CN101792145A - Method for separating and extracting shell pieces and clitellum from kieselguhr or diatoms - Google Patents
Method for separating and extracting shell pieces and clitellum from kieselguhr or diatoms Download PDFInfo
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- CN101792145A CN101792145A CN201010033699A CN201010033699A CN101792145A CN 101792145 A CN101792145 A CN 101792145A CN 201010033699 A CN201010033699 A CN 201010033699A CN 201010033699 A CN201010033699 A CN 201010033699A CN 101792145 A CN101792145 A CN 101792145A
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Abstract
The invention discloses a method for separating and extracting shell pieces and clitellum from kieselguhr or diatoms. The method comprises the following steps of: classifying and extracting the shell pieces and the clitellum by adopting a Stokes sedimentation method in the extraction process; calculating the sedimentation velocity difference between the shell pieces and the clitellum with same particle diameters by combining with a fluid dynamics theory; and carrying out sedimentation by adding deionized water a plurality of times to finish high-purity classification and extraction of the shell pieces and the clitellum. The method can not damage structures of the shell pieces and the clitellum and keep the topography and the microstructure of the original species of diatoms, and the shell pieces and the clitellum are only separated at connecting strips. 0.2 to 0.6g of shell pieces and 0.1 to 0.3g of clitellum can be extracted from 1g of siliceous shells.
Description
Technical field
The present invention relates to a kind of extracting method of microorganism structure, more particularly say, being meant a kind of is starting material with diatomite, diatom, therefrom the method for separation and Extraction shell sheet and endless belt.
Background technology
Diatomite is that the dead later silicate remains of the unicellular algae of diatom form, and its composition is aqueous amorphousness SiO
2Diatomite has various profile, unique shell structure, bigger serface, high porosity, low density, advantageous property such as high temperature resistant, and wide material sources, cheap.At the beginning of last century, diatomite ore is exploited in a large number and is widely used in industry, develops the product of high yields such as diatomite adsorbant, flocculating aids, lagging material, sound-proof material.China's diatomite proven reserve occupy the second in the world, and main mineral resources is the rotary strainer algae diatomite in Jilin and the melosira diatomite of Shengzhou, Zhejiang.The output of super-cell, insulating brick is at the forefront in the world.
Diatom is miscellaneous hydrobiont, and monomer cell 3 μ m～600 μ m are divided into " center guiding principle " and " pennates ", and kind surplus in the of about 11000 is distributed widely in lake, river, ocean, the soil, is product oxygen person and bait important in the ocean.The cell wall constituent of diatom is a soft silica, pattern is various, structure is unique because of having for this crepis, hole system evenly, water white transparency, adsorptivity be strong, with advantage such as silicon process technology compatibility, become micro-nano Study on Technology focus, and formed diatom nanotechnology direction.The diatom crepis pattern of different genera is different, includes shapes such as circle, ellipse, rectangle, kidney shape, trilateral, aciculiform, rhombus, and the surface all has regularly arranged micropore.If the diatom test that pattern is different is placed in together, can build up " the quartzy museum " of a seat minitype.
All contain crepis in diatomite or the diatom, crepis is divided into shell sheet and endless belt two portions again.The diatom pattern of different genera is different, thereby shell sheet, endless belt also have different shapes and characteristic.Shell sheet aspect, center guiding principle diatom test sheet have more big concavo-convex, pore chamber big and arrange in order, this kind structure makes diatom can better assemble sunlight to carry out photosynthesis; Pennates shell sheet is flat, longitudinal furrow, angle hair is arranged, sting microstructures such as protruding, and this kind structure makes easier rock and the other biological surface of being adsorbed on of diatom.The endless belt aspect, the endless belt shape thickness of different diatoms is different, and annulus, kidney shape, trilateral etc. are arranged, and certain elastic deformability is arranged.
But existing research is not often treated shell sheet and endless belt differentiation, therefore the effect that has influenced research and used, as diatomite adsorbant, flocculating aids, the main component rotary strainer algae diatomite that use are processed more, have the endless belt of a part of rotary strainer algae in this diatomite, and there is not hole system in endless belt, specific surface area is little, substantially do not have adsorptive power, but occupy the quality of product about 15%, can remove fully.On the other hand, almost nil to the applied research of endless belt both at home and abroad, the endless belt external diameter is contained 1 μ m～100 μ m, this appearance and size and more existing optics, the micro element of communicating by letter are similar, as the focus wave strap of X-ray microscope, optical fiber micro-ring resonator etc., as seen endless belt may not be good for nothing, and does not just have effective means that endless belt is extracted in a large number.
Can separation and Extraction as shell sheet and endless belt, the production technique and the effect of many products be will improve, and little part, particularly ring parts of multiple different-shape feature obtained, enriched the material depot of micro-nano research.
Summary of the invention
The objective of the invention is to propose a kind of method that from diatomite, diatom, extracts shell sheet and endless belt, this method adopts sedimentation method to the extraction of classifying of shell sheet and endless belt, can the structure of shell sheet and endless belt not damaged like this, the pattern and the microstructure that have kept original kind diatom, and only separate from connecting band between shell sheet and the endless belt.
Of the present invention a kind of from diatomite or diatom the method for separation and Extraction shell sheet and endless belt, it comprises that step has:
(A) crepis that diatomite or diatom are obtained after pre-treatment is put into Glass Containers, adds mass percent concentration and be 95% dehydrated alcohol; And Glass Containers placed the ultrasonic cleaning machine, behind ultrasonic cleaning 30min～60min under the condition of power 700W～1000W, operating frequency 25KHz～40KHz, adopting the aperture is that the filter cloth of 3 μ m～20 μ m separates, and filters and obtains the filter cloth topper;
The dehydrated alcohol that adds 50ml～100ml in the crepis of consumption: 1g;
(B) with the filter cloth topper behind dry 4h～6h under 110 ℃～150 ℃ temperature, make the dried powder that contains shell sheet and endless belt;
(C) the dried powder adding of 1g～2g is equipped with in the graduated cylinder of 50ml deionized water, after stirring 5s～20s under the rotating speed of 50r/min～100r/min, leaves standstill 10min～40min, and pipette out 35ml first mixed solution from graduated cylinder top to container with pipettor;
(D) in graduated cylinder, inject the 35ml deionized water once more, after stirring 5s～20s under the rotating speed of 50r/min～100r/min, leave standstill 10～40min, and pipette out 35ml second mixed solution from graduated cylinder top to the container of step (C) with pipettor;
(E) in graduated cylinder, inject the 35ml deionized water once more, after stirring 5s～20s under the rotating speed of 50r/min～100r/min, leave standstill 10～40min, and pipette out 35ml the 3rd mixed solution from graduated cylinder top to the container of step (C) with pipettor;
(F) surplus solution in the graduated cylinder is screened with 3 μ m～20 μ m filter clothes, the filter cloth topper behind dry 4h～6h under 110 ℃～150 ℃ temperature, is made the shell sheet;
(G) mixed solution in the container is screened with 3 μ m～20 μ m filter clothes, the filter cloth topper behind dry 4h～6h under 110 ℃～150 ℃ temperature, is made endless belt; Described mixed solution is the summation of first mixed solution, second mixed solution and the 3rd mixed solution;
In the present invention, can extract the shell sheet of 0.2g～0.6g in the crepis of 1g, the endless belt of 0.1g～0.3g.
By observation at microscopically, the pattern and the microtexture that adopt shell sheet that method separation and Extraction of the present invention goes out and endless belt all to keep original kind diatom.
In step of the present invention (A), be to the pre-treatment step of diatom:
(A) diatom being put into mass percent concentration is that 50%～70% sulfuric acid mixes and obtains diatom suspension;
The sulfuric acid that adds 40ml～60ml in the diatom of consumption: 1g;
(B) diatom suspension is taken out and puts into whizzer after being incubated 30min～60min under 90 ℃～100 ℃ temperature; Behind centrifugal treating 8min～20min under the rotating speed of 3000r/min～7000r/min, take out, remove supernatant liquid, obtain first mixture;
(C) in first mixture, add deionized water, behind centrifugal treating 8min～20min under the rotating speed of 3000r/min～7000r/min, take out, remove supernatant liquid, obtain second mixture;
The deionized water that adds 40ml～60ml in first mixture of consumption: 10ml;
In the present invention, step (C) is for removing impurity and removing vitriolization, and the operation that repeats this step can be 2 times～7 times.
(D) in second mixture, add deionized water, behind centrifugal treating 8min～20min under the rotating speed of 3000r/min～7000r/min, take out, remove supernatant liquid, obtain the 3rd mixture;
The deionized water that adds 40ml～60ml in second mixture of consumption: 10ml;
(E) add deionized water in the 3rd mixture, behind centrifugal treating 8min～20min under the rotating speed of 3000r/min～7000r/min, take out, remove supernatant liquid, obtain 4 mixture, this 4 mixture is crepis;
The deionized water that adds 40ml～60ml in the 3rd mixture of consumption: 10ml.
In the present invention, step (C), step (D) and step (E) are sulfuric acid and the impurity that exists in the mixture for removing, and this impurity is mainly protein, thereby obtain crepis.Therefore, main component is a crepis in first mixture, second mixture, the 3rd mixture and the 4 mixture.
In step of the present invention (A), be to diatomaceous pre-treatment step:
Commercially available diatomite is put into Glass Containers, and the adding mass percent concentration is 95% dehydrated alcohol, behind ultrasonic cleaning 10min～30min under the condition of power 700W～1000W, operating frequency 25KHz～40KHz, the use aperture is that the filter cloth of 5 μ m～100 μ m separates, filtration obtains filter cloth topper, i.e. crepis;
The dehydrated alcohol that adds 50～100ml in the diatomite of consumption: 1g.
Of the present invention from diatomite or diatom the advantage of separation and Extraction shell sheet and endless belt method:
1. this method is removed the organic matter at diatom connecting band place by the vitriol oil, and adds the ultrasonic high-frequency vibration of dehydrated alcohol and make the nano level convex closure of shell sheet and endless belt contact surface and pit loosening, finally makes the disengagement of shell sheet and endless belt.
2. the present invention uses sedimentation method that shell sheet and endless belt have been carried out the classification extraction.The stokes sedimentation theory often is used for the particle of different-grain diameter is carried out category filter, the present invention there are differences in conjunction with shell sheet and the endless belt settling velocity that fluid dynamic theory calculates same particle diameter, and extract the test method easy handling by the high purity classification that settling test has been finished shell sheet and endless belt.
3. the present invention extracts the shell sheet and the endless belt of different-shape from the different genera diatom, for micro-nano research provides new material.
Description of drawings
Fig. 1 is C292 type diatomite microscopically is produced in the place of production for Shantou, Guangdong an original pattern photo.
Figure 1A is the crepis microphotograph of rotary strainer algae diatomite after the pre-treatment of embodiment 1 with Fig. 1.
Figure 1B is the microphotograph that adopts the complete shell sheet of rotary strainer algae that embodiment 1 method makes.
Fig. 1 C is the microphotograph that adopts the complete endless belt of rotary strainer algae that embodiment 1 method makes.
Fig. 2 is that the place of production is the original pattern photo of Shengzhou, Zhejiang melosira diatomite microscopically.
Fig. 2 A is the electromicroscopic photograph with the crepis pattern of melosira diatomite after the pre-treatment of embodiment 2 of Fig. 2.
Fig. 2 B is the electromicroscopic photograph that adopts the complete shell sheet of the melosira pattern that embodiment 2 methods make.
Fig. 2 C is the electromicroscopic photograph that adopts the complete endless belt pattern of melosira that embodiment 2 methods make.
Fig. 3 is the original pattern photo of the curved algae microscopically of bridge.
Fig. 3 A is the electromicroscopic photograph with the curved crepis pattern of algae after the pre-treatment of embodiment 3 of bridge of Fig. 3.
Fig. 3 B is the amplification electromicroscopic photograph of the curved algae pattern of single bridge among Fig. 3 A.
Fig. 3 C is the electromicroscopic photograph that adopts the curved complete shell sheet of the algae pattern of bridge that embodiment 3 methods make.
Fig. 3 D is the electromicroscopic photograph that adopts the curved complete endless belt pattern of algae of bridge that embodiment 3 methods make.
Embodiment
The method that the present invention extracts shell sheet and endless belt is that the crepis that respectively diatomite or diatom is carried out obtaining after the pre-treatment carries out, and mainly uses sedimentation method.The stokes sedimentation theory often is used for the particle of different-grain diameter is carried out category filter, in the leaching process of shell sheet and endless belt, the present invention calculates the shell sheet of same particle diameter and the difference that the endless belt settling velocity exists in conjunction with fluid dynamic theory, carries out the high purity classification extraction that shell sheet and endless belt have been finished in sedimentation by repeatedly adding deionized water.
Of the present invention a kind of from diatomite or diatom the method for separation and Extraction shell sheet and endless belt, it comprises that step has:
(A) crepis that diatomite or diatom are obtained after pre-treatment is put into Glass Containers, adds mass percent concentration and be 95% dehydrated alcohol; And Glass Containers placed the ultrasonic cleaning machine, behind ultrasonic cleaning 30min～60min under the condition of power 700W～1000W, operating frequency 25KHz～40KHz, adopting the aperture is that the filter cloth of 3 μ m～20 μ m separates, and filters and obtains the filter cloth topper;
The dehydrated alcohol that adds 50ml～100ml in the crepis of consumption: 1g;
(B) with the filter cloth topper behind dry 4h～6h under 110 ℃～150 ℃ temperature, make the dried powder that contains shell sheet and endless belt;
(C) the dried powder adding of 1g～2g is equipped with in the graduated cylinder of 50ml deionized water, after stirring 5s～20s under the rotating speed of 50r/min～100r/min, leaves standstill 10min～40min, and pipette out 35ml first mixed solution from graduated cylinder top to container with pipettor;
(D) in graduated cylinder, inject the 35ml deionized water once more, after stirring 5s～20s under the rotating speed of 50r/min～100r/min, leave standstill 10～40min, and pipette out 35ml second mixed solution from graduated cylinder top to the container of step (C) with pipettor;
(E) in graduated cylinder, inject the 35ml deionized water once more, after stirring 5s～20s under the rotating speed of 50r/min～100r/min, leave standstill 10～40min, and pipette out 35ml the 3rd mixed solution from graduated cylinder top to the container of step (C) with pipettor;
(F) surplus solution in the graduated cylinder is screened with 3 μ m～20 μ m filter clothes, the filter cloth topper behind dry 4h～6h under 110 ℃～150 ℃ temperature, is made the shell sheet;
(G) mixed solution in the container is screened with 3 μ m～20 μ m filter clothes, the filter cloth topper behind dry 4h～6h under 110 ℃～150 ℃ temperature, is made endless belt; Described mixed solution is the summation of first mixed solution, second mixed solution and the 3rd mixed solution;
In the present invention, can extract the shell sheet of 0.2g～0.6g in the crepis of 1g, the endless belt of 0.1g～0.3g.
By observation at microscopically, the pattern and the microtexture that adopt shell sheet that method separation and Extraction of the present invention goes out and endless belt all to keep original kind diatom.
In step of the present invention (A), be to the pre-treatment step of diatom:
(A) diatom being put into mass percent concentration is that 50%～70% sulfuric acid mixes and obtains diatom suspension;
The sulfuric acid that adds 40ml～60ml in the diatom of consumption: 1g;
(B) diatom suspension is taken out and puts into whizzer after being incubated 30min～60min under 90 ℃～100 ℃ temperature; Behind centrifugal treating 8min～20min under the rotating speed of 3000r/min～7000r/min, take out, remove supernatant liquid, obtain first mixture;
(C) in first mixture, add deionized water, behind centrifugal treating 8min～20min under the rotating speed of 3000r/min～7000r/min, take out, remove supernatant liquid, obtain second mixture;
The deionized water that adds 40ml～60ml in first mixture of consumption: 10ml;
In the present invention, step (C) is for removing impurity and removing vitriolization, and the operation that repeats this step can be 2 times～7 times.
(D) in second mixture, add deionized water, behind centrifugal treating 8min～20min under the rotating speed of 3000r/min～7000r/min, take out, remove supernatant liquid, obtain the 3rd mixture;
The deionized water that adds 40ml～60ml in second mixture of consumption: 10ml;
(E) add deionized water in the 3rd mixture, behind centrifugal treating 8min～20min under the rotating speed of 3000r/min～7000r/min, take out, remove supernatant liquid, obtain 4 mixture, this 4 mixture is crepis;
The deionized water that adds 40ml～60ml in the 3rd mixture of consumption: 10ml.
In the present invention, step (C), step (D) and step (E) are sulfuric acid and the impurity that exists in the mixture for removing, and this impurity is mainly protein, thereby obtain crepis.Therefore, main component is a crepis in first mixture, second mixture, the 3rd mixture and the 4 mixture.
In step of the present invention (A), be to diatomaceous pre-treatment step:
Commercially available diatomite is put into Glass Containers, and the adding mass percent concentration is 95% dehydrated alcohol, behind ultrasonic cleaning 10min～30min under the condition of power 700W～1000W, operating frequency 25KHz～40KHz, the use aperture is that the filter cloth of 5 μ m～100 μ m separates, filtration obtains filter cloth topper, i.e. crepis;
The dehydrated alcohol that adds 50～100ml in the diatomite of consumption: 1g.
Embodiment 1Separation and Extraction rotary strainer frustule sheet and endless belt from C292 type diatomite
Use Shantou, Guangdong to produce C292 type diatomite (its pattern as shown in Figure 1), particle diameter 20 orders, its starting material are all the Tu Kuang that the diatom remains form, and organic matter decomposes already.
One, the diatomaceous pre-treatment of C292 type
C292 type diatomite is put into Glass Containers, and the adding mass percent concentration is 95% dehydrated alcohol, behind ultrasonic cleaning 30min under the condition of power 800W, operating frequency 25KHz, the use aperture is that the filter cloth of 20 μ m separates, and the filter cloth topper is crepis;
The dehydrated alcohol that adds 100ml in the diatomite of consumption: 1g.
In the present invention, adopting microscope can observe out crepis is rotary strainer algae crepis, and its pattern is shown in Figure 1A, and as can be seen from the figure, the impurity in the C292 type diatomite is eliminated, and composition is clean rotary strainer frustule sheet and endless belt.
Two, crepis mesochite sheet and endless belt separates
(A) rotary strainer algae crepis is put into Glass Containers, the adding mass percent concentration is 95% dehydrated alcohol, and Glass Containers placed the ultrasonic cleaning machine, behind ultrasonic cleaning 30min under the condition of power 800W, operating frequency 25KHz, the employing aperture is that the filter cloth of 20 μ m separates, and filters and obtains the filter cloth topper;
The dehydrated alcohol that adds 100ml in the rotary strainer algae crepis of consumption: 1g;
(B) with the filter cloth topper at 120 ℃ down behind the dry 4h, make the dried powder that contains shell sheet and endless belt;
(C) the dried powder adding of 1g is equipped with in the graduated cylinder of 50ml deionized water, after stirring 5s under the rotating speed of 50r/min, is leaving standstill 20min, and pipetting out 35ml first mixed solution from graduated cylinder top to container with pipettor;
(D) in graduated cylinder, inject the 35ml deionized water once more, after stirring 5s under the 50r/min rotating speed, leave standstill 20min, and pipette out 35ml second mixed solution from graduated cylinder top to the container of step (C) with pipettor;
(E) in graduated cylinder, inject the 35ml deionized water once more, after stirring 5s under the rotating speed of 50r/min, leave standstill 20min, and pipette out 35ml the 3rd mixed solution from graduated cylinder top to the container of step (C) with pipettor;
(F) surplus solution in the graduated cylinder is screened with 20 μ m filter clothes, the filter cloth topper behind 120 ℃ of following dry 4h of temperature, is made the shell sheet; Shown in Figure 1B, as can be seen from the figure, the complete shell sheet of rotary strainer algae content reaches more than 80%, no fine impurities, and shell sheet cleaning surfaces, micropore is high-visible.
(G) mixed solution in the container (mixing of first mixed solution, second mixed solution and the 3rd mixed solution) is screened with 20 μ m filter clothes, the filter cloth topper behind 120 ℃ of following dry 4h of temperature, is made endless belt; Shown in Fig. 1 C, as can be seen from the figure, rotary strainer algal rim band content reaches more than 90%, does not have other impurity.
In the present invention, can extract the shell sheet of 0.5g in the diatomite of 1g, the endless belt of 0.2g.
Embodiment 2Separation and Extraction rotary strainer frustule sheet and endless belt from the melosira diatomite of Shengzhou, Zhejiang
Use Shengzhou, Zhejiang melosira diatomite (its pattern as shown in Figure 2), particle diameter 200 orders, its starting material are all the Tu Kuang that the diatom remains form, and organic matter decomposes already.
One, the diatomaceous pre-treatment of Shengzhou, Zhejiang melosira
Shengzhou, Zhejiang melosira diatomite is put into Glass Containers, the adding mass percent concentration is 95% dehydrated alcohol, and Glass Containers placed the ultrasonic cleaning machine, behind ultrasonic cleaning 15min under the condition of power 1000W, operating frequency 40KHz, the employing aperture is that the filter cloth of 10 μ m separates, and the filter cloth topper is crepis;
The dehydrated alcohol that adds 80ml in the diatomite of consumption: 1g.
In the present invention, the pattern that the employing microscope can be observed out the melosira crepis is shown in Fig. 2 A, and as can be seen from the figure, the impurity (protein) in the melosira diatomite of Shengzhou, Zhejiang is eliminated, and composition is clean straight chain frustule sheet and endless belt.
Two, the separating step of crepis mesochite sheet and endless belt
(A) crepis is put into Glass Containers, the adding mass percent concentration is 95% dehydrated alcohol, and Glass Containers placed the ultrasonic cleaning machine, behind ultrasonic cleaning 45min under the condition of power 1000W, operating frequency 40KHz, the employing aperture is that the filter cloth of 10 μ m separates, and filters and obtains the filter cloth topper;
The dehydrated alcohol that adds 80ml in the diatom crepis of consumption: 1g;
(B) with the filter cloth topper at 150 ℃ down behind the dry 4h, make the dried powder that contains shell sheet and endless belt;
(C) the dried powder adding of 2g is equipped with in the graduated cylinder of 50ml deionized water, after stirring 5s under the rotating speed of 100r/min, is leaving standstill 10min, and pipetting out 35ml first mixed solution from graduated cylinder top to container with pipettor;
(D) in graduated cylinder, inject the 35ml deionized water once more, after stirring 10s under the rotating speed of 100r/min, leave standstill 10min, and pipette out 35ml second mixed solution from graduated cylinder top to container with pipettor;
(E) in graduated cylinder, inject the 35ml deionized water once more, after stirring 10s under the rotating speed of 100r/min, leave standstill 10min, and pipette out 35ml the 3rd mixed solution from graduated cylinder top to container with pipettor;
(F) in graduated cylinder, inject the 35ml deionized water once more, after stirring 10s under the rotating speed of 100r/min, leave standstill 10min, and pipette out 35ml the 4th mixed solution from graduated cylinder top to container with pipettor;
(G) in graduated cylinder, inject the 35ml deionized water once more, after stirring 10s under the rotating speed of 100r/min, leave standstill 10min, and pipette out 35ml the 5th mixed solution from graduated cylinder top to container with pipettor;
(H) surplus solution in the graduated cylinder is screened with 10 μ m filter clothes, filter cloth upper strata residual particles behind dry 4h under 150 ℃, is made endless belt; Shown in Fig. 2 C.As can be seen from the figure, melosira endless belt content reaches more than 90%, and surface micropore is clear.
(I) mixed solution in the container is screened with 10 μ m filter clothes, filter cloth upper strata residual particles behind 150 ℃ of following dry 4h of temperature, is made the shell sheet; Shown in Fig. 2 B.As can be seen from the figure, straight chain frustule sheet content reaches more than 80%, shell sheet cleaning surfaces, and micropore is high-visible.
In the present invention, can extract the shell sheet of 0.7g in the diatomite of 2g, the endless belt of 0.5g.
Embodiment 3Curved frustule sheet of separation and Extraction bridge and endless belt from the curved algae of bridge
One, organic treatment step is removed in the diatom deactivation
(A) the curved algae (as shown in Figure 3) of the bridge of culturing being put into mass percent concentration is that 70% sulfuric acid mixes and obtains diatom suspension;
The sulfuric acid that adds 50ml in the curved algae of the bridge of consumption: 1g;
(B) diatom suspension is put into whizzer behind the insulation 40min down for 90 ℃ in temperature; Behind centrifugal treating 15min under the rotating speed of 6000r/min, take out, remove supernatant liquid, obtain first mixture;
(C) in first mixture, add deionized water, behind centrifugal treating 8min under the rotating speed of 6000r/min, take out, remove supernatant liquid, obtain second mixture;
The deionized water that adds 40ml in first mixture of consumption: 10ml;
(D) in second mixture, add deionized water, behind centrifugal treating 8min under the rotating speed of 6000r/min, take out, remove supernatant liquid, obtain the 3rd mixture;
The deionized water that adds 40ml in second mixture of consumption: 10ml;
(E) in the 3rd mixture, add deionized water, behind centrifugal treating 8min under the rotating speed of 6000r/min, take out, remove supernatant liquid, obtain 4 mixture;
The deionized water that adds 40ml in the 3rd mixture of consumption: 10ml;
(F) in 4 mixture, add deionized water, behind centrifugal treating 8min under the rotating speed of 6000r/min, take out, remove supernatant liquid, obtain the 5th mixture, be i.e. the curved algae crepis of bridge;
The deionized water that adds 40ml in the 4 mixture of consumption: 10ml;
In the present invention, adopting microscope can observe out second the ingredients of a mixture is the curved algae crepis of bridge, and its pattern as can be seen from the figure, has tangible micropore on the curved algae crepis of bridge shown in Fig. 3 A, Fig. 3 B, do not have organic the existence.
Two, the separating step of crepis mesochite sheet and endless belt
(A) the curved algae crepis of bridge is put into Glass Containers, the adding mass percent concentration is 95% dehydrated alcohol, and Glass Containers placed the ultrasonic cleaning machine, behind ultrasonic cleaning 60min under the condition of power 1000W, operating frequency 40KHz, the employing aperture is that the filter cloth of 3 μ m separates, and filters and obtains the filter cloth topper;
The dehydrated alcohol that adds 100ml in the diatom crepis of consumption: 1g;
(B) with the filter cloth topper at 120 ℃ down behind the dry 4h, make the dried powder that contains shell sheet and endless belt;
(C) the dried powder adding of 1g is equipped with in the graduated cylinder of 50ml deionized water, after stirring 15s under the rotating speed of 50r/min, is leaving standstill 40min, and pipetting out 35ml first mixed solution from graduated cylinder top to container with pipettor;
(D) in graduated cylinder, inject the 35ml deionized water once more, after stirring 15s under the rotating speed of 50r/min, leave standstill 40min, and pipette out 35ml second mixed solution from graduated cylinder top to container with pipettor;
(E) in graduated cylinder, inject the 35ml deionized water once more, after stirring 15s under the rotating speed of 50r/min, leave standstill 40min, and pipette out 35ml the 3rd mixed solution from graduated cylinder top to container with pipettor;
(F) surplus solution in the graduated cylinder is screened with 3 μ m filter clothes, the filter cloth topper behind 120 ℃ of following dry 4h of temperature, is made the shell sheet; Shown in Fig. 3 C, as can be seen from the figure, the curved frustule sheet content of bridge reaches more than 80%, and surface micropore is clear, and integrity degree is higher.
(G) mixed solution in the container is screened with 3 μ m filter clothes, the filter cloth topper behind 120 ℃ of following dry 4h of temperature, is made endless belt; Shown in Fig. 3 D, as can be seen from the figure, the curved algal rim band content of bridge reaches more than 90%, and integrity degree is higher.
In the present invention, can extract the shell sheet of 0.4g in the curved algae of the bridge of 1g, the endless belt of 0.1g.
Embodiment 4Separation and Extraction little ring frustule sheet and endless belt from little ring algae
One, organic treatment step is removed in the diatom deactivation
(A) it is that 50% sulfuric acid mixes and obtains little ring algae suspension that the little ring algae that will culture is put into mass percent concentration;
The sulfuric acid that adds 40ml in the little ring algae of consumption: 1g;
(B) whizzer is put in the taking-up after 100 ℃ of temperature are incubated 30min down of diatom suspension; Behind centrifugal treating 8min under the rotating speed of 3500r/min, take out, remove supernatant liquid, obtain first mixture;
(C) in first mixture, add deionized water, behind centrifugal treating 12min under the rotating speed of 4500r/min, take out, remove supernatant liquid, obtain second mixture;
The deionized water that adds 50ml in first mixture of consumption: 10ml;
(D) in second mixture, add deionized water, behind centrifugal treating 12min under the rotating speed of 4500r/min, take out, remove supernatant liquid, obtain the 3rd mixture;
The deionized water that adds 50ml in second mixture of consumption: 10ml;
(E) in the 3rd mixture, add deionized water, behind centrifugal treating 12min under the rotating speed of 4500r/min, take out, remove supernatant liquid, obtain 4 mixture, promptly little ring algae crepis;
The deionized water that adds 50ml in first mixture of consumption: 10ml;
Two, the separating step of crepis mesochite sheet and endless belt
(A) little ring algae crepis is put into Glass Containers, the adding mass percent concentration is 95% dehydrated alcohol, and Glass Containers placed the ultrasonic cleaning machine, behind ultrasonic cleaning 30min under the condition of power 700W, operating frequency 25KHz, the employing aperture is that the filter cloth of 5 μ m separates, and filters and obtains the filter cloth topper;
The dehydrated alcohol that adds 60ml in the diatom crepis of consumption: 1g;
(B) with the filter cloth topper at 150 ℃ down behind the dry 6h, make the dried powder that contains shell sheet and endless belt;
(C) the dried powder adding of 2g is equipped with in the graduated cylinder of 50ml deionized water, after stirring 10s under the rotating speed of 100r/min, is leaving standstill 10min, and pipetting out 35ml first mixed solution from graduated cylinder top to container with pipettor;
(D) in graduated cylinder, inject the 35ml deionized water once more, after stirring 10s under the rotating speed of 100r/min, leave standstill 15min, and pipette out 35ml second mixed solution from graduated cylinder top to container with pipettor;
(E) in graduated cylinder, inject the 35ml deionized water once more, after stirring 10s under the rotating speed of 100r/min, leave standstill 15min, and pipette out 35ml the 3rd mixed solution from graduated cylinder top to container with pipettor;
(F) surplus solution in the graduated cylinder is screened with 5 μ m filter clothes, the filter cloth topper behind 150 ℃ of following dry 6h of temperature, is made the shell sheet;
(G) mixed solution in the container is screened with 5 μ m filter clothes, the filter cloth topper behind 150 ℃ of following dry 6h of temperature, is made endless belt;
In the present invention, can extract the shell sheet of 0.6g in the little ring algae of 1g, the endless belt of 0.2g.
The shell sheet that adopts the inventive method to make can be as sorbent material, flocculating aids, nanocomposite optical device, medicament slow release device, biochip dna vector etc.
The endless belt that adopts the inventive method to make can be made optics, communication micro element, as focus wave strap, the optical fiber micro-ring resonator of X-ray microscope.
Diatom becomes the research focus in micro-nano field because of its outstanding microtexture and silicon material, and the separation and Extraction of different-shape endless belt and shell sheet is for micro-nano research and application provide new material.
Claims (4)
1. the method for separation and Extraction shell sheet and endless belt from a diatomite or a diatom is characterized in that comprising that step has:
(A) crepis that diatomite or diatom are obtained after pre-treatment is put into Glass Containers, adds mass percent concentration and be 95% dehydrated alcohol; And Glass Containers placed the ultrasonic cleaning machine, behind ultrasonic cleaning 30min～60min under the condition of power 700W～1000W, operating frequency 25KHz～40KHz, adopting the aperture is that the filter cloth of 3 μ m～20 μ m separates, and filters and obtains the filter cloth topper;
The dehydrated alcohol that adds 50ml～100ml in the crepis of consumption: 1g;
(B) with the filter cloth topper behind dry 4h～6h under 110 ℃～150 ℃ temperature, make the dried powder that contains shell sheet and endless belt;
(C) the dried powder adding of 1g～2g is equipped with in the graduated cylinder of 50ml deionized water, after stirring 5s～20s under the rotating speed of 50r/min～100r/min, leaves standstill 10min～40min, and pipette out 35ml first mixed solution from graduated cylinder top to container with pipettor;
(D) in graduated cylinder, inject the 35ml deionized water once more, after stirring 5s～20s under the rotating speed of 50r/min～100r/min, leave standstill 10～40min, and pipette out 35ml second mixed solution from graduated cylinder top to the container of step (C) with pipettor;
(E) in graduated cylinder, inject the 35ml deionized water once more, after stirring 5s～20s under the rotating speed of 50r/min～100r/min, leave standstill 10～40min, and pipette out 35ml the 3rd mixed solution from graduated cylinder top to the container of step (C) with pipettor;
(F) surplus solution in the graduated cylinder is screened with 3 μ m～20 μ m filter clothes, the filter cloth topper behind dry 4h～6h under 110 ℃～150 ℃ temperature, is made the shell sheet;
(G) mixed solution in the container is screened with 3 μ m～20 μ m filter clothes, the filter cloth topper behind dry 4h～6h under 110 ℃～150 ℃ temperature, is made endless belt; Described mixed solution is the summation of first mixed solution, second mixed solution and the 3rd mixed solution;
Can extract the shell sheet of 0.2g～0.6g in the crepis of 1g, the endless belt of 0.1g～0.3g.
2. according to claim 1 from diatomite or diatom the method for separation and Extraction shell sheet and endless belt, it is characterized in that: the pattern and the microtexture that adopt shell sheet that method separation and Extraction of the present invention goes out and endless belt all to keep original kind diatom.
3. according to claim 1 from diatomite or diatom the method for separation and Extraction shell sheet and endless belt, it is characterized in that in step (A), to the pre-treatment step of diatom be:
(A) diatom being put into mass percent concentration is that 50%～70% sulfuric acid mixes and obtains diatom suspension;
The sulfuric acid that adds 40ml～60ml in the diatom of consumption: 1g;
(B) diatom suspension is taken out and puts into whizzer after being incubated 30min～60min under 90 ℃～100 ℃ temperature; Behind centrifugal treating 8min～20min under the rotating speed of 3000r/min～7000r/min, take out, remove supernatant liquid, obtain first mixture;
(C) in first mixture, add deionized water, behind centrifugal treating 8min～20min under the rotating speed of 3000r/min～7000r/min, take out, remove supernatant liquid, obtain second mixture;
The deionized water that adds 40ml～60ml in first mixture of consumption: 10ml;
(D) in second mixture, add deionized water, behind centrifugal treating 8min～20min under the rotating speed of 3000r/min～7000r/min, take out, remove supernatant liquid, obtain the 3rd mixture;
The deionized water that adds 40ml～60ml in second mixture of consumption: 10ml;
(E) add deionized water in the 3rd mixture, behind centrifugal treating 8min～20min under the rotating speed of 3000r/min～7000r/min, take out, remove supernatant liquid, obtain 4 mixture, this 4 mixture is crepis;
The deionized water that adds 40ml～60ml in the 3rd mixture of consumption: 10ml.
4. according to claim 1 from diatomite or diatom the method for separation and Extraction shell sheet and endless belt, it is characterized in that in step (A) being to diatomaceous pre-treatment step:
Commercially available diatomite is put into Glass Containers, and the adding mass percent concentration is 95% dehydrated alcohol, behind ultrasonic cleaning 10min～30min under the condition of power 700W～1000W, operating frequency 25KHz～40KHz, the use aperture is that the filter cloth of 5 μ m～100 μ m separates, filtration obtains filter cloth topper, i.e. crepis;
The dehydrated alcohol that adds 50～100ml in the diatomite of consumption: 1g.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010033699A CN101792145B (en) | 2010-01-11 | 2010-01-11 | Method for separating and extracting shell pieces and clitellum from kieselguhr or diatoms |
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| CN201010033699A CN101792145B (en) | 2010-01-11 | 2010-01-11 | Method for separating and extracting shell pieces and clitellum from kieselguhr or diatoms |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826556A (en) * | 2012-09-21 | 2012-12-19 | 海南大学 | Method for separating and extracting diatom shells from diatom |
| CN106430089A (en) * | 2016-09-27 | 2017-02-22 | 中国农业大学 | Diatom shell micro particle single layer array method |
| CN108101067A (en) * | 2017-12-22 | 2018-06-01 | 燕山大学 | A kind of simple and easy method that siliceous housing is extracted from Skeletonema Costatum |
| CN108220345A (en) * | 2018-01-10 | 2018-06-29 | 中国海洋大学 | A kind of manufacturing method of 3D structural levels porous silica microparticle |
-
2010
- 2010-01-11 CN CN201010033699A patent/CN101792145B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826556A (en) * | 2012-09-21 | 2012-12-19 | 海南大学 | Method for separating and extracting diatom shells from diatom |
| CN102826556B (en) * | 2012-09-21 | 2014-07-09 | 海南大学 | Method for separating and extracting diatom shells from diatom |
| CN106430089A (en) * | 2016-09-27 | 2017-02-22 | 中国农业大学 | Diatom shell micro particle single layer array method |
| CN108101067A (en) * | 2017-12-22 | 2018-06-01 | 燕山大学 | A kind of simple and easy method that siliceous housing is extracted from Skeletonema Costatum |
| CN108220345A (en) * | 2018-01-10 | 2018-06-29 | 中国海洋大学 | A kind of manufacturing method of 3D structural levels porous silica microparticle |
| CN108220345B (en) * | 2018-01-10 | 2022-05-03 | 中国海洋大学 | Manufacturing method of porous silicon dioxide microparticles with 3D structure level |
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| Publication number | Publication date |
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| CN101792145B (en) | 2012-10-10 |
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