CN109455954A - The preparation method and applications of surface deposition Organic Iron treated basalt fiber - Google Patents
The preparation method and applications of surface deposition Organic Iron treated basalt fiber Download PDFInfo
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- CN109455954A CN109455954A CN201811372423.0A CN201811372423A CN109455954A CN 109455954 A CN109455954 A CN 109455954A CN 201811372423 A CN201811372423 A CN 201811372423A CN 109455954 A CN109455954 A CN 109455954A
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- basalt fibre
- iron
- organic iron
- organic
- basalt
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/66—Chemical treatment, e.g. leaching, acid or alkali treatment
-
- 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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F2003/001—Biological treatment of water, waste water, or sewage using granular carriers or supports for the microorganisms
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Microbiology (AREA)
- Engineering & Computer Science (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Water Supply & Treatment (AREA)
- Biodiversity & Conservation Biology (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention belongs to technical field of composite materials, it is related to micron order basalt fibre method of modifying, more particularly to a kind of preparation method of surface deposition Organic Iron treated basalt fiber, it include: that basalt fibre segment is immersed in removal of impurities in dilute hydrochloric acid solution, activates, then basalt fibre segment is wound in umbrella basalt fibre beam using stainless steel wire as core material, umbrella type basalt fibre beam is hung in reactor；Organic acid soln and iron salt solutions are prepared respectively, it is slowly added dropwise simultaneously, so that Organic Iron modifier solution liquid level is maintained on the umbrella type basalt fibre beam, after being added dropwise, continue 0.5~1 h of immersion, it then takes out, the modified basalt fibre of cleaning, drying to obtain Organic Iron, the Organic Iron modifying agent generates after being reacted by organic acid soln and iron salt solutions.Presently disclosed method is easy to operate, simple process, is suitable for industrialized production, and made Organic Iron treated basalt fiber is the novel purification of water quality microbe carrier of green.
Description
Technical field
The invention belongs to technical field of composite materials, it is related to micron order basalt fibre method of modifying, more particularly to a kind of
The preparation method and applications of surface deposition Organic Iron treated basalt fiber.
Background technique
Basalt fibre (Basalt fiber, BF) is a kind of high performance fibre material of micron order novel inorganic environmental protection,
It is passed through made of platinum-rhodium alloy bushing high speed pulling after high-temperature fusion as natural basalt.Domestic basalt storage capacity
It is abundant, it can satisfy the growth requirement of basalt fibre industry completely.Chinese patent is " a kind of de- based on basalt fibre filler
Nitrogen microorganism nest and its cultural method " (CN106277315A) refer to basalt fibre because its with better mechanical strength,
The advantages such as lower use cost and recoverable have been developed to the novel purification of water quality of one kind in recent years and use microorganism
Carrier material.But basalt fibre is a kind of inorfil, and surface is without carboxyl, hydroxyl isopolarity hydrophilic radical, surface hydrophilicity
Difference, electronegativity is higher and surface is smooth, and bioaffinity more takes second place compared with carbon fiber.Therefore basalt fibre is answered
Before engineering practice, need modified to its surface.
Fe ion can be used as the activator of enzyme in microorganism, promote the reaction rate of enzyme, and then keep microorganism secretion more
Extracellular polymeric (Extracellular polymeric substance, EPS).The main component of EPS is polysaccharide, albumen
Matter, nucleic acid and lipid etc. can play the agglutination of microorganism, so that more microorganisms are attached to carrier surface.Separately
On the one hand, Fe2+/Fe3+With positive charge, bacterium has negative electrical charge mostly in neutral conditions, thus can enhance carrier and bacterium
Between electrostatic attraction effect so that more microorganism is attached to carrier surface.
Therefore, the present invention proposes to use Organic Iron treated basalt fiber, and Organic Iron is uniformly sunk using liquid phase deposition
Product improves the bioaffinity of BF to the surface BF, promotes microorganism in the attachment behavior on Organic Iron treated basalt fiber surface,
And microorganism generates more extracellular polymerics because being influenced by Organic Iron, and extracellular polymeric plays agglutination to microorganism and makees
With, the membranaceous flocculate of formation is stronger on the surface MBF, and it is not easily to fall off, so that more microorganisms participate in purification of water quality,
And then improve sewage/wastewater treatment efficiency.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, the object of the present invention is to provide a kind of modified basalt of Organic Iron is fine
The preparation method of dimension, the disadvantage for overcoming basalt fibre bioaffinity general improves the surface property of BF, to realize micro- life
Object is in basalt fibre surface fast enriching.
In order to achieve the above object, The technical solution adopted by the invention is as follows:
A kind of preparation method of surface deposition Organic Iron treated basalt fiber, includes the following steps:
(1) it pre-processes: basalt fibre being cut into section, it is miscellaneous to remove surface to be immersed in 0.5~1.5 h in dilute hydrochloric acid solution
Matter, while playing the role of activating surface functional group, basalt fibre segment is then wound in umbrella using stainless steel wire as core material
Shape basalt fibre beam, wherein the basalt fibre is micro inorganic basalt fibre, 7~18 μm of filament diameter, preferably
13μm；The stainless steel wire be 304 stainless steel wires or 316 stainless steel wires, basalt fibre and stainless steel wire winding segment length 3~
5 cm, preferably 5 cm；The concentration of the dilute hydrochloric acid solution is 0.5~2 mol/L, preferably 1 mol/L；Soaking time preferably 1 h；
(2) it prepares treated basalt fiber: umbrella type basalt fibre beam being fixed on above reactor, it is made to hang on reaction
In device；Organic acid soln and iron salt solutions are prepared respectively, while being slowly added dropwise into reactor, so that Organic Iron modifier solution
Liquid level is on the umbrella type basalt fibre beam, after being added dropwise, continues 0.5~1 h of immersion, preferably 1 h；Then it takes
Out, the modified basalt fibre of cleaning, drying to obtain Organic Iron, the Organic Iron modifying agent is by above-mentioned organic acid soln and iron
It is generated after salting liquid reaction.
In the more excellent disclosed example of the present invention, organic acid described in step (2) is oxalic acid, citric acid, acetic acid etc., preferably oxalic acid；
The molysite is trivalent iron salt or ferrous salt, specially sulphate of iron or iron chloride salt, preferably sulfuric acid molysite；The Organic Iron changes
Property agent in the molar ratio (n:n, mol: mol) of acid ion and iron ion be 1:1~1.5:1, preferably 1.2:1.
Further, in the more excellent disclosed example of the present invention, the liquid phase deposition that Organic Iron treated basalt fiber uses can be with
Assisting magnetic or mechanical stirring, mixing speed controls 20~100 r/min, to guarantee that Organic Iron is uniform on basalt fibre surface
Deposition.
A further object of the invention is, prepared surface is deposited Organic Iron treated basalt fiber, as micro-
Bio-carrier is to sewage purification.
The bioaffinity of Organic Iron treated basalt fiber prepared by the present invention is commented by pure bacterium adsorption experiment
Estimate, the specific steps are as follows:
Bacillus subtilis (B. subtilis) (5 g/L of peptone, beef leach 3 g/L of object, chlorination to liquid medium within
Sodium 5 g/L, MnSO4·H25 mg/L of O, pH=7.0) in 30 DEG C of aerobic culture 10 h, revolving speed 150r/min, to obtain pair
Bacterial suspension (the OD in number growth period600=1.0), OD600It is divided for bacterial suspension under 600 nm wavelength with ultraviolet-visible
The absorbance of photometer measurement.It is contained being added in superclean bench after basalt fibre segment (0.1 g, 5 cm) sterilization treatment
In the conical flask for having 50mL fluid nutrient medium, it is added 100 μ l'sB. subtilisSuspension (OD600=1.0), in isothermal vibration
12 h of aerobic culture in shaking table, cultivation temperature are 30 DEG C, and revolving speed is 150 r/min.Sample is taken out after 12 h, using 0.02 M
PBS solution (pH=7.2) cleans 3 times, is placed in 4% formalin and fixes 24 h(4 DEG C, is protected from light).Then, sample is subjected to second
Alcohol serial dehydration handles (25%, 50%, 75%, 95%, 100%, per 15 min of stage), and freeze-drying is placed in SEM electricity microscopic observation bacterium
Adsorption effect.
Through the modified basalt fibre of Organic Iron, surface is rich in iron ion, microorganism secretion can be promoted more extracellular
Polymer realizes microorganism in basalt to play the role of being aggregated microorganism on Organic Iron treated basalt fiber surface
The membranaceous flocculate of fiber surface fast enriching, formation is stronger on the surface MBF, not easily to fall off, so that more microorganism ginsengs
With into purification of water quality, and then improve sewage/wastewater treatment efficiency.
Beneficial effect
The present invention uses liquid phase deposition in one layer of Organic Iron of basalt fibre surface uniform deposition, so that basalt fibre surface
Roughness increases；Basalt raw material is sufficient, at low cost, and basalt fibre production technology is environmentally protective, and Organic Iron modifying agent is free of
Any poisonous and harmful substances, presently disclosed method is easy to operate, and simple process is easy to spread, is suitable for industrialized production, made
The Organic Iron treated basalt fiber obtained is a kind of novel purification of water quality microbe carrier of green.
Detailed description of the invention
Fig. 1 Organic Iron treated basalt fiber preparation flow schematic diagram；
Fig. 2 MBF-3 surface microscopic topographic figure (SEM)；
The bacterial adsorption effect picture (SEM) of Fig. 3 basalt fibre.
Specific embodiment
The following describes the present invention in detail with reference to examples, so that those skilled in the art more fully understand this hair
It is bright, but the invention is not limited to following embodiments.
Embodiment 1
(1) basalt fibre is cut into the segment of 5 cm, is immersed in 1 h in the hydrochloric acid of 1M, is with 304 stainless steel wires
Basalt fibre segment is wound in umbrella type basalt fibre beam by core material.
(2) umbrella type basalt fibre beam is placed in a beaker, is fixed on beaker upper end with rope, is hung vertically in it
In beaker.Citric acid and ferric sulfate are weighed respectively, is configured to citric acid solution and ferrum sulfuricum oxydatum solutum, wherein acid group in citric acid
The molar ratio (n:n, mol: mol) of iron ion is 1.5:1 in ion and ferrum sulfuricum oxydatum solutum.To the burning for filling basalt fibre beam
Citric acid solution and ferrum sulfuricum oxydatum solutum is slowly added dropwise simultaneously at normal temperature in cup, beaker is built in magnetic stirring apparatus, is slightly stirred
It mixes, after solution is all added dropwise, continues to impregnate 1 h, so that ironic citrate uniform deposition is on the surface BF.It is fine to take out basalt
Dimension with deionized water gently clean the surface suspended state organoiron compound, and is allowed to cleaning to neutrality, and naturally dry is had
The modified basalt fibre (MBF-1) of machine iron.
Embodiment 2
(1) basalt fibre is cut into the segment of 20 cm, 1 h in the hydrochloric acid of 0.5 M is immersed in, with 304 stainless steels
Basalt fibre segment is wound in umbrella type basalt fibre beam for core material by silk.
(2) umbrella type basalt fibre beam is placed in a beaker, is fixed on beaker upper end with band, is hung vertically in it
In beaker.Acetum and ferrous sulfate solution are prepared respectively, wherein acid ion and ferrous iron in ferrous sulfate solution in acetic acid
The molar ratio (n:n, mol: mol) of ion is 1.5:1.It is slow simultaneously at normal temperature into the beaker for filling basalt fibre beam
Acetum is added dropwise and ferrous sulfate solution, beaker are built in magnetic stirring apparatus, gentle agitation is all added dropwise to solution
After continue impregnate 1 h so that ferrous acetate uniform deposition is on the surface BF.Basalt fibre is taken out, is gently cleaned with deionized water
Surfactant suspension state organoiron compound, and cleaning is allowed to neutrality, naturally dry is to obtain the modified basalt fibre of Organic Iron
(MBF-2).
Embodiment 3
(1) basalt fibre is cut into the segment of 10 cm, 1 h in the hydrochloric acid of 1 M is immersed in, with 316 stainless steel wires
Basalt fibre segment is wound in umbrella type basalt fibre beam for core material.
(2) umbrella type basalt fibre beam is placed in a beaker, is fixed on beaker upper end with band, is hung vertically in it
In beaker.Oxalic acid solution and ferrous sulfate solution are prepared respectively, wherein acid ion and ferrous iron in ferrous sulfate solution in oxalic acid
The molar ratio (n:n, mol: mol) of ion is 1.2:1.It is slow simultaneously at normal temperature into the beaker for filling basalt fibre beam
Oxalic acid solution is added dropwise and ferrous sulfate solution, beaker are built in magnetic stirring apparatus, gentle agitation is all added dropwise to solution
After continue impregnate 1 h so that ferrous oxalate uniform deposition is on the surface BF.Basalt fibre is taken out, is gently cleaned with deionized water
Surfactant suspension state organoiron compound, and cleaning is allowed to neutrality, naturally dry is to obtain the modified basalt fibre of Organic Iron
(MBF-3).
Embodiment 4
(1) basalt fibre is cut into the segment of 15 cm, 0.5 h in the hydrochloric acid of 1 M is immersed in, with 304 stainless steels
Basalt fibre segment is wound in umbrella type basalt fibre beam for core material by silk.
(2) umbrella type basalt fibre beam is placed in a beaker, is fixed on beaker upper end with band, is hung vertically in it
In beaker.Oxalic acid solution and solution of ferrous chloride are prepared respectively, wherein acid ion and ferrous iron in solution of ferrous chloride in oxalic acid
The molar ratio (n:n, mol: mol) of ion is 1:1.It is slowly dripped simultaneously at normal temperature into the beaker for filling basalt fibre beam
Add oxalic acid solution and solution of ferrous chloride, continues to impregnate 0.5 h after solution is all added dropwise, so that ferrous oxalate uniformly sinks
Product is on the surface BF.Basalt fibre is taken out, with deionized water gently clean the surface suspended state organoiron compound, and is allowed to clean
To neutrality, naturally dry is to obtain the modified basalt fibre (MBF-4) of Organic Iron.
It can be seen that by attached drawing 3, the bioaffinity of Organic Iron treated basalt fiber significantly improves, and Organic Iron can promote micro-
Biology adheres on its surface, and the biomass of basalt fibre surface attachment obviously increases.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification is applied directly or indirectly in other relevant technical fields,
Similarly it is included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of surface deposition Organic Iron treated basalt fiber, which comprises the steps of:
(1) it pre-processes: basalt fibre being cut into section, is immersed in 0.5~1.5h in dilute hydrochloric acid solution；Then with stainless steel wire
Basalt fibre segment is wound in umbrella basalt fibre beam for core material, wherein the basalt fibre is micro inorganic
Basalt fibre, 7~18 μm of filament diameter；Basalt fibre and stainless steel wire wind 3~5 cm of segment length；The dilute hydrochloric acid is molten
The concentration of liquid is 0.5~2 mol/L；
(2) it prepares treated basalt fiber: umbrella type basalt fibre beam being fixed on above reactor, it is made to hang on reaction
In device；Organic acid soln and iron salt solutions are prepared respectively, while being slowly added dropwise into reactor, so that Organic Iron modifier solution
Liquid level is on the umbrella type basalt fibre beam, after being added dropwise, continues 0.5~1 h of immersion, preferably 1 h；Then it takes
Out, the modified basalt fibre of cleaning, drying to obtain Organic Iron, the Organic Iron modifying agent is by above-mentioned organic acid soln and iron
It is generated after salting liquid reaction.
2. the preparation method of surface deposition Organic Iron treated basalt fiber according to claim 1, it is characterised in that: step
(1) described that basalt fibre is cut into section, it is immersed in 1 h in dilute hydrochloric acid solution.
3. the preparation method of surface deposition Organic Iron treated basalt fiber according to claim 1, it is characterised in that: step
(1) basalt fibre is micro inorganic basalt fibre, 13 μm of filament diameter.
4. the preparation method of surface deposition Organic Iron treated basalt fiber according to claim 1, it is characterised in that: step
(1) basalt fibre and stainless steel wire wind 5 cm of segment length.
5. the preparation method of surface deposition Organic Iron treated basalt fiber according to claim 1, it is characterised in that: step
(1) concentration of the dilute hydrochloric acid solution is 1 mol/L.
6. the preparation method of surface deposition Organic Iron treated basalt fiber according to claim 1, it is characterised in that: step
(2) organic acid is oxalic acid, citric acid, acetic acid, preferably oxalic acid.
7. the preparation method of surface deposition Organic Iron treated basalt fiber according to claim 1, it is characterised in that: step
(2) molysite is trivalent iron salt or ferrous salt, specially sulphate of iron or iron chloride salt, preferably sulfuric acid molysite；It is described organic
The molar ratio of acid ion and iron ion is 1:1~1.5:1, preferably 1.2:1 in iron modifying agent.
8. the preparation method of surface deposition Organic Iron treated basalt fiber according to claim 1, it is characterised in that: step
(2) liquid phase deposition that the Organic Iron treated basalt fiber uses, assisting magnetic or mechanical stirring, mixing speed 20~
100 r/min。
9. surface made from -8 any the methods deposits Organic Iron treated basalt fiber according to claim 1.
10. a kind of application of deposition Organic Iron treated basalt fiber in surface as claimed in claim 9, it is characterised in that: by it
As microbe carrier to sewage purification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811372423.0A CN109455954A (en) | 2018-11-19 | 2018-11-19 | The preparation method and applications of surface deposition Organic Iron treated basalt fiber |
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| CN201811372423.0A CN109455954A (en) | 2018-11-19 | 2018-11-19 | The preparation method and applications of surface deposition Organic Iron treated basalt fiber |
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| CN201811372423.0A Pending CN109455954A (en) | 2018-11-19 | 2018-11-19 | The preparation method and applications of surface deposition Organic Iron treated basalt fiber |
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