CN105671687B - A kind of continuous SiO2The preparation method of airsetting glue fiber - Google Patents

A kind of continuous SiO2The preparation method of airsetting glue fiber Download PDF

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CN105671687B
CN105671687B CN201511029850.5A CN201511029850A CN105671687B CN 105671687 B CN105671687 B CN 105671687B CN 201511029850 A CN201511029850 A CN 201511029850A CN 105671687 B CN105671687 B CN 105671687B
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fiber
solution
acid
sio
silicate
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CN105671687A (en
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朱美芳
孟思
陆秋旭
江晓泽
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Donghua University
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/152—Preparation of hydrogels
    • C01B33/154—Preparation of hydrogels by acidic treatment of aqueous silicate solutions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157—After-treatment of gels
    • C01B33/158—Purification; Drying; Dehydrating
    • C01B33/1585—Dehydration into aerogels
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/06—Wet spinning methods

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  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Silicon Compounds (AREA)
  • Inorganic Fibers (AREA)

Abstract

The present invention relates to a kind of continuous SiO2The preparation method of airsetting glue fiber.Preparation method includes：Silicate or silanol colloidal sol are configured to spinning solution；Acid solution is added in coagulating basin as coagulating bath；Spinning solution is added in coagulating bath, carries out reaction wet spinning, obtains orthosilicic acid/silicate fiber；By orthosilicic acid/silicate fiber winding, immerse room temperature in aged solution and be aged 2~10 days, be washed with deionized to neutrality, then carry out solvent displacement, it is dry, to obtain the final product.The method of the present invention has the characteristics that raw material is cheap and easily-available, reaction process is simple, good spinnability, solves SiO2Aeroge is difficult to the problem for being spun into fibre.Inorganic SiO prepared by the present invention2Airsetting glue fiber has abundant hole, high specific surface area, high temperature resistant, resistant to chemical etching, while pulp freeness is adjustable, available for fields such as catalyst carrier field and adsorption filtrations.

Description

A kind of continuous SiO2The preparation method of airsetting glue fiber
Technical field
The invention belongs to the preparation field of airsetting glue fiber, more particularly to a kind of continuous SiO2The preparation side of airsetting glue fiber Method.
Background technology
The medium that aeroge (aerogel) refers to be full of in the spacial framework in gel is not solvent but gas, Appearance is in the special gel of solid-like, because almost without solvent composition inside it, therefore also referred to as xerogel.Aeroge is A kind of nano-meter porous amorphous state solid material of low-density, has unique structure, its solid phase forms spacial framework, net Network structure and internetwork pore structure are all Nano grade.Because of the uniqueness of its structure, aeroge is set equally to have many only Characteristic energy, such as high porosity, high-ratio surface, strong adsorptivity, low-density, low acoustic impedance, low heat conductivity, low refraction.
SiO2Its high-specific surface area of aeroge can provide substantial amounts of reaction/interaction activated centre, be particularly conducive to With the relevant process of interface interaction, such as absorption, catalysis and electrochemical action；Its duct can be used as Multifunctional memory and single point Scattered nano-reactor；The space and field that its special nano pore and shape bring and its enrich for the research of cross discipline Institute, such as the dispersal behavior of biomolecule, drug molecule, reactant molecule in nano pore, the contact with activated centre Energy, reactivity etc. all have close relationship with pore structure；And skin effect caused by the network structure of its nanoscale and Quantum size effect, the SiO for making some pass through functional modification2Aerogel material is in sensor, lithium battery and nano-device Show excellent performance；Before its lower thermal conductivity makes it have huge applications in fields such as insulated wall, heat-insulation window, tent thermal insulation layers Scape.Exactly unique advantage of the aeroge in micro interface structure and material property, makes them become the heat in investigation of materials field One of point.
The performance of aeroge also has important in addition to related with its microscopic appearance with composite porous macro morphology Relation.For SiO2Aerogel material, nowadays has substantial amounts of document report zero dimension powder, two-dimensional film, three-dimensional block, But to one-dimensional SiO2Airsetting glue fiber is but seldom reported.The porous material of this other dimension that are primarily due to compare, fiber Shape porous material has more requirements to preparing raw material, preparation condition etc..However, fibrous porous material but have it is other Excellent properties not available for dimension material.Analogy is similarly the porous active carbon fiber of inorganic porous fiber, traditional activity Charcoal is a kind of porous charcoal by activation process, is powdered or graininess, and activated carbon fiber is then threadiness, cloth on fiber Full micropore, it is several times to tens times higher in atmosphere than granular activated carbon to organic gas adsorption capacity, high by 5 in aqueous~ 6 times, fast 100~1000 times of the rate of adsorption.The fibre diameter of activated carbon fiber is 5~20 μm, specific surface area it is average 1000~ 1500m2/ g or so, average pore size are uniformly distributed in fiber surface in 1.0~4.0nm, micropore.Compared with activated carbon, activated carbon Fiber micropore size is small and uniform, simple in structure, and fast for the absorption small-molecule substance rate of adsorption, adsorption rate is high, easily solution Absorption.It is big with the contact area of absorbate, and uniformly can contact and adsorb, sorbing material is fully utilized.Efficiency Height, and be directly open in fiber surface with various very thin statements, holes such as fiber, felt, cloth and paper, its adsorbate, which reaches, to be inhaled The diffusion path of attached position is short, and the external surface area of itself is higher by two orders of magnitude compared with internal surface area.In air or water body purification side Face, granular or powdery structure, easily stacks, its adsorption rate is slower, and separative efficiency is not high, particularly its physics Form has many inconvenience in application, limits application range.Activated carbon fibre aperture is small and narrowly distributing, and adsorption rate is fast, inhales Attached amount is big, regenerating easily.Compared with powdery (5nm~30nm) activated carbon, micro mist that activated carbon fibre produces in use Dirt is few, can be made into the product of the variforms such as yarn, line, fabric, felt, and when use is more flexible and convenient.And block or membranaceous knot Structure so that air or water body by when can produce very big resistance, it is very big with the differing pressure after filtering before filter.By SiO2Airsetting Fibre morphology is made in glue, its performance will be made more excellent.
Document report prepares SiO at present2The method of airsetting glue fiber has not been reported.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of continuous SiO2The preparation method of airsetting glue fiber, this method Have the characteristics that raw material is cheap and easily-available, reaction process is simple, good spinnability.Machine SiO is prepared2Fiber has abundant hole It is hole, the specific surface area of superelevation, high temperature resistant, resistant to chemical etching, while pulp freeness is adjustable.
A kind of continuous SiO of the present invention2The preparation method of airsetting glue fiber, including：
(1) silicate or silanol colloidal sol are configured to spinning solution；
(2) acid solution is added in coagulating basin as coagulating bath；
(3) spinning solution in step (1) is added in step (2) in coagulating bath, carries out reaction wet spinning, obtain original Silicic acid/silicate fiber；Spinning solution runs into coagulating bath acid and quick strong acid weak acid reaction generation solid phase orthosilicic acid occurs, real Quick liquid-solid phase transformation required by existing wet spinning, forms orthosilicic acid/silicate fiber, collosol and gel occurs at the same time for this process Change.
(4) orthosilicic acid in step (3)/silicate fiber is wound, immerses room temperature in aged solution and be aged 2~10 days, It is washed with deionized to neutrality, then carries out solvent displacement with deionized water or ethanol, it is dry, obtain continuous SiO2Aeroge Fiber；Ageing make orthosilicic acid/silicate fiber that collosol and gel further occur, realize from orthosilicic acid/silicate fiber to SiO2Fiber changes, while forms a large amount of holes.
Silicate is sodium silicate, potassium water glass or nine water sodium metasilicate in the step (1)；Silanol colloidal sol is positive silicic acid second The hydrolytic sol of ester, methyltriethoxysilane, methyltrimethoxysilane or phenyltrimethoxysila,e under the conditions of diluted acid.
The specification of spinning solution in the step (1)：Sodium silicate, the modulus of potassium water glass are 2~3, Baume degrees 35 ~50, nine water sodium metasilicate directly heat into solution without solubilizer again, and the viscosity of silanol colloidal sol is 0.01~0.1PaS, and silicon contains Amount is more than 10 wt%.
In the step (2) acid solution be concentration be 0.2mol/L~0.8mol/L dilution heat of sulfuric acid, concentration 0.4 The dilute hydrochloric acid solution or concentration of mol/L~1.2mol/L is the acetic acid of 12mol/L~15mol/L.
The condition of reaction wet spinning is normal temperature and pressure in the step (3).
The speed of winding is 0.1~2m/s in the step (4).
Aged solution is preparation low concentration acid solution in the step (4)：Concentration is 0.005mol/L~0.1mol/L's The dilute hydrochloric acid solution or concentration that dilution heat of sulfuric acid, concentration are 0.01mol/L~0.2mol/L are 0.005mol/L~0.1mol/L Oxalic acid.
It is dry for freeze-drying or supercritical drying in the step (4).
The continuous SiO of the present invention2Airsetting glue fiber can continuously be wound, its hole can lead in nanoscale scope Change preparation condition is crossed to adjust specific surface area size.
The present invention utilizes strong acid weak acid and collosol and gel principle, and continuous SiO is realized by reacting spinning2Porous fibre Preparation, finally by freeze-drying or supercritical drying obtain continuous SiO2Airsetting glue fiber, has novelty.Prepared Continuous SiO2Airsetting glue fiber has more prominent advantage in a series of fields such as catalysis, absorption, sensing, has very huge Potential demand, has practicality.
Continuous SiO in the present invention2The preparation method of airsetting glue fiber, is using cheap silicate and silanol colloidal sol as spinning Silk stock solution, using different acid solutions as coagulating bath, occurs the reaction of strong acid weak acid simultaneously by silicate and silanol colloidal sol with acid Generation collosol and gel, part generate solid phase orthosilicic acid, obtain orthosilicic acid/silicate fiber, by take-up roll by fiber into Row winding.Then, orthosilicic acid/silicate fiber of winding is immersed in low concentration acid solution and is aged, pass through ageing Process makes fiber further carry out collosol and gel, realizes from orthosilicic acid/silicate fiber to SiO2Fiber changes, and is formed at the same time A large amount of holes.After ageing, washed using deionized water, then solvent displacement is carried out using ethanol, finally by freezing Dry or supercritical drying obtains final continuous SiO2Airsetting glue fiber.Method used in the present invention is cheaply easy with raw material , the characteristics of reaction process is simple, good spinnability, solve SiO2Aeroge is difficult to the problem for being spun into fibre.Obtained nothing Machine SiO2Airsetting glue fiber has abundant hole, high specific surface area, high temperature resistant, resistant to chemical etching, while specific fiber surface Product is adjustable, available for fields such as catalyst carrier field and adsorption filtrations.
Beneficial effect
(1) method used in the present invention has the characteristics that raw material is cheap and easily-available, reaction process is simple, good spinnability, solution Determined SiO2Aeroge is difficult to the problem for being spun into fibre；
(2) inorganic SiO of the invention2Airsetting glue fiber has abundant hole, high specific surface area, high temperature resistant, resistance to Chemical attack, while pulp freeness is adjustable, available for fields such as catalyst carrier field and adsorption filtrations.
Brief description of the drawings
Fig. 1 is SiO in embodiment 12The microscope figure of aeroge fiber morphology；
Fig. 2 is SiO in embodiment 12Aeroge fibrous inside hole pattern scanning electron microscope (SEM) photograph；
Fig. 3 is SiO in embodiment 12Airsetting glue fiber N2Adsorb De contamination isollaothermic chart；
Fig. 4 is SiO in embodiment 12Aeroge fiber graph of pore diameter distribution；
Fig. 5 is SiO in embodiment 12After aeroge fibers adsorption methylene blue different time, methylene blue removal rate is at any time Between variation diagram.
Embodiment
With reference to specific embodiment, the present invention is further explained.It is to be understood that these embodiments are merely to illustrate the present invention Rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited Scope.
Embodiment 1
Using modulus as 2, the sodium silicate of 50 Baume degrees is spinning solution, using the dilution heat of sulfuric acid of 0.8mol/L as solidification Bath, carries out reaction wet spinning.Orthosilicic acid/the silicate fiber formed in coagulating bath is rolled up with the winding speed of 0.1m/s Around.The dilute sulfuric acid that fiber after winding immerses 0.005mol/L is aged for 10 days, realize from orthosilicic acid/silicate fiber to SiO2Fiber changes, while forms a large amount of holes.After ageing, fiber is washed with deionized, until neutral.Use deionization Solution in water displacement fiber, it is freeze-dried, up to SiO2Airsetting glue fiber.It is very smooth in spinning process, not fracture of wire.System The SiO obtained2Aeroge pulp freeness is 565.8m2/ g, most probable pore size 10nm.5min can reach absorption methylene The 64% of blue maximal absorptive capacity.Obtained SiO2The microscope figure of aeroge fiber morphology is as shown in Figure 1；Obtained SiO2Airsetting Glue fiber inner void topography scan electron microscope is as shown in Figure 2；Obtained SiO2Airsetting glue fiber N2Adsorb De contamination isollaothermic chart As shown in Figure 3；Obtained SiO2Aeroge fiber graph of pore diameter distribution is as shown in Figure 4；Obtained SiO2Aeroge fibers adsorption methylene After base indigo plant different time, it is as shown in Figure 5 that methylene blue removal rate changes over time figure.
Embodiment 2
Using modulus as 3, the potassium water glass of 35 Baume degrees is spinning solution, using the dilution heat of sulfuric acid of 0.2mol/L as solidification Bath, carries out reaction wet spinning.The orthosilicic acid formed in coagulating bath/sodium metasilicate fiber is rolled up with the winding speed of 0.5m/s Around.The dilute sulfuric acid that fiber after winding immerses 0.005mol/L is aged for 10 days, realize from orthosilicic acid/silicate fiber to SiO2Fiber changes, while forms a large amount of holes.After ageing, fiber is washed with deionized, until neutral.Use deionization Solution in water displacement fiber, it is freeze-dried, up to SiO2Airsetting glue fiber.There is fracture of wire phenomenon in spinning process once in a while.System The SiO obtained2Aeroge pulp freeness is 421.6m2/ g, most probable pore size 10nm.5min can reach absorption methylene The 59% of blue maximal absorptive capacity.
Embodiment 3
Using modulus as 3, the potassium water glass of 35 Baume degrees is spinning solution, using the dilution heat of sulfuric acid of 0.8mol/L as solidification Bath, carries out reaction wet spinning.The orthosilicic acid formed in coagulating bath/potassium silicate fiber is rolled up with the winding speed of 1m/s Around.The dilute sulfuric acid that fiber after winding immerses 0.1mol/L is aged for 5 days, is realized from orthosilicic acid/silicate fiber to SiO2 Fiber changes, while forms a large amount of holes.After ageing, fiber is washed with deionized, until neutral.Put using deionized water The solution in fiber is changed, it is freeze-dried, up to SiO2Airsetting glue fiber.There is fracture of wire phenomenon in spinning process once in a while.It is obtained SiO2Aeroge pulp freeness is 435.4m2/ g, most probable pore size 11nm.5min can reach absorption methylene blue most The 60% of big adsorbance.
Embodiment 4
Using nine water sodium metasilicate directly heat solution as spinning solution, using the dilute hydrochloric acid solution of 0.4mol/L as coagulating bath, Carry out reaction wet spinning.Orthosilicic acid/the silicate fiber formed in coagulating bath is wound with the winding speed of 2m/s.Volume The dilute hydrochloric acid that fiber after immerses 0.01mol/L is aged for 10 days, is realized from orthosilicic acid/sodium metasilicate fiber to SiO2Fiber Transformation, while form a large amount of holes.After ageing, fiber is washed with deionized, until neutral.Replaced using deionized water fine Solution in dimension, it is freeze-dried, up to SiO2Airsetting glue fiber.Often fracture of wire phenomenon occurs in spinning process.Obtained SiO2 Aeroge pulp freeness is 252.3m2/ g, most probable pore size 15nm.5min can reach the maximum suction of absorption methylene blue The 38% of attached amount.
Embodiment 5
Using nine water sodium metasilicate directly heat solution as spinning solution, using the dilute hydrochloric acid solution of 1.2mol/L as coagulating bath, Carry out reaction wet spinning.Orthosilicic acid/the silicate fiber formed in coagulating bath is wound with the winding speed of 1m/s.Volume The dilute hydrochloric acid that fiber after immerses 0.2mol/L is aged for 2 days, is realized from orthosilicic acid/sodium metasilicate fiber to SiO2Fiber turns Become, while form a large amount of holes.After ageing, fiber is washed with deionized, until neutral.Fiber is replaced using deionized water In solution, it is freeze-dried, up to SiO2Airsetting glue fiber.Fracture of wire phenomenon occurs in spinning process once in a while.Obtained SiO2Gas Gelatinous fibre specific surface area is 285.5m2/ g, most probable pore size 17nm.5min can reach absorption methylene blue maximum adsorption The 40% of amount.
Embodiment 6
The colloidal sol of viscosity 0.01PaS, silicon content 12wt% is hydrolyzed into as spinning solution using ethyl orthosilicate plus dilute hydrochloric acid, Using the acetum of 12 mol/L as coagulating bath, reaction wet spinning is carried out.The orthosilicic acid formed in coagulating bath/silicate is fine Dimension is with the winding speed of 1 m/s.The oxalic acid that fiber after winding immerses 0.005mol/L is aged for 10 days, is realized by orthosilicic acid Fiber is to SiO2Fiber changes, while forms a large amount of holes.After ageing, fiber is washed with deionized, until neutral.Make The solution in fiber is replaced with deionized water, through supercritical drying, up to SiO2Airsetting glue fiber.Occur once in a while in spinning process Fracture of wire phenomenon.Obtained SiO2Aeroge pulp freeness is 440.3m2/ g, most probable pore size 6nm.5min can reach Adsorb the 60% of methylene blue maximal absorptive capacity.
Embodiment 7
The colloidal sol of viscosity 0.05PaS, silicon content 18wt% are hydrolyzed into as spinning using methyltriethoxysilane plus dilute hydrochloric acid Silk stock solution, using the acetum of 15mol/L as coagulating bath, carries out reaction wet spinning.Orthosilicic acid/the silicon that will be formed in coagulating bath Silicate fiber is with the winding speed of 1m/s.The oxalic acid that fiber after winding immerses 0.1mol/L is aged for 5 days, is realized by former silicon Sour fiber is to SiO2Fiber changes, while forms a large amount of holes.After ageing, fiber is washed with deionized, until neutral.Make The solution in fiber is replaced with absolute ethyl alcohol, through supercritical drying, up to SiO2Airsetting glue fiber.Do not break in spinning process Silk phenomenon.Obtained SiO2Aeroge pulp freeness is 650.3m2/ g, most probable pore size 8nm.5min can reach suction The 64% of attached methylene blue maximal absorptive capacity.
Embodiment 8
The colloidal sol of viscosity 0.1PaS, silicon content 22wt% are hydrolyzed into as spinning using methyltrimethoxysilane plus dilute hydrochloric acid Stoste, using the acetum of 15mol/L as coagulating bath, carries out reaction wet spinning.Orthosilicic acid/the silicic acid that will be formed in coagulating bath Salt fiber is with the winding speed of 1m/s.The oxalic acid that fiber after winding immerses 0.1mol/L is aged for 5 days, is realized by orthosilicic acid Fiber is to SiO2Fiber changes, while forms a large amount of holes.After ageing, fiber is washed with deionized, until neutral.Use Solution in absolute ethyl alcohol displacement fiber, through supercritical drying, up to SiO2Airsetting glue fiber.Fracture of wire does not occur in spinning process Phenomenon.Obtained SiO2Aeroge pulp freeness is 669.8m2/ g, most probable pore size 5nm.5min can reach absorption The 64% of methylene blue maximal absorptive capacity.
Embodiment 9
The colloidal sol of viscosity 0.08PaS, silicon content 20wt% are hydrolyzed into as spinning using phenyltrimethoxysila,e plus dilute hydrochloric acid Silk stock solution, using the glacial acetic acid solution of 15mol/L as coagulating bath, carries out reaction wet spinning.By the orthosilicic acid formed in coagulating bath/ Silicate fiber is with the winding speed of 1m/s.The oxalic acid that fiber after winding immerses 0.1mol/L is aged for 5 days, is realized by original Silicate fiber is to SiO2Fiber changes, while forms a large amount of holes.After ageing, fiber is washed with deionized, until neutral. The solution in fiber is replaced using absolute ethyl alcohol, through supercritical drying, up to SiO2Airsetting glue fiber.Do not occur in spinning process Fracture of wire phenomenon.Obtained SiO2Aeroge pulp freeness is 608.2m2/ g, most probable pore size 6nm.5min can reach Adsorb the 61% of methylene blue maximal absorptive capacity.

Claims (5)

  1. A kind of 1. continuous SiO2The preparation method of airsetting glue fiber, including：
    (1) silicate is configured to spinning solution；Wherein, silicate is sodium silicate, potassium water glass or nine water sodium metasilicate；
    (2) acid solution is added in coagulating basin as coagulating bath；Wherein, acid solution be concentration be 0.2mol/L~ The dilute hydrochloric acid solution or concentration that the dilution heat of sulfuric acid of 0.8mol/L, concentration are 0.4mol/L~1.2mol/L be 12mol/L~ The acetic acid of 15mol/L；
    (3) spinning solution in step (1) is added in step (2) in coagulating bath, carries out reaction wet spinning, obtain former silicon Acid/silicate fiber；
    (4) orthosilicic acid in step (3)/silicate fiber is wound, immerses room temperature in aged solution and be aged 2~10 days, spend Then ion water washing carries out solvent displacement, drying, obtains continuous SiO to neutrality with deionized water or ethanol2Aeroge is fine Dimension；Wherein, aged solution be concentration be 0.005mol/L~0.1mol/L dilution heat of sulfuric acid, concentration be 0.01mol/L~ The dilute hydrochloric acid solution or concentration of 0.2mol/L is the oxalic acid of 0.005mol/L~0.1mol/L.
  2. A kind of 2. continuous SiO according to claim 12The preparation method of airsetting glue fiber, it is characterised in that the step (1) specification of spinning solution in：Sodium silicate, the modulus of potassium water glass are 2~3, and Baume degrees is 35~50, and nine water sodium metasilicate are straight Connect and be heated into solution without solubilizer, silicone content are more than 10wt% again.
  3. A kind of 3. continuous SiO according to claim 12The preparation method of airsetting glue fiber, it is characterised in that the step (3) condition of reaction wet spinning is normal temperature and pressure in.
  4. A kind of 4. continuous SiO according to claim 12The preparation method of airsetting glue fiber, it is characterised in that the step (4) speed of winding is 0.1~2m/s in.
  5. A kind of 5. continuous SiO according to claim 12The preparation method of airsetting glue fiber, it is characterised in that the step (4) it is dry for freeze-drying or supercritical drying in.
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CN110983490B (en) * 2019-12-24 2022-06-14 中国科学院苏州纳米技术与纳米仿生研究所 Silica aerogel fiber with adjustable transparency and hydrophobicity, preparation method and application
CN111847463B (en) * 2020-08-04 2022-10-18 泰中新材料(山东)有限公司 Preparation method of silicon dioxide nano aerogel fiber
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CN104071796A (en) * 2013-03-28 2014-10-01 北京化工大学 Preparation method of flexible silicon dioxide aerosol
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