CN105506782A - Preparation method of porous basalt fibers - Google Patents
Preparation method of porous basalt fibers Download PDFInfo
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- CN105506782A CN105506782A CN201511018245.8A CN201511018245A CN105506782A CN 105506782 A CN105506782 A CN 105506782A CN 201511018245 A CN201511018245 A CN 201511018245A CN 105506782 A CN105506782 A CN 105506782A
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- 229920002748 Basalt fiber Polymers 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000009987 spinning Methods 0.000 claims abstract description 21
- 238000002844 melting Methods 0.000 claims abstract description 13
- 230000008018 melting Effects 0.000 claims abstract description 13
- 239000000835 fiber Substances 0.000 claims description 44
- 235000002639 sodium chloride Nutrition 0.000 claims description 35
- 150000003839 salts Chemical class 0.000 claims description 26
- 239000011812 mixed powder Substances 0.000 claims description 21
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 238000004513 sizing Methods 0.000 claims description 16
- 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
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 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
- 238000004090 dissolution Methods 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
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 6
- 235000011152 sodium sulphate Nutrition 0.000 claims description 6
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 4
- 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
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 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
- 239000004846 water-soluble epoxy resin Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000001816 cooling Methods 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 4
- 238000010298 pulverizing process Methods 0.000 description 13
- 239000013078 crystal Substances 0.000 description 12
- 238000005491 wire drawing Methods 0.000 description 12
- 239000012153 distilled water Substances 0.000 description 9
- 229910000629 Rh alloy Inorganic materials 0.000 description 8
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 description 8
- 238000013019 agitation Methods 0.000 description 7
- 230000009514 concussion Effects 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 238000010792 warming Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 238000007654 immersion Methods 0.000 description 6
- 238000007689 inspection Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 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
- 239000000843 powder Substances 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
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000000378 calcium silicate Substances 0.000 description 2
- 229910052918 calcium silicate Inorganic materials 0.000 description 2
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 2
- 239000012876 carrier material Substances 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
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000002344 fibroplastic effect Effects 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
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000002791 soaking Methods 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)
- Inorganic Fibers (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a preparation method of porous basalt fibers. Porous basalt ores are subjected to process steps of material preparation, melting, mixing, spinning, cooling and dissolving to obtain porous basalt fibers. The method is capable of overcoming the defect that the porous basalt fibers cannot be prepared in the prior art. And the preparation method has the advantages of low production cost and simple production process and is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to basalt fiber material field, be specifically related 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, one of four large high-performance fibers of giving priority to of following China, the basalt building stones that it is made up of oxides such as silica, aluminium oxide, calcium oxide, iron oxide and titanium dioxide, after high-temperature fusion, are prepared from by spinning technique.Basalt continuous fiber is good stability not only, but also there is electrical insulating property, anticorrosive, flame resistant, the multiple excellent properties such as high temperature resistant, and, the discarded object that the production technology of basalt fibre produces is few, environmental pollution is little, can directly proceed in ecological environment after product abandonment, without any harm, because of but a kind of genuine green, environment-friendly materials.Basalt fibre is widely used in many aspects such as fibre reinforced composites, friction material, shipbuilding materials, heat-barrier material, automobile industry, high temperature filtration fabric and protection fields.
Basalt fibre is non-crystalline material, rigidity is large, internal stress is large, fusing point is high, easily rupture when bending, stretching, so the preparation method adopting traditional interpolation pore creating material to prepare porous fibre is difficult to obtain the basalt fibre of loose structure, the basalt fibre major part prepared now is all solid fibers, and fiber surface is smooth, and specific area is little, density is large, be unfavorable for that basalt fibre is at light material, the application in carrier material field.
China Patent Publication No. CN1884164 discloses the method for the manufacture of basalt filament, and the method is first ground by basalt rock, then washs, and then melts, finally with collimation mode drawing of fiber, and by fiber roll around thus obtain basalt fibre.It is controlled that the method has fibre diameter, basalt fibre heat resistance is better, the advantage that cost is lower, but owing to being direct melt drawing, pore creating material etc. is not used may to form raw material or the process of loose structure yet, the basalt fibre obtained by the method can not have loose structure, and the method thus can not be adopted to prepare the basalt fibre of loose structure.
China Patent Publication No. CN102786220A discloses a kind of production method of ultra-fine basalt continuous filament, the method adopts tapered platinum bushing plate to carry out wire drawing to obtain basalt fibre, the method is the wire drawing of solid hole equally, pore creating material etc. is not used may to form raw material or the process of loose structure yet, the basalt fibre obtained by the method can not have loose structure, so the method can not be adopted to prepare the basalt fibre of loose structure.
The basalt fibre adopting the above-mentioned method preparing basalt fibre to prepare is solid fibers, fiber surface is smooth, specific area is little, density is large, be unfavorable for that basalt fibre is at light material, application in carrier material field, thus, invent a kind of promotion and application of method to basalt fibre that can prepare the basalt fiber material with loose structure and there is important value.
Summary of the invention
This defect that all can not obtain the basalt fibre with loose structure in order to solve existing preparation method, proposes a kind of preparation method of porous basalt fiber.
The method be a kind of by basalt ore by getting the raw materials ready, melting, mixing, spinning, cooling, dissolution process step prepare the method for the basalt fibre with loose structure, overcome the defect of the porous basalt fiber that prior art can not prepare, it is low that this preparation method has production cost, production technology is simple, is applicable to the advantage of large-scale industrial production.
The preparation method of a kind of porous basalt fiber of the present invention, its concrete preparation process is as follows:
1) basalt ore is immersed in pond, rinse, the impurity that removing surface may be adhered to, then take out and dry, the basalt ore dried and inorganic salts pulverizer are carried out pulverization process, mixes after pulverizing, fineness is 2.0-4.0mm, obtains the mixed powder of basalt and inorganic salts;
2) by step 1) obtain mixed powder and join in kiln, be warming up to 1200-1500 DEG C, make the complete melting of mixed powder, and Keep agitation, form mixed molten liquid;
3) in step 2) add nano inorganic toughening material in the liquation that obtains, it is mixed with liquation, obtains spinning liquation;
4) by step 3) the spinning liquation that obtains carries out wire drawing with platinum-rhodium alloy bushing with holes, obtains the basalt blended fiber containing nano inorganic toughening material and inorganic salts;
5) by step 4) blended fiber that obtains directly is immersed in sizing agent, cools fast, take out for subsequent use;
6) be immersed in distilled water by the blended fiber that step 5) cools, carry out concussion process 30-60min with ultrasonic wave, after repeatedly soaking 5-8 time, taking-up is dried and is obtained porous basalt fiber simultaneously.
In the preparation method of above-mentioned a kind of porous basalt fiber, step 1) inorganic salts selected have soluble in water, and, there is not chemical reaction with under basalt hot conditions in high-melting-point higher boiling, not labile feature; Described inorganic salts are one or more in sodium sulphate, potassium sulfate, potassium chloride, sodium chloride.
In the preparation method of above-mentioned a kind of porous basalt fiber, step 1) in basalt ore be 1: 0.5-4 with the mass ratio mixed of inorganic salts; Very few inorganic salts can not form crystal grain, cannot obtain hole, and the crystal grain quantity that too much inorganic salts are formed is too many too large, and destroy the structure of fiber, easy fracture, cannot stretch and obtain fiber.
In the preparation method of above-mentioned a kind of porous basalt fiber, the use amount of the nano inorganic toughening material described in step 3) is the 2%-10% of liquation gross mass; Nano inorganic toughening material is one or more of nano inorganic particle and nano inorganic whisker; Nano inorganic particle is silica, carborundum, the silicon nitride aluminum nanoparticles of diameter≤50nm; Nano inorganic whisker is the nano whisker of length≤100nm, the titanium nitride of draw ratio >=5, aluminium carbide, calcium silicates.
In the preparation method of above-mentioned a kind of porous basalt fiber, step 4) in the bore dia of platinum-rhodium alloy bushing be 10-100 μm.
In the preparation method of above-mentioned a kind of porous basalt fiber, step 5) described in sizing agent be one in aqueous polyurethane sizing agent, water-soluble epoxy resin sizing agent, infiltration temperature is 0-50 DEG C.
Adding of nano inorganic toughening material, the toughness of basalt fibre being improved: when stretching, nano inorganic toughening material is formed with sequence structure under the effect of stress, reducing the rigidity of basalt fibre; Nano particle or whisker can disperse the Impact direction of basalt fibre internal stress, improve stress and bear the upper limit.Nano inorganic toughening material can also as nucleator, inorganic salts crystallization is made to form crystal grain, and the speed of controlled cooling model is carried out by the temperature controlling sizing agent, thus control the growth time of crystal grain, obtain the crystal grain of different-diameter, for the smooth wire drawing of basalt fibre, the formation of hole, the control of hole size provides guarantee.
In the preparation method of above-mentioned a kind of porous basalt fiber, the distilled water temperature described in step 6) is 40-100 DEG C; Inorganic salts solubility in the hot water and rate of dissolution are larger, and dissolve inorganic salts crystal grain that can be faster and better forms hole.
In the preparation method of above-mentioned a kind of porous basalt fiber, step 6) adopt ultrasonic oscillation, the inorganic salts crystal grain in blended fiber can be made to loosen, form gap and contact with water, thus rapid solution, and the integrality of basalt fibre can not be destroyed, thus form loose structure, there is speed fast, effective feature; In described ultrasonic oscillation, power is 600-800W, and frequency is 40-80KHz.
In the preparation method of above-mentioned a kind of porous basalt fiber, step 6) described in porous basalt fibre diameter be 0.5-50 μm, porosity 10%-80%.
The preparation method of a kind of porous basalt fiber of the present invention, by basalt ore by getting the raw materials ready, melting, mixing, spinning, cooling, dissolution process step obtain the basalt fibre with loose structure.First basalt ore and inorganic salts are carried out Hybrid Heating melting, adding nano inorganic toughening material again carries out toughness reinforcing to mixed molten liquid, the blended fiber containing inorganic salts crystal grain is obtained by spinning, finally the inorganic salts crystal grain in blended fiber is dissolved in distilled water under the subsidiary conditions of ultrasonic oscillation and forms hole, thus form the basalt fibre of porous.Instant invention overcomes the defect of the porous basalt fiber that prior art can not prepare, prepare a kind of basalt fiber material with loose structure, it is low that the inventive method has production cost, production technology is simple, be applicable to the advantage of large-scale industrial production, there is wide market application foreground.
The preparation method of a kind of porous basalt fiber of the present invention, its outstanding feature and beneficial effect are:
1, the present invention by basalt ore by getting the raw materials ready, melting, mixing, spinning, cooling, dissolution process step prepared the basalt fibre with loose structure.
2, the present invention uses nano inorganic toughening material to carry out toughness reinforcing to basalt fibre, has prepared porous basalt fiber.
3, the inorganic salts that the present invention uses have recyclable reusable feature, namely economical, environmental protection again.
4, production cost of the present invention is low, and production technology is simple, is applicable to large-scale industrial production.
The porous basalt fiber that the present invention prepares is through inspection, and performance is as follows:
| Performance | Structure | Density (g/cm) | Porosity (%) | Diameter (μm) |
| Result | Porous fibrous structure | 0.6-2.5 | 10-80 | 0.5-50 |
Accompanying drawing illustrates:
Fig. 1 is the process chart of the preparation method of porous basalt fiber of the present invention.
Detailed description of the invention
Below in conjunction with test example and detailed description of the invention, the present invention is described in further detail.But this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment, all technology realized based on content of the present invention all belong to scope of the present invention.
embodiment 1
1) basalt ore is immersed in pond, rinse, the impurity that removing surface may be adhered to, then take out and dry, the basalt ore dried and sodium sulphate pulverizer are carried out pulverization process, and wherein basalt ore is 1: 0.5 with the mass ratio mixed of sodium sulphate, mixes after pulverizing, fineness is 2.0mm, obtains the mixed powder of basalt and sodium sulphate;
2) by step 1) obtain mixed powder and join in kiln, be warming up to 1200 DEG C, make the complete melting of mixed powder, and Keep agitation, form mixed molten liquid;
3) in step 2) 2% particle diameter that adds liquation gross mass in the liquation that obtains is the silicon-carbide particle of 10nm, it mixed with liquation, obtains spinning liquation;
4) by step 3) the spinning liquation bore dia that obtains is that the platinum-rhodium alloy bushing of 10 μm carries out wire drawing, obtains the basalt blended fiber containing nano silicon carbide granulate and sodium sulphate crystal grain;
5) by step 4) to be directly immersed in temperature be in 0 DEG C of sizing agent for the blended fiber that obtains, cool fast, take out for subsequent use;
6) to be immersed in temperature be in 40 DEG C of distilled water to blended fiber step 5) cooled, and be 600W with power, frequency is that the ultrasonic wave of 40KHz carries out concussion process 30min simultaneously, repeatedly immersion 5 times afterwards taking-up dry and obtain porous basalt fiber.
The porous basalt fiber that the present embodiment prepares is through inspection, and performance is as follows:
| Performance | Structure | Density (g/cm) | Porosity (%) | Diameter (μm) |
| Result | Porous fibrous structure | 2.0 | 33 | 0.5 |
embodiment 2
1) basalt ore is immersed in pond, rinse, the impurity that removing surface may be adhered to, then take out and dry, the basalt ore dried and potassium sulfate pulverizer are carried out pulverization process, and wherein basalt ore is 1: 4 with the mass ratio mixed of inorganic salts, mixes after pulverizing, fineness is 2.0mm, obtains the mixed powder of basalt and inorganic salts;
2) by step 1) obtain mixed powder and join in kiln, be warming up to 1500 DEG C, make the complete melting of mixed powder, and Keep agitation, form mixed molten liquid;
3) in step 2) 10% draw ratio that adds liquation gross mass in the liquation that obtains is 5, length is the Nano titanium nitride whisker of 100nm, it is mixed with liquation, obtains spinning liquation;
4) by step 3) the spinning liquation bore dia that obtains is that the platinum-rhodium alloy bushing of 100 μm carries out wire drawing, obtains the basalt blended fiber containing Nano titanium nitride whisker and potassium sulfate crystal grain;
5) by step 4) to be directly immersed in temperature be in 50 DEG C of sizing agents for the blended fiber that obtains, cool fast, take out for subsequent use;
6) to be immersed in temperature be in 100 DEG C of distilled water to blended fiber step 5) cooled, and be 800W with power, frequency is that the ultrasonic wave of 80KHz carries out concussion process 60min simultaneously, repeatedly immersion 8 times afterwards taking-up dry and obtain porous basalt fiber.
The porous basalt fiber that the present embodiment prepares is through inspection, and performance is as follows:
| Performance | Structure | Density (g/cm) | Porosity (%) | Diameter (μm) |
| Result | Porous fibrous structure | 0.6 | 80 | 50 |
embodiment 3
1) basalt ore is immersed in pond, rinse, the impurity that removing surface may be adhered to, then take out and dry, the basalt ore dried and potassium chloride pulverizer are carried out pulverization process, and wherein basalt ore is 1: 1 with the mass ratio mixed of inorganic salts, mixes after pulverizing, fineness is 4.0mm, obtains the mixed powder of basalt and potassium chloride;
2) by step 1) obtain mixed powder and join in kiln, be warming up to 1300 DEG C, make the complete melting of mixed powder, and Keep agitation, form mixed molten liquid;
3) in step 2) 5% particle diameter that adds liquation gross mass in the liquation that obtains is the silicon nitride particle of 30nm, it mixed with liquation, obtains spinning liquation;
4) by step 3) the spinning liquation bore dia that obtains is that the platinum-rhodium alloy bushing of 50 μm carries out wire drawing, obtains the basalt blended fiber containing nano silicon nitride silicon grain and potassium chloride crystal grain;
5) by step 4) to be directly immersed in temperature be in 30 DEG C of sizing agents for the blended fiber that obtains, cool fast, take out for subsequent use;
6) to be immersed in temperature be in 60 DEG C of distilled water to blended fiber step 5) cooled, and be 700W with power, frequency is that the ultrasonic wave of 50KHz carries out concussion process 50min simultaneously, repeatedly immersion 6 times afterwards taking-up dry and obtain porous basalt fiber.
The porous basalt fiber that the present embodiment prepares is through inspection, and performance is as follows:
| Performance | Structure | Density (g/cm) | Porosity (%) | Diameter (μm) |
| Result | Porous fibrous structure | 1.5 | 50 | 20 |
Comparative example
1) immerse in pond by basalt ore, rinse, the impurity that removing surface may be adhered to, then take out and dry, the basalt ore pulverizer dried is carried out pulverization process, and fineness is 4.0mm, obtains basalt ore powder;
2) by step 1) obtain powder and join in kiln, be warming up to 1300 DEG C, make the complete melting of powder, and Keep agitation, form liquation;
3) in step 2) 5% particle diameter that adds liquation gross mass in the liquation that obtains is the silicon nitride particle of 30nm, it mixed with liquation, obtains spinning liquation;
4) by step 3) the spinning liquation bore dia that obtains is that the platinum-rhodium alloy bushing of 50 μm carries out wire drawing, obtains the basalt blended fiber containing nano silicon nitride silicon grain;
5) by step 4) to be directly immersed in temperature be in 30 DEG C of sizing agents for the blended fiber that obtains, cool fast, take out for subsequent use;
6) to be immersed in temperature be in 60 DEG C of distilled water to blended fiber step 5) cooled, and be 700W with power, frequency is that the ultrasonic wave of 50KHz carries out concussion process 50min simultaneously, repeatedly immersion 6 times afterwards taking-up dry and obtain basalt fibre.
The basalt fibre that the present embodiment prepares is through inspection, and performance is as follows:
| Performance | Structure | Density (g/cm) | Porosity (%) | Diameter (μm) |
| Result | Solid fibers | 2.9 | 0 | 20 |
Owing to not adding potassium chloride in above-mentioned comparative example, in step 6), there is no the material that can dissolve, just can not form hole yet, the basalt fibre of porous can not be obtained.
embodiment 4
1) basalt ore is immersed in pond, rinse, the impurity that removing surface may be adhered to, then take out and dry, the basalt ore dried and sodium chloride pulverizer are carried out pulverization process, and wherein basalt ore is 1: 3 with the mass ratio mixed of inorganic salts, mixes after pulverizing, fineness is 3.0mm, obtains the mixed powder of basalt and sodium chloride;
2) by step 1) obtain mixed powder and join in kiln, be warming up to 1400 DEG C, make the complete melting of mixed powder, and Keep agitation, form mixed molten liquid;
3) in step 2) 6% draw ratio that adds liquation gross mass in the liquation that obtains is 10, length is the calcium silicate whisker of 60nm, it is mixed with liquation, obtains spinning liquation;
4) by step 3) the spinning liquation bore dia that obtains is that the platinum-rhodium alloy bushing of 60 μm carries out wire drawing, obtains the basalt blended fiber containing nanometer calcium silicate whisker and sodium chloride;
5) by step 4) to be directly immersed in temperature be in 40 DEG C of sizing agents for the blended fiber that obtains, cool fast, take out for subsequent use;
6) to be immersed in temperature be in 60 DEG C of distilled water to blended fiber step 5) cooled, and be 600W with power, frequency is that the ultrasonic wave of 80KHz carries out concussion process 40min simultaneously, repeatedly immersion 7 times afterwards taking-up dry and obtain porous basalt fiber.
The porous basalt fiber that the present embodiment prepares is through inspection, and performance is as follows:
| Performance | Structure | Density (g/cm) | Porosity (%) | Diameter (μm) |
| Result | Porous fibrous structure | 0.75 | 75 | 12 |
Comparative example
1) basalt ore is immersed in pond, rinse, the impurity that removing surface may be adhered to, then take out and dry, the basalt ore dried and sodium chloride pulverizer are carried out pulverization process, and wherein basalt ore is 1: 3 with the mass ratio mixed of inorganic salts, mixes after pulverizing, fineness is 3.0mm, obtains the mixed powder of basalt and sodium chloride;
2) by step 1) obtain mixed powder and join in kiln, be warming up to 1400 DEG C, make the complete melting of mixed powder, and Keep agitation, form mixed molten liquid;
3) by step 2) the mixed molten liquid bore dia that obtains is that the platinum-rhodium alloy bushing of 60 μm carries out wire drawing, obtains the basalt blended fiber containing sodium chloride;
4) by step 3) to be directly immersed in temperature be in 40 DEG C of sizing agents for the blended fiber that obtains, cool fast, take out for subsequent use;
5) to be immersed in temperature be in 60 DEG C of distilled water to blended fiber step 4) cooled, and be 600W with power, frequency is that the ultrasonic wave of 80KHz carries out concussion process 40min simultaneously, repeatedly immersion 7 times afterwards taking-up dry and obtain porous particle not of uniform size.
Owing to not adding nano inorganic toughening material in above-mentioned comparative example, lacking toughness, easily rupture when carrying out wire drawing in step 3), wire drawing is very difficult, what obtain is blended fiber different in size, through step 4), 5) process, sodium chloride is dissolved, but due to lacking toughness and support, hole collapses, fibre structure is destroyed, the fibre structure of porous can not be formed, also can not get porous basalt fiber, it can thus be appreciated that adding of nano inorganic toughening material ensures the fibroplastic necessary condition of porous basalt.
Claims (10)
1. a preparation method for porous basalt fiber, is characterized in that preparation process is as follows:
1) basalt ore and inorganic salts pulverizer are pulverized, and mix, obtain the mixed powder of basalt and inorganic salts;
2) by step 1) obtain mixed powder and join in kiln, heat up, make mixed powder melting, form mixed molten liquid;
3) in step 2) add toughening material in the liquation that obtains, obtain spinning liquation;
4) by step 3) the spinning liquation that obtains carries out spinning, obtains basalt blended fiber;
5) by step 4) blended fiber that obtains is immersed in sizing agent, cools;
6) blended fiber that step 5) cools is immersed in water, carries out dissolution process, dry and obtain porous basalt fiber.
2. the preparation method of porous basalt fiber according to claim 1, is characterized in that step 1) in basalt ore be 1: 0.5-4 with the mass ratio mixed of inorganic salts.
3. the preparation method of porous basalt fiber according to claim 1, is characterized in that described inorganic salts are one or more in sodium sulphate, potassium sulfate, potassium chloride, sodium chloride.
4. the preparation method of porous basalt fiber according to claim 1, is characterized in that the use amount of described toughening material is the 2%-10% of basalt and inorganic salts gross mass.
5. the preparation method of porous basalt fiber according to claim 1, is characterized in that described toughening material is one or more of nano inorganic particle and nano inorganic whisker; Nano inorganic particle is one or more in the silica of diameter≤50nm, carborundum, silicon nitride aluminum nanoparticles; Nano inorganic whisker is one or more in the nano whisker of length≤100nm, the titanium nitride of draw ratio >=5, aluminium carbide, calcium silicates.
6. the preparation method of porous basalt fiber according to claim 1, is characterized in that described sizing agent is the one in aqueous polyurethane sizing agent, water-soluble epoxy resin sizing agent.
7. the preparation method of porous basalt fiber according to claim 6, is characterized in that described sizing agent temperature is 0-50 DEG C.
8. the preparation method of porous basalt fiber according to claim 1, is characterized in that described coolant-temperature gage is 40-100 DEG C.
9. the preparation method of porous basalt fiber according to claim 1, it is characterized in that using ultrasonic oscillation accelerate dissolution, ultrasonic power is 600-800W, and frequency is 40-80KHz.
10. the preparation method of porous basalt fiber according to claim 1, is characterized in that described porous basalt fibre diameter is 0.5-50 μm, porosity 10%-80%.
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| CN108929463A (en) * | 2017-05-24 | 2018-12-04 | 江苏创曦复合材料科技有限公司 | A kind of high-performance composite materials and preparation method thereof |
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| 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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