CN107973542A - A kind of Leaking Stoppage in Coal Mine wind microorganism self-healing capsule and preparation method thereof and its application - Google Patents
A kind of Leaking Stoppage in Coal Mine wind microorganism self-healing capsule and preparation method thereof and its application Download PDFInfo
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- CN107973542A CN107973542A CN201710962128.XA CN201710962128A CN107973542A CN 107973542 A CN107973542 A CN 107973542A CN 201710962128 A CN201710962128 A CN 201710962128A CN 107973542 A CN107973542 A CN 107973542A
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- leaking stoppage
- coal mine
- healing capsule
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/10—Coating or impregnating
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
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Abstract
A kind of Leaking Stoppage in Coal Mine wind microorganism self-healing capsule and preparation method thereof and its application; bacterial spore dry powder is uniformly dispersed in water; adaptable substrate is chosen according to the species of bacterial spore; necessarily matched with substrate according to bacterial spore; substrate is added in finely dispersed mixed liquor; stirring evenly makes its agglomerating; doughy mix is slowly added into multifunction granulating machine and is extruded; open cooling system; keep temperature of charge; the strip of extrusion is added to it is round as a ball in spheronizator, screening, dry to obtain particulate；Microorganism self-healing capsule is prepared using vacuum impregnation technology or interfacial polymerization by particulate and wall material, microorganism self-healing capsule is used in mixed way with wind leaking stoppage material of main part, once there is crack in concrete, the gemma of material internal is just activated, carry out normal metabolism, constantly induction precipitation of calcium carbonate, realizes the selfreparing in crack.
Description
Technical field
The present invention relates to a kind of Leaking Stoppage in Coal Mine wind material, more particularly to a kind of Leaking Stoppage in Coal Mine wind microorganism self-healing capsule and
Its preparation method and its application.
Background technology
Spontaneous combustionof coal is the major hidden danger for threatening China's coal-mine safety in production.Wind leaking stoppage is that prevention the important of spontaneous combustionof coal is arranged
Apply.Cement class material, coal ash foam material, macromolecule sprayed on material, colloid, clay composite material, foamed material and height
Molecular flexibility body is currently used wind leaking stoppage material, these materials play important work in terms of Safety of Coal Mine Production is ensured
With.However, existing wind leaking stoppage material inevitably results from a large amount of microfissures under the effect of ore deposit pressure, if cannot send out in time
Now and these microfissures are repaired, it will link up goaf, form the passage that leaks out, and then trigger goaf coal spontaneous combustion, cause to be difficult to
The economic loss and casualties retrieved.
For wind leaking stoppage material crack, current main restorative procedure is repaired for subsequent reparation or timing, but this
Passive planned repair mode be directed to macroscopic crack mostly, and reparation position is mostly at material rapid wear, and is repaired
The limitation of the problems such as material construction technology, location of cracks are also easy to produce secondary cracking.In addition, in actual wind leaking stoppage material, its
Inside is there are many micro-cracks, due to the limitation of current Detection Techniques, detect and repair these micro-cracks still suffer from it is larger
Difficulty.Therefore, it is necessary to develop it is a kind of have crack self diagnosis, the wind leaking stoppage material system of selfreparing, to meet current coal
The particular/special requirement of ore deposit wind leaking stoppage zone material.
The content of the invention
The purpose of the present invention is the deficiency of Leaking Stoppage in Coal Mine wind material in above technical background, there is provided one kind makes full use of micro- life
Thing, structure have crack self diagnosis and selfreparing, environmentally protective wind leaking stoppage material, and preparation method thereof, and its application concurrently.Exist
Alkaline-resisting thalline gemma and its nutriment are mixed in the whipping process of concrete, once there is crack in concrete, material internal
Gemma is just activated, and carries out normal metabolism, constantly induces precipitation of calcium carbonate, realize the selfreparing in crack.
Above-mentioned purpose is achieved by the following technical solution：
A kind of Leaking Stoppage in Coal Mine wind microorganism self-healing capsule, its feature are that the microorganism self-healing capsule includes cyst wall, cyst wall
In be wrapped in microbial spore, substrate, its preparation method is as follows：
（1）Adaptable substrate is chosen according to the species of bacterial spore, is 1 according to the mass ratio of bacterial spore and substrate：100-
120 mix, and the dry powder of bacterial spore containing 2.5-3.5g in every 150g water, makes it be uniformly dispersed in water, be then added to substrate
In finely dispersed mixed liquor, stirring evenly makes its agglomerating；
（2）Above-mentioned doughy mix is slow（The speed of about 50g/min）It is added in multifunction granulating machine and extrudes, comminutor net
Orifice plate mesh number is 30-45 mesh, while opens cooling system, and it is 2-5 DEG C to keep temperature of charge, and the strip of extrusion is added to rolling
Round as a ball in circular knitting machine, finally again by 35-40 mesh sieves point, drying is that can obtain the single particulate of particle diameter at 2-5 DEG C；
（3）According to particulate：The mass ratio of wall material is 1:The ratio of 0.6-1.4 weighs wall material；
（4）Microorganism self-healing capsule is prepared using vacuum impregnation technology or interfacial polymerization.
The cyst wall thickness of microorganism self-healing capsule described above is 0.5-8 μm, and the outer radius of capsule is 3-110 μm.
Microbial spore described above is selected from Pasteur's gemma sarcine, Bacillus pasteurii, Bacillus sphaericus, Coriolis
One or more in bacillus, false bacillus firmus, bacillus subtilis and nitrobacteria.
Substrate described above for inosine, dusty yeast, hydroxypropyl methyl cellulose, microcrystalline cellulose, calcium lactate, calcium nitrate,
One or more in calcium formate or calcium acetate.
Step described above（4）During the middle preparation using vacuum impregnation technology, wall material is porous light aggregate, sodium alginate, silicon
At least one of gel, clay particle, diatomite, haydite；When being prepared using interfacial polymerization, wall material is epoxy resin, three
At least one of paracyanogen amine-formaldehyde resin, Lauxite, polyurethane, polyvinyl alcohol and cellulose acetate-butyrate.
In addition, the application of the Leaking Stoppage in Coal Mine wind microorganism self-healing capsule described in more than one, its feature are micro- life
Thing self-healing capsule is used in mixed way with wind leaking stoppage material of main part, and wherein wind leaking stoppage material of main part is cement class material, fine coal blub
At least one of foam material, macromolecule sprayed on material.
Compared with existing Leaking Stoppage in Coal Mine wind material, Leaking Stoppage in Coal Mine wind microorganism self-healing capsule described herein is being applied
In there are following outstanding advantages：
1）Microorganism self-healing system can realize the automatic detection in crack, automatic healing；
2）Bacterium can repeatedly repair crack, and healing properties have sustainability；
3）The calcium carbonate that bacterium mineralising is formed, matches with material of main part, environmentally protective, pollution-free；
4）Capsule wraps up a kind of protective layer outside bacterium, can be very good to protect bacteria from the influence of external environment, improves
The service life of microorganism；
5）Without additional culture medium, it is possible to achieve the intelligence reparation of material；
6）Selfreparing occur when, a small amount of microbial spore that only crack influences is activated, other microbial spores still in
Resting state, makes self-repairing system permanently effective, while avoids the microbial spore of mortality to wind leaking stoppage material of main part
The influence of intensity；
7）This self-repairing system can realize big model since microbial capsules are largely evenly distributed in wind leaking stoppage material of main part
Enclose, uniformly repair.
Brief description of the drawings
Fig. 1 repairs crack schematic diagram for microbial mineralization diagenesis；
Fig. 2 is microorganism induction tosca schematic diagram.
Embodiment
In order to which technical scheme is more clearly understood, the present invention is made further with reference to embodiment
Bright, following embodiments are only embodiment citing, and the protection domain of the application is not restricted to following embodiments scope.
Embodiment 1：Microbial spore is Coriolis subtilis spore used by the present embodiment, and selected wall material is asphalt mixtures modified by epoxy resin
At least one of fat, melamine formaldehyde resin, Lauxite, polyurethane, polyvinyl alcohol and cellulose acetate-butyrate, institute
The selective plugging material of main part that leaks out is cement class material.
Inosine 5g, dusty yeast 25g, hydroxypropyl methyl cellulose 5g, microcrystalline cellulose 150g are weighed, is uniformly mixed, at the same time
Take 150g water and adding 3g spore dry powder makes its dispersed, the 150g calcium nitrate weighed is dissolved in again is dispersed with spore afterwards
In the water of son, liquid solution is then added to mixed uniformly inosine, dusty yeast, hydroxypropyl methyl cellulose, microcrystalline cellulose
In element, and stirring evenly makes its agglomerating, and doughy mix is slowly added into multifunction granulating machine and is extruded, selected from mesh
Number is the mesh plate of 40 mesh, while opens cooling system, and it is 2-5 DEG C to keep temperature of charge, and the strip of extrusion is added to rolling
Carried out in circular knitting machine it is round as a ball, finally again by screening and further low temperature drying i.e. can obtain the single particulate of particle diameter, according to particulate：
Wall material=1:1.2 weigh wall material, and then particulate is placed in beaker with wall material and is uniformly mixed, and the mixture is placed in 50 DEG C of water
30min or so is kept the temperature in bath, 2.7g curing agent KH-792 is added, makes epoxy resin cure, and is stirred evenly, equally by it
Progress precuring 40min in 50 DEG C of water-baths is placed in, then the good mixture of precuring is transferred to containing the poly- diformazans of 150-250g
In the three-necked flask of base silicone oil, stirred with the rotating speed of 300rpm, mixture is uniformly dispersed, concurrently set suitable bath temperature
For 50 DEG C and constant temperature is kept, by the curing reaction of 2h, makes wall material completion of cure；Products therefrom is finally filtered into simultaneously washes clean
The polydimethyl siloxane fluid on surface, and dried in the low temperature drying case less than 50 DEG C, that is, self-healing capsule is obtained, this is interface
It is prepared by polymerization.
Microorganism selfreparing capsule is poured into water first, is stirred until capsule is dispersed.Then water is poured into stirring
In device, cement class material needed for addition, pours into mould after mixing, smoothes out, and conserves 24h, then demoulds, at ambient temperature
28d is conserved, the cuboid sample of 40 × 40 × 160mm is made in cement material.
The sample of 3 groups of maintenance 28d is taken, every group 3 pieces, precompressed destruction is carried out, produces crack, water and air is entered by crack,
Then it is 95% the sample of destruction to be placed on humidity, and temperature is in 20 DEG C of fog room, and capsule is interior as gash fracture discharges
The bacterial spore in portion, under suitable environment, the activity of spore is excited out, produces precipitation of calcium carbonate.Three pieces of sample difference
Conserve 3d, 7d and 28d.There is calcite generation to the SEM observation discoveries of sample crack, and curing time is longer, and calcite is brilliant
Body is more.
Embodiment 2：Microbial spore is Pasteur's gemma sarcine, Bacillus pasteurii, ball used by the present embodiment
At least one of shape bacillus, Coriolis bacillus, false bacillus firmus, bacillus subtilis and nitrobacteria, institute
Wall material is selected as at least one of porous light aggregate, sodium alginate, Silica hydrogel, clay particle, diatomite, haydite, institute's selective plugging
The material of main part that leaks out is coal ash foam material.
Weigh dusty yeast 3g, peptone 5g, deionized water 1000mL preparing microorganism culture mediums, by the way that NaOH solution is added dropwise
It is 9.0 to adjust pH value.After 121 DEG C of high-temperature sterilization 30min are cooled to room temperature, Bacillus pasteurii is inoculated with, while add 30mL
Concentration is the urea liquid of 4mol/L.The shaken cultivation at 30 DEG C, frequency of oscillation 170r/min, cultivates 24h.
Porous light aggregate crosses 0.075mm and sieves and wash, and particle size range 0.075mm-4.75mm, weighs 300g and be added to
In the above-mentioned inoculums of 375g, porous light aggregate is set to soak 8h, frequency of oscillation 130r/min under oscillating condition.
300mL urea calcium source solution is added into above-mentioned porous light aggregate and bacterium mixed-culture medium.Calcium source selects chlorine
Change calcium.Urea concentration is 0.5mol/L, calcium chloride concentration 0.5mol/L in urea calcium source solution.Taken out after vibration 24h porous
Aglite, frequency of oscillation 130r/min.
Porous light aggregate after processing is dried to constant weight while in heat gun under artificial stirring, dried
Instilled in journey admittedly containing the polycarboxylic acid series high efficiency water reducing agent that mass fraction is 30%, be 2-5mL per 1000g aggregates volume, this is vacuum
It is prepared by infusion process.
Porous light aggregate after the microbiological treatment that the present embodiment is obtained is according to according to cement mortar rate 1:5th, water-cement ratio
0.97 is made the cuboid mortar specimen of 40 × 40 × 160mm, conserves 24h, then demoulds, conserve 28d at ambient temperature.
The sample of 3 groups of maintenance 28d is taken, every group 3 pieces, precompressed destruction is carried out, produces crack, water and air is entered by crack,
Then it is 95% the sample of destruction to be placed on humidity, and temperature is in 20 DEG C of fog room, and the bacterium in porous light aggregate is suitable
Under suitable environment, its activity is excited out, produces precipitation of calcium carbonate.Three pieces of samples conserve 3d, 7d and 28d respectively.To sample
There is calcite generation in crack with SEM observation discoveries, and curing time is longer, and calcite crystal is more.
Claims (10)
- A kind of 1. Leaking Stoppage in Coal Mine wind microorganism self-healing capsule, it is characterised in that：The microorganism self-healing capsule includes cyst wall, capsule Microbial spore, substrate are wrapped in wall.
- A kind of 2. Leaking Stoppage in Coal Mine wind microorganism self-healing capsule according to claim 1, it is characterised in that：The microorganism The cyst wall thickness of self-healing capsule is 0.5-8 μm, and the outer radius of capsule is 3-110 μm.
- A kind of 3. Leaking Stoppage in Coal Mine wind microorganism self-healing capsule according to claim 1 or 2, it is characterised in that：It is described micro- The cyst material of biological self-healing capsule is selected from epoxy resin, porous light aggregate, sodium alginate, Silica hydrogel, clay particle, silicon Diatomaceous earth, haydite, melamine formaldehyde resin, one kind in Lauxite, polyurethane, polyvinyl alcohol and cellulose acetate-butyrate It is or a variety of.
- A kind of 4. Leaking Stoppage in Coal Mine wind microorganism self-healing capsule according to claim 1 or 2, it is characterised in that：It is described micro- Biological spore is selected from Pasteur's gemma sarcine, Bacillus pasteurii, Bacillus sphaericus, Coriolis bacillus, false strong bud One or more in spore bacillus, bacillus subtilis and nitrobacteria.
- A kind of 5. Leaking Stoppage in Coal Mine wind microorganism self-healing capsule according to claim 1 or 2, it is characterised in that：The bottom Thing is in inosine, dusty yeast, hydroxypropyl methyl cellulose, microcrystalline cellulose, calcium lactate, calcium nitrate, calcium formate or calcium acetate It is one or more of.
- A kind of 6. preparation method of Leaking Stoppage in Coal Mine wind microorganism self-healing capsule as claimed in claim 1 or 2, it is characterised in that Preparation method is as follows：（1）Substrate is chosen according to the species of bacterial spore, is 1 according to the mass ratio of bacterial spore and substrate：100-120 is mixed, The dry powder of bacterial spore containing 2.5-3.5g in per 150g water, makes it be uniformly dispersed in water, is then added to substrate and is uniformly dispersed Mixed liquor in, stirring evenly makes its agglomerating；（2）Above-mentioned doughy mix is added in multifunction granulating machine and is extruded, comminutor mesh plate mesh number is 30-45 mesh, together When open cooling system, it is 2-5 DEG C to keep temperature of charge, the strip of extrusion is added to it is round as a ball in spheronizator, finally after 5-40 mesh sieves point, the single particulate of particle diameter is can obtain in 2-5 DEG C of drying；（3）According to particulate：The mass ratio of wall material is 1:The ratio of 0.6-1.4 weighs wall material；（4）Microorganism self-healing capsule is prepared using vacuum impregnation technology or interfacial polymerization.
- A kind of 7. preparation method of Leaking Stoppage in Coal Mine wind microorganism self-healing capsule according to claim 6, it is characterised in that: Step（1）In, when bacterial spore is Pasteur's gemma sarcine, Bacillus pasteurii, Bacillus sphaericus, Coriolis gemma bar Substrate is when bacterium, false bacillus firmus, bacillus subtilis：Inosine, dusty yeast, hydroxypropyl methyl cellulose, microcrystalline cellulose One or more in element, calcium lactate, calcium formate, calcium acetate and calcium nitrate, when bacterial spore is nitrobacteria, substrate is：Ferment One or more in female powder, calcium nitrate, hydroxypropyl methyl cellulose, microcrystalline cellulose, calcium lactate, calcium formate or calcium acetate.
- A kind of 8. preparation method of Leaking Stoppage in Coal Mine wind microorganism self-healing capsule according to claim 6, it is characterised in that: Step（4）During the middle preparation using vacuum impregnation technology, wall material is porous light aggregate, sodium alginate, Silica hydrogel, clay particle, silicon At least one of diatomaceous earth, haydite.
- A kind of 9. preparation method of Leaking Stoppage in Coal Mine wind microorganism self-healing capsule according to claim 6, it is characterised in that: Step（4）During the middle preparation using interfacial polymerization, wall material is epoxy resin, melamine formaldehyde resin, Lauxite, poly- ammonia At least one of ester, polyvinyl alcohol and cellulose acetate-butyrate.
- 10. a kind of application of Leaking Stoppage in Coal Mine wind microorganism self-healing capsule as described in claim 1 or 2 or 7 or 8 or 9, it is special Sign is：The microorganism self-healing capsule is mixed with cement class material and/or coal ash foam material and/or macromolecule sprayed on material Close and use.
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| CN108558260A (en) * | 2018-05-24 | 2018-09-21 | 中交四航工程研究院有限公司 | A kind of self union concrete complex enzyme microencapsulation material and preparation method thereof |
| CN108823198A (en) * | 2018-07-20 | 2018-11-16 | 山东科技大学 | A kind of microcapsules and preparation method thereof that may continue from repairing Leaking Stoppage in Coal Mine wind material crack |
| CN108947308A (en) * | 2018-07-22 | 2018-12-07 | 黑龙江工程学院 | A kind of concrete external doped dose of permanent seal cooling |
| CN109666669A (en) * | 2018-12-21 | 2019-04-23 | 滨州学院 | A kind of preparation method and application method of the dust Explosion suppressant based on microbial capsules |
| CN109943164A (en) * | 2019-01-25 | 2019-06-28 | 京润矿安科技(北京)有限公司 | A kind of sprayed on material and preparation method thereof suitable for coal mine down-hole tunnel |
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