itself and the nano lanthanum oxide adding phosphorus modification
Solution of sodium alginate mixes, and stirs；With syringe by its instillation calcium chloride solution drop by drop, that is, generate calcium alginate
Embedding bead, the embedding obtaining bead is continued to be placed in hardening in calcium chloride solution, to improve its hardness, then filters and take out simultaneously
Deionized water is rinsed several times;
Finally the embedding cleaned bead equivalent is dispensed into equipped with the bottle of culture fluid；
Step 11, the triangular pyramidal bottle being loaded into embedding bead are placed in 50 DEG C of constant-temperature table in 360r/min, vibration
Culture, filters, that is, obtains nanoscale composite biological material, and then sample preparation is sieved 30-40 mesh.
3. novel composite nano biomaterial according to claim 2 is it is characterised in that described composite Nano biology material
The preparation of the culture medium of material, its formula is（L-1）：11.5 g glucoses, 0.23g ammonium tartrate, 1.8 g anhydrous sodium propionates,
0.5gNaH2PO4,0.06gMgSO4 7H2O, 0.08gCaCl2,0.002g biotin, 0.002g Folic Acid.
4. novel composite nano biomaterial according to claim 2 is it is characterised in that in described step 10, HUANGQING
Mould bacteria suspension and sodium alginate soln by volume 1:2 mixing.
5. novel composite nano biomaterial according to claim 2 is it is characterised in that in described step 6, Muffle furnace
Atmosphere is 30% nitrogen+70% oxygen atmosphere.
6. a kind of novel composite nano biomaterial as described in power 1-4 is for removing the application in terms of heavy metal in waste water.
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| CN201611045749.3A CN106396131A (en) | 2016-11-24 | 2016-11-24 | Novel composite nano-biomaterial and application thereof |
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| CN201611045749.3A CN106396131A (en) | 2016-11-24 | 2016-11-24 | Novel composite nano-biomaterial and application thereof |
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| CN106396131A true CN106396131A (en) | 2017-02-15 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106753391A (en) * | 2016-11-28 | 2017-05-31 | 新沂市中诺新材料科技有限公司 | A kind of nano material and preparation method for being passivated heavy metal in rehabilitating soil |
-
2016
- 2016-11-24 CN CN201611045749.3A patent/CN106396131A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106753391A (en) * | 2016-11-28 | 2017-05-31 | 新沂市中诺新材料科技有限公司 | A kind of nano material and preparation method for being passivated heavy metal in rehabilitating soil |
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Application publication date: 20170215 |