CN105506782B - A kind of preparation method of porous basalt fiber - Google Patents
A kind of preparation method of porous basalt fiber Download PDFInfo
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- CN105506782B CN105506782B CN201511018245.8A CN201511018245A CN105506782B CN 105506782 B CN105506782 B CN 105506782B CN 201511018245 A CN201511018245 A CN 201511018245A CN 105506782 B CN105506782 B CN 105506782B
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- 229920002748 Basalt fiber Polymers 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000009987 spinning Methods 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000004090 dissolution Methods 0.000 claims abstract description 6
- 239000000835 fiber Substances 0.000 claims description 44
- 235000002639 sodium chloride Nutrition 0.000 claims description 35
- 239000002131 composite material Substances 0.000 claims description 28
- 150000003839 salts Chemical class 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 24
- 239000011812 mixed powder Substances 0.000 claims description 20
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 9
- 239000011780 sodium chloride Substances 0.000 claims description 9
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000001103 potassium chloride Substances 0.000 claims description 6
- 235000011164 potassium chloride Nutrition 0.000 claims description 6
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 6
- 235000012241 calcium silicate Nutrition 0.000 claims description 4
- 239000010954 inorganic particle Substances 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 4
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 4
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 4
- 235000011151 potassium sulphates Nutrition 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- TWHBEKGYWPPYQL-UHFFFAOYSA-N aluminium carbide Chemical compound [C-4].[C-4].[C-4].[Al+3].[Al+3].[Al+3].[Al+3] TWHBEKGYWPPYQL-UHFFFAOYSA-N 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 235000015424 sodium Nutrition 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- 239000004846 water-soluble epoxy resin Substances 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910003978 SiClx Inorganic materials 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 239000010936 titanium Substances 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 239000002994 raw material Substances 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 4
- 238000002844 melting Methods 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 description 12
- 238000005491 wire drawing Methods 0.000 description 11
- 229910000629 Rh alloy Inorganic materials 0.000 description 8
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 8
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 description 8
- 230000009514 concussion Effects 0.000 description 7
- 239000012153 distilled water Substances 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- 238000010298 pulverizing process Methods 0.000 description 7
- 238000002791 soaking Methods 0.000 description 7
- 238000010792 warming Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 230000002045 lasting effect Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002657 fibrous material Substances 0.000 description 3
- 239000005543 nano-size silicon particle Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000011435 rock Substances 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000012876 carrier material Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000002783 friction material Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Inorganic Fibers (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a kind of preparation method of porous basalt fiber, this method be it is a kind of by basalt ore by getting the raw materials ready, melting, mix, the method that spinning, cooling, dissolution process step prepare the basalt fibre with loose structure, overcome the defect for the porous basalt fiber that prior art can not be prepared, the preparation method has production cost low, simple production process, is adapted to the advantage of large-scale industrial production.
Description
Technical field
The present invention relates to basalt fiber material field, and in particular to a kind of preparation method of porous basalt fiber.
Background technology
Basalt fibre is a kind of emerging novel inorganic environment-friendly and green high performance fibre material, is following China's emphasis
One of four big high-performance fibers of development, it is aoxidized by silica, aluminum oxide, calcium oxide, iron oxide and titanium dioxide etc.
The basalt building stones of thing composition are prepared from after high-temperature fusion by spinning technique.Basalt continuous fiber is not only stablized
Property it is good, but also with a variety of excellent properties such as electrical insulating property, anticorrosive, flame resistant, high temperature resistant, moreover, basalt fibre
The discarded object that production technology is produced is few, and environmental pollution is small, directly can be transferred to after product abandonment in ecological environment, without any danger
Evil, thus be a kind of qualified green, environment-friendly materials.Basalt fibre fibre reinforced composites, friction material,
The many aspects such as shipbuilding materials, heat-barrier material, automobile industry, high temperature filtration fabric and protection field have obtained widely should
With.
Basalt fibre is non-crystalline material, and rigidity is big, internal stress is big, fusing point is high, is easily broken off in bending, stretching, institute
The basalt fibre for obtaining loose structure is difficult to the preparation method that porous fibre is prepared using traditional addition pore creating material, now
It is all solid fibre that the basalt fibre of preparation is most of, and fiber surface is smooth, and specific surface area is small, density is big, is unfavorable for the Black Warrior
Application of the rock fiber in light material, carrier material field.
China Patent Publication No. CN1884164 discloses the method for manufacturing basalt filament, and this method is first will be profound
Military rock rock is ground, then is washed, and is then melted, and fiber is finally stretched with the mode of collimation, and by fiber roll around so as to obtain
To basalt fibre.This method has fibre diameter controllable, and basalt fibre heat resistance is more preferable, the lower advantage of cost, but
Due to being direct melt drawing, do not use pore creating material etc. to be likely to form the raw material or process of loose structure yet, pass through
The basalt fibre that this method is obtained can not possibly have loose structure, thus can not prepare loose structure using this method
Basalt fibre.
China Patent Publication No. CN102786220A discloses a kind of production method of ultra-fine basalt continuous filament, the party
Method is to carry out wire drawing using tapered platinum bushing plate to obtain basalt fibre, and this method is equally solid hole wire drawing, is not also had
The raw material or process of loose structure are likely to form using pore creating material etc., the basalt fibre obtained by this method can not
There can be loose structure, so the basalt fibre of loose structure can not be prepared using this method.
The basalt fibre prepared using the above-mentioned method for preparing basalt fibre is solid fibre, fiber surface
Smooth, specific surface area is small, density is big, is unfavorable for application of the basalt fibre in light material, carrier material field, thus,
Invention is a kind of to prepare promotion and application of the method to basalt fibre of the basalt fiber material with loose structure
With important value.
The content of the invention
This hair can not all obtain the defect of the basalt fibre with loose structure to solve existing preparation method, propose
A kind of preparation method of porous basalt fiber.
This method be one kind by basalt ore by getting the raw materials ready, melting, mix, spinning, cooling, dissolution process step prepare
The method for obtaining the basalt fibre with loose structure, overcomes the porous basalt fiber that prior art can not be prepared
Defect, the preparation method has production cost low, simple production process, is adapted to the advantage of large-scale industrial production.
A kind of preparation method of porous basalt fiber of the present invention, its specific preparation process is as follows：
1）Basalt ore is immersed in pond, is rinsed, the impurity that surface may be adhered to is removed, then takes out and dry in the air
It is dry, the basalt ore dried and inorganic salts are subjected to pulverization process with pulverizer, are well mixed after crushing, fineness is 2.0-
4.0mm, obtains the mixed powder of basalt and inorganic salts；
2）By step 1) obtain mixed powder and be added in kiln, 1200-1500 DEG C is warming up to, mixed powder is melted completely
Melt, and continue stirring, form mixed molten liquid；
3）In step 2）Nano inorganic toughening material is added in obtained liquation, it is well mixed with liquation, spun
Silk liquation；
4）By step 3) obtained spinning liquation carries out wire drawing with platinum-rhodium alloy bushing with holes, obtains containing nanometer
The basalt composite fibre of inorganic toughening material and inorganic salts；
5）By step 4) obtained composite fibre is directly immersed in size, quickly cooled down, taken out standby；
6）By step 5）The composite fibre of cooling is immersed in distilled water, while carrying out concussion processing 30- with ultrasonic wave
60min, taking-up, which is dried, after soaking 5-8 times repeatedly obtains porous basalt fiber.
In a kind of preparation method of above-mentioned porous basalt fiber, step 1) selection inorganic salts have it is soluble in water, it is high
Do not chemically reacted under fusing point higher boiling, with basalt hot conditions, the characteristics of being not easily decomposed；Described inorganic salts are sulfuric acid
One or more in sodium, potassium sulfate, potassium chloride, sodium chloride.
In a kind of preparation method of above-mentioned porous basalt fiber, step 1) in basalt ore and inorganic salts mixing
Mass ratio is 1: 0.5-4；Very few inorganic salts can not form crystal grain, it is impossible to obtain hole, the crystal grain that excessive inorganic salts are formed
Quantity is too many too big, destroys the structure of fiber, easy fracture, it is impossible to which stretching obtains fiber.
In a kind of preparation method of above-mentioned porous basalt fiber, step 3）The use of described nano inorganic toughening material
Measure as the 2%-10% of liquation gross mass；Nano inorganic toughening material is one kind or many of nano inorganic particle and nano inorganic whisker
Kind；Nano inorganic particle is diameter≤50nm silica, carborundum, silicon nitride aluminum nanoparticles；Nano inorganic whisker
For length≤100nm, the titanium nitride of draw ratio >=5, aluminium carbide, calcium silicates nano whisker.
In a kind of preparation method of above-mentioned porous basalt fiber, step 4) in the bore dia of platinum-rhodium alloy bushing be
10-100μm。
In a kind of preparation method of above-mentioned porous basalt fiber, step 5) described in size be aqueous polyurethane infiltration
One kind in agent, water-soluble epoxy resin size, infiltration temperature is 0-50 DEG C.
The addition of nano inorganic toughening material, can improve the toughness of basalt fibre：In stretching, nano inorganic toughness reinforcing material
Material forms ordered structure in the presence of stress, reduces the rigidity of basalt fibre；Nano particle or whisker can disperse basalt
The Impact direction of fibrous inside stress, improves stress and bears the upper limit.Nano inorganic toughening material can also make inorganic as nucleator
Salt crystallizes to form crystal grain, and controls by controlling the temperature of size the speed of cooling, so that the growth time of crystal grain is controlled,
The crystal grain of different-diameter is obtained, is smooth wire drawing, the formation of hole of basalt fibre, the control of hole size, which is provided, to be protected
Card.
In a kind of preparation method of above-mentioned porous basalt fiber, step 6）Described distillation coolant-temperature gage is 40-100 DEG C；
Inorganic salts solubility in the hot water and rate of dissolution are bigger, dissolving inorganic salts crystal grain that can be faster and better, form hole.
In a kind of preparation method of above-mentioned porous basalt fiber, step 6) ultrasonic oscillation is used, mixing can be made fine
Inorganic salts crystal grain in dimension loosens, and forms gap and is contacted with water, so as to quickly dissolve, and will not destroy the complete of basalt fibre
Whole property, so that loose structure is formed, effect good the characteristics of fast with speed；In described ultrasonic oscillation, power be 600-
800W, frequency is 40-80KHz.
In a kind of preparation method of above-mentioned porous basalt fiber, step 6) described in porous basalt fibre diameter be
0.5-50 μm, porosity 10%-80%.
A kind of preparation method of porous basalt fiber of the present invention, by basalt ore by getting the raw materials ready, melting, mix, spin
Silk, cooling, dissolution process step have obtained the basalt fibre with loose structure.First basalt ore and inorganic salts are carried out
Hybrid Heating is melted, and is added nano inorganic toughening material and is carried out toughness reinforcing to mixed molten liquid, is obtained by spinning containing inorganic salts
The composite fibre of crystal grain, is finally dissolved in distillation by the inorganic salts crystal grain in composite fibre under the subsidiary conditions of ultrasonic oscillation
Hole is formed in water, so as to form porous basalt fibre.Instant invention overcomes prior art can not prepare it is many
The defect of hole basalt fibre, has prepared a kind of basalt fiber material with loose structure, and the inventive method has
Production cost is low, simple production process, is adapted to the advantage of large-scale industrial production, with wide market application foreground.
A kind of preparation method of porous basalt fiber of the present invention, its outstanding feature and beneficial effect are：
1st, the present invention by basalt ore by getting the raw materials ready, melting, mix, spinning, cooling, dissolution process step prepare
There is the basalt fibre of loose structure.
2nd, the present invention carries out toughness reinforcing using nano inorganic toughening material to basalt fibre, has prepared porous basalt
Fiber.
3rd, the characteristics of inorganic salts that the present invention is used have recyclable reuse, i.e., it is economical and environmentally friendly.
4th, production cost of the present invention is low, simple production process, is adapted to large-scale industrial production.
The porous basalt fiber that the present invention is prepared is through examining, and performance is as follows：
| Performance | Structure | Density（g/cm） | Porosity（%） | Diameter（μm） |
| As a result | Porous fibrous structure | 0.6-2.5 | 10-80 | 0.5-50 |
Brief description of the drawings：
Fig. 1 is the process chart of the preparation method of porous basalt fiber of the present invention.
Embodiment
With reference to test example and embodiment, the present invention is described in further detail.But this should not be understood
Following embodiment is only limitted to for the scope of above-mentioned theme of the invention, it is all that this is belonged to based on the technology that present invention is realized
The scope of invention.
Embodiment 1
1）Basalt ore is immersed in pond, is rinsed, the impurity that surface may be adhered to is removed, then takes out and dry in the air
It is dry, the basalt ore dried and sodium sulphate are subjected to pulverization process with pulverizer, wherein basalt ore and sodium sulphate is mixed
The mass ratio of conjunction is 1: 0.5, is well mixed after crushing, fineness is 2.0mm, obtains the mixed powder of basalt and sodium sulphate；
2）By step 1) obtain mixed powder and be added in kiln, 1200 DEG C are warming up to, mixed powder is melted completely, and
Lasting stirring, forms mixed molten liquid；
3）In step 2）In obtained liquation add liquation gross mass 2% particle diameter be 10nm silicon-carbide particle, by its with
Liquation is well mixed, and obtains spinning liquation；
4）By step 3) obtained spinning liquation carries out wire drawing with bore dia for 10 μm of platinum-rhodium alloy bushing, obtains
Basalt composite fibre containing nano silicon carbide granulate and sodium sulphate crystal grain；
5）By step 4) obtained composite fibre is directly immersed in temperature in 0 DEG C of size, quickly to be cooled down, taking-up
It is standby；
6）By step 5）The composite fibre of cooling is immersed in temperature in 40 DEG C of distilled water, while be 600W with power, frequency
The ultrasonic wave that rate is 40KHz carries out concussion processing 30min, and taking-up, which is dried, after soaking 5 times repeatedly obtains porous basalt fiber.
The porous basalt fiber that the present embodiment is prepared is through examining, and performance is as follows：
| Performance | Structure | Density（g/cm） | Porosity（%） | Diameter（μm） |
| As a result | Porous fibrous structure | 2.0 | 33 | 0.5 |
Embodiment 2
1）Basalt ore is immersed in pond, is rinsed, the impurity that surface may be adhered to is removed, then takes out and dry in the air
It is dry, the basalt ore dried and potassium sulfate are subjected to pulverization process with pulverizer, wherein basalt ore and inorganic salts is mixed
The mass ratio of conjunction is 1: 4, is well mixed after crushing, fineness is 2.0mm, obtains the mixed powder of basalt and inorganic salts；
2）By step 1) obtain mixed powder and be added in kiln, 1500 DEG C are warming up to, mixed powder is melted completely, and
Lasting stirring, forms mixed molten liquid；
3）In step 2）10% draw ratio that liquation gross mass is added in obtained liquation is 5, and length is 100nm nanometer
Titanium nitride whisker, it is well mixed with liquation, obtains spinning liquation；
4）By step 3) obtained spinning liquation carries out wire drawing with bore dia for 100 μm of platinum-rhodium alloy bushing, obtains
To the basalt composite fibre containing Nano titanium nitride whisker and potassium sulfate crystal grain；
5）By step 4) obtained composite fibre is directly immersed in temperature in 50 DEG C of sizes, quickly to be cooled down, taken
Go out standby；
6）By step 5）The composite fibre of cooling is immersed in temperature in 100 DEG C of distilled water, while be 800W with power, frequency
The ultrasonic wave that rate is 80KHz carries out concussion processing 60min, and taking-up, which is dried, after soaking 8 times repeatedly obtains porous basalt fiber.
The porous basalt fiber that the present embodiment is prepared is through examining, and performance is as follows：
| Performance | Structure | Density（g/cm） | Porosity（%） | Diameter（μm） |
| As a result | Porous fibrous structure | 0.6 | 80 | 50 |
Embodiment 3
1）Basalt ore is immersed in pond, is rinsed, the impurity that surface may be adhered to is removed, then takes out and dry in the air
It is dry, the basalt ore dried and potassium chloride are subjected to pulverization process with pulverizer, wherein basalt ore and inorganic salts is mixed
The mass ratio of conjunction is 1: 1, is well mixed after crushing, fineness is 4.0mm, obtains the mixed powder of basalt and potassium chloride；
2）By step 1) obtain mixed powder and be added in kiln, 1300 DEG C are warming up to, mixed powder is melted completely, and
Lasting stirring, forms mixed molten liquid；
3）In step 2）In obtained liquation add liquation gross mass 5% particle diameter be 30nm silicon nitride particle, by its with
Liquation is well mixed, and obtains spinning liquation；
4）By step 3) obtained spinning liquation carries out wire drawing with bore dia for 50 μm of platinum-rhodium alloy bushing, obtains
Basalt composite fibre containing nano silicon nitride silicon grain and potassium chloride crystal grain；
5）By step 4) obtained composite fibre is directly immersed in temperature in 30 DEG C of sizes, quickly to be cooled down, taken
Go out standby；
6）By step 5）The composite fibre of cooling is immersed in temperature in 60 DEG C of distilled water, while be 700W with power, frequency
The ultrasonic wave that rate is 50KHz carries out concussion processing 50min, and taking-up, which is dried, after soaking 6 times repeatedly obtains porous basalt fiber.
The porous basalt fiber that the present embodiment is prepared is through examining, and performance is as follows：
| Performance | Structure | Density（g/cm） | Porosity（%） | Diameter（μm） |
| As a result | Porous fibrous structure | 1.5 | 50 | 20 |
Comparative example
1）Basalt ore is immersed in pond, is rinsed, the impurity that surface may be adhered to is removed, then takes out and dry in the air
It is dry, the basalt ore dried is subjected to pulverization process with pulverizer, fineness is 4.0mm, obtains basalt ore powder；
2）By step 1) obtain powder and be added in kiln, 1300 DEG C are warming up to, powder is melted completely, and is persistently stirred
Mix, form liquation；
3）In step 2）In obtained liquation add liquation gross mass 5% particle diameter be 30nm silicon nitride particle, by its with
Liquation is well mixed, and obtains spinning liquation；
4）By step 3) obtained spinning liquation carries out wire drawing with bore dia for 50 μm of platinum-rhodium alloy bushing, obtains
Basalt composite fibre containing nano silicon nitride silicon grain；
5）By step 4) obtained composite fibre is directly immersed in temperature in 30 DEG C of sizes, quickly to be cooled down, taken
Go out standby；
6）By step 5）The composite fibre of cooling is immersed in temperature in 60 DEG C of distilled water, while be 700W with power, frequency
The ultrasonic wave that rate is 50KHz carries out concussion processing 50min, and taking-up, which is dried, after soaking 6 times repeatedly obtains basalt fibre.
The basalt fibre that the present embodiment is prepared is through examining, and performance is as follows：
| Performance | Structure | Density（g/cm） | Porosity（%） | Diameter（μm） |
| As a result | Solid fibre | 2.9 | 0 | 20 |
Due to no addition potassium chloride in above-mentioned comparative example, in step 6）In there is no the material that can be dissolved, also just not
Hole can be formed, porous basalt fibre can not be obtained.
Embodiment 4
1）Basalt ore is immersed in pond, is rinsed, the impurity that surface may be adhered to is removed, then takes out and dry in the air
It is dry, the basalt ore dried and sodium chloride are subjected to pulverization process with pulverizer, wherein basalt ore and inorganic salts is mixed
The mass ratio of conjunction is 1: 3, is well mixed after crushing, fineness is 3.0mm, obtains the mixed powder of basalt and sodium chloride；
2）By step 1) obtain mixed powder and be added in kiln, 1400 DEG C are warming up to, mixed powder is melted completely, and
Lasting stirring, forms mixed molten liquid；
3）In step 2）6% draw ratio that liquation gross mass is added in obtained liquation is 10, and length is 60nm calcium silicates
Whisker, it is well mixed with liquation, obtains spinning liquation；
4）By step 3) obtained spinning liquation carries out wire drawing with bore dia for 60 μm of platinum-rhodium alloy bushing, obtains
Basalt composite fibre containing nanometer calcium silicate whisker and sodium chloride；
5）By step 4) obtained composite fibre is directly immersed in temperature in 40 DEG C of sizes, quickly to be cooled down, taken
Go out standby；
6）By step 5）The composite fibre of cooling is immersed in temperature in 60 DEG C of distilled water, while be 600W with power, frequency
The ultrasonic wave that rate is 80KHz carries out concussion processing 40min, and taking-up, which is dried, after soaking 7 times repeatedly obtains porous basalt fiber.
The porous basalt fiber that the present embodiment is prepared is through examining, and performance is as follows：
| Performance | Structure | Density（g/cm） | Porosity（%） | Diameter（μm） |
| As a result | Porous fibrous structure | 0.75 | 75 | 12 |
Comparative example
1）Basalt ore is immersed in pond, is rinsed, the impurity that surface may be adhered to is removed, then takes out and dry in the air
It is dry, the basalt ore dried and sodium chloride are subjected to pulverization process with pulverizer, wherein basalt ore and inorganic salts is mixed
The mass ratio of conjunction is 1: 3, is well mixed after crushing, fineness is 3.0mm, obtains the mixed powder of basalt and sodium chloride；
2）By step 1) obtain mixed powder and be added in kiln, 1400 DEG C are warming up to, mixed powder is melted completely, and
Lasting stirring, forms mixed molten liquid；
3）By step 2) obtained mixed molten liquid carries out wire drawing with bore dia for 60 μm of platinum-rhodium alloy bushing, obtains
Basalt composite fibre containing sodium chloride；
4）By step 3) obtained composite fibre is directly immersed in temperature in 40 DEG C of sizes, quickly to be cooled down, taken
Go out standby；
5）By step 4）The composite fibre of cooling is immersed in temperature in 60 DEG C of distilled water, while be 600W with power, frequency
The ultrasonic wave that rate is 80KHz carries out concussion processing 40min, and taking-up, which is dried, after soaking 7 times repeatedly obtains not of uniform size porous
Grain.
Due to not adding nano inorganic toughening material, lacking toughness, in step 3 in above-mentioned comparative example）It is middle to be drawn
It is easily broken off during silk, wire drawing is extremely difficult, and what is obtained is composite fibre different in size, through step 4）、5）Processing, sodium chloride
It is dissolved, but due to lacking toughness and support, hole collapses, and fibre structure is destroyed, it is impossible to form porous fibre structure,
It cannot get porous basalt fiber, it follows that the addition of nano inorganic toughening material is to ensure that porous basalt fiber is formed
Necessary condition.
Claims (10)
1. a kind of preparation method of porous basalt fiber, it is characterised in that preparation process is as follows：
1）Basalt ore is crushed with inorganic salts with pulverizer, and is well mixed, the mixed of basalt and inorganic salts is obtained
Close powder；
2）By step 1) obtain mixed powder and be added in kiln, heat up, melt mixed powder, form mixed molten liquid；
3）In step 2）Toughening material is added in obtained liquation, spinning liquation is obtained；
4）By step 3) obtained spinning liquation carries out spinning, obtains basalt composite fibre；
5）By step 4) obtained composite fibre is immersed in size, cooled down；
6）By step 5）The composite fibre of cooling is immersed in water, is carried out dissolution process, is dried and obtain porous basalt fiber.
2. the preparation method of porous basalt fiber according to claim 1, it is characterised in that step 1) in basalt ore deposit
The mass ratio of the mixing of stone and inorganic salts is 1: 0.5-4.
3. the preparation method of porous basalt fiber according to claim 1, it is characterised in that described inorganic salts are sulphur
One or more in sour sodium, potassium sulfate, potassium chloride, sodium chloride.
4. the preparation method of porous basalt fiber according to claim 1, it is characterised in that described toughening material
Usage amount is basalt and the 2%-10% of inorganic salts gross mass.
5. the preparation method of porous basalt fiber according to claim 1, it is characterised in that described toughening material is
The one or more of nano inorganic particle and nano inorganic whisker；Nano inorganic particle is diameter≤50nm silica, carbon
One or more in SiClx, silicon nitride aluminum nanoparticles；Nano inorganic whisker is length≤100nm, the nitrogen of draw ratio >=5
Change the one or more in titanium, aluminium carbide, the nano whisker of calcium silicates.
6. the preparation method of porous basalt fiber according to claim 1, it is characterised in that described size is water
One kind in property polyurethane size, water-soluble epoxy resin size.
7. the preparation method of porous basalt fiber according to claim 6, it is characterised in that the size temperature is
0-50℃。
8. the preparation method of porous basalt fiber according to claim 1, it is characterised in that described coolant-temperature gage is 40-
100℃。
9. the preparation method of porous basalt fiber according to claim 1, it is characterised in that added using ultrasonic oscillation
Instant solution, ultrasonic power is 600-800W, and frequency is 40-80KHz.
10. the preparation method of porous basalt fiber according to claim 1, it is characterised in that described porous basalt
Fibre diameter is 0.5-50 μm, porosity 10%-80%.
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| CN106752687B (en) * | 2016-11-29 | 2019-05-24 | 江苏亨通光电股份有限公司 | Basalt fibre reinforcing strip and preparation method |
| CN106521709B (en) * | 2016-11-29 | 2018-11-09 | 深圳市高科塑化有限公司 | Special basalt fibre of a kind of polyphenyl thioether material enhancing and preparation method thereof |
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| CN107808718A (en) * | 2017-09-30 | 2018-03-16 | 四川力智久创知识产权运营有限公司 | A kind of oil-impregnated paper insulation cable |
| CN107833670A (en) * | 2017-09-30 | 2018-03-23 | 四川力智久创知识产权运营有限公司 | A kind of high mechanical properties insulated cable |
| CN109020184A (en) * | 2018-07-10 | 2018-12-18 | 四川千然科技有限公司 | A kind of production method and equipment of porous basalt cellucotton |
| TWI680790B (en) * | 2018-11-14 | 2020-01-01 | 陳宣甫 | Method of manufacturing water filter material |
| CN109487371A (en) * | 2018-12-19 | 2019-03-19 | 长春安旨科技有限公司 | A kind of high-strength and high ductility fiber and preparation method thereof |
| CN113318700A (en) * | 2021-05-26 | 2021-08-31 | 盛和深 | Porous cellucotton and preparation method and application thereof |
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