CN105442098B - A kind of toughness SiO of PVP coatings2The preparation method of airsetting glue fiber - Google Patents

A kind of toughness SiO of PVP coatings2The preparation method of airsetting glue fiber Download PDF

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CN105442098B
CN105442098B CN201511027755.1A CN201511027755A CN105442098B CN 105442098 B CN105442098 B CN 105442098B CN 201511027755 A CN201511027755 A CN 201511027755A CN 105442098 B CN105442098 B CN 105442098B
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fiber
sio
pvp
toughness
acid
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CN105442098A (en
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朱美芳
孟思
舒鑫
周哲
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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
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • 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
    • 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
    • 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
    • D01F9/10—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/356—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms
    • D06M15/3562—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms containing nitrogen

Abstract

The present invention relates to a kind of toughness SiO of PVP coatings2The preparation method of airsetting glue fiber.Preparation method, including：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, is wound, ageing, washs to neutrality, carries out solvent displacement, dry；Dried fiber is immersed in the PVP aqueous solution, is taken out, and is dried, is produced.Method used in the present invention has the characteristics of raw material is cheap and easily-available, course of reaction is simple, good spinnability, obtained inorganic SiO2Airsetting glue fiber has abundant hole, high specific surface area, high temperature resistant, resistant to chemical etching, while pulp freeness is adjustable, has certain toughness, can expand the application of airsetting glue fiber, more with practical value.

Description

A kind of toughness SiO of PVP coatings2The preparation method of airsetting glue fiber
Technical field
The invention belongs to airsetting glue fiber and its preparation field, more particularly to a kind of toughness SiO of PVP coatings2Aeroge The preparation method of fiber.
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 there is no 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, and 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 The process related to interface interaction, such as absorption, catalysis and electrochemical action；Its duct can be used as Multifunctional memory and single point Scattered nano-reactor；Its special nano pore and it is shaped as space and field that the research of cross discipline brings and its enriched 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, them are made to turn into the heat in investigation of materials field One of point.
The performance of aeroge also has important in addition to relevant with its microscopic appearance with composite porous macro morphology Relation.For SiO2Aerogel material, nowadays have 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 higher several times to tens times 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 construction, 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, is easily stacked, and its adsorption rate is slower, and separative efficiency is not high, particularly its thing Reason form has many inconvenience in application, limits application.NACF aperture is small and narrowly distributing, and adsorption rate is fast, Adsorbance is big, regenerating easily.Compared with powdery (5nm~30nm) activated carbon, NACF is caused micro- in use Dust is few, can be made into the product of the variforms such as yarn, line, fabric, felt, more flexible and convenient during use.It is and block or membranaceous 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 SiO2Gas Fibre morphology is made in gel, and its performance will be made more excellent.
But due to SiO2Aeroge is inorganic material, and it is internal again with the presence of a large amount of holes so that SiO2Aeroge is very crisp It is weak, frangible.And SiO is made2After airsetting glue fiber, it is easier to fracture.In order that SiO2The excellent in performance of airsetting glue fiber is more Extensive field is applied, and needs me badly to SiO2Airsetting glue fiber is modified, and it is become tough.
At present on a kind of toughness SiO using PVP coatings2The document 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 toughness SiO of PVP coatings2The preparation side of airsetting glue fiber Method, this method has the characteristics of raw material is cheap and easily-available, course of reaction is simple, good spinnability, obtained to use the one of PVP coatings Kind toughness SiO2Airsetting glue fiber has the abundant hole, specific surface area of superelevation, high temperature resistant, resistant to chemical etching, while fiber Specific surface area is adjustable, there is certain toughness, can expand the application of airsetting glue fiber, more with practical value.
The toughness SiO of the PVP coatings of the present invention2Airsetting glue fiber, the hole of the airsetting glue fiber is in nanoscale model Enclose, and specific surface area size can be adjusted by changing preparation condition.
A kind of toughness SiO of PVP coatings 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 coagulating bath, carries out reaction wet spinning, obtain orthosilicic acid/silicic acid Salt fiber；Spinning solution runs into coagulating bath acid and quick strong acid weak acid reaction generation solid phase orthosilicic acid occurs, and realizes Wet-spinning Quick liquid-solid phase transformation required by silk, forms orthosilicic acid/silicate fiber, simultaneously collosol and gel occurs for this process；
(4) orthosilicic acid in step (3)/silicate fiber is wound, is then immersed in normal temperature ageing 2~10 in aged solution My god；Make orthosilicic acid/silicate fiber that collosol and gel further occur, realize from orthosilicic acid/silicate fiber to SiO2Fiber Transformation, while form a large amount of holes；
(5) fiber after being aged in step (4) is washed with deionized to neutrality, solvent displacement is carried out using ethanol, And dry at normal temperatures；
(6) dried fiber in step (5) is immersed in the PVP aqueous solution that concentration is 5wt%~15wt% after 5min, Take out, repeat to immerse PVP and drying process 2-5 time, dry, obtain the toughness SiO that PVP is coated2Airsetting glue fiber.
Silicate is sodium silicate, KP1 or nine water sodium metasilicate in the step (1), and silanol colloidal sol is positive silicic acid second Ester, MTES, MTMS or phenyltrimethoxysila,e are hydrolyzed into molten under the conditions of diluted acid Glue.
Spinning solution sodium silicate, the modulus of KP1 are 2~3 in the step (1), and Baume degrees is 35~50, nine Water sodium metasilicate directly heats into solution without solubilizer again, and the viscosity of silanol colloidal sol is 0.01~0.1PaS, and silicone content is more than 10wt%.
In the step (2) acid solution be concentration be 0.2mol/L~0.8mol/L dilution heat of sulfuric acid, concentration be 0.4mol/L~1.2mol/L dilute hydrochloric acid solution or concentration is 12mol/L~15mol/L acetic acid.
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.
Dried in the step (6) as freeze-drying or supercritical drying.
A kind of toughness SiO that the present invention is coated using PVP2The preparation method of airsetting glue fiber, using strong acid weak acid and Collosol and gel principle, SiO is prepared by reacting spinning2Airsetting glue fiber.Then using a kind of toughness SiO of PVP coatings2Gas Gelatinous fibre surface, supporting layer is formed on surface, so as to prepare a kind of toughness SiO2The preparation of airsetting glue fiber.
The present invention will mix the cellulose solution of different proportion as spinning solution in cheap silicate and silanol colloidal sol, Using different acid solutions as coagulating bath, reacted by silicate and silanol colloidal sol with acid generation strong acid weak acid and colloidal sol occurs Gelation, part generate the orthosilicic acid of solid phase, obtain orthosilicic acid/silicate fiber, wound fiber by take-up roll.With Afterwards, orthosilicic acid/silicate fiber of winding is immersed in low concentration acid solution and be aged, fiber is made by ageing process Collosol and gel is further carried out, is realized from orthosilicic acid/silicate fiber to SiO2Fiber changes, while forms a large amount of holes. After ageing, washed using deionized water, then carry out solvent displacement using ethanol.PVP solution is being used to fiber table Face is coated, and a kind of toughness SiO using PVP coatings is obtained finally by freeze-drying or supercritical drying2Aeroge is fine Dimension, there is novelty.A kind of prepared toughness SiO coated using PVP2Airsetting glue fiber is in catalysis, absorption, filtering, guarantor There is more prominent advantage in the fields such as temperature, dress ornament, there is very huge potential demand, there is practicality.
After being dried at room temperature in the present invention, fiber is immersed in PVP solution after 5min, taken out, is dried, repeat to immerse PVP and drying process 5 times.The fiber for having soaked PVP is obtained finally using PVP coatings by freeze-drying or supercritical drying A kind of toughness SiO2Airsetting glue fiber.Method used in the present invention has that raw material is cheap and easily-available, course of reaction is simple, spinnability The characteristics of good, obtained inorganic SiO2Airsetting glue fiber has abundant hole, high specific surface area, high temperature resistant, chemically-resistant Corrosion, while pulp freeness is adjustable, has certain toughness, can expand the application of airsetting glue fiber, with more practicality Value.
Beneficial effect
Method used in the present invention has the characteristics of raw material is cheap and easily-available, course of reaction is simple, good spinnability, obtained Inorganic SiO2Airsetting glue fiber has abundant hole, high specific surface area, high temperature resistant, resistant to chemical etching, while fiber ratio Surface area is adjustable, has certain toughness, can expand the application of airsetting glue fiber, more with practical value.
Brief description of the drawings
Fig. 1 is the toughness SiO that PVP is coated in embodiment 12Airsetting glue fiber fastens thing figure；
Fig. 2 is the toughness SiO that PVP is coated in embodiment 12The SEM figures of aeroge fiber surface morphology；
Fig. 3 is the toughness SiO that PVP is coated in embodiment 12Aeroge fiber hole pattern SEM schemes.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited Scope.
Embodiment 1
Using modulus as 2, the sodium silicate of 50 Baume degrees is spinning solution, using 0.8mol/L dilution heat of sulfuric acid as solidification Bath, carries out reaction wet spinning.Orthosilicic acid/the silicate fiber formed in coagulating bath is rolled up with 0.1m/s winding speed 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.Entered using ethanol Row solvent is replaced, and is dried at normal temperatures.Fiber is immersed after drying in the 10wt% PVP aqueous solution after 5min, taking-up, repetition Immerse PVP and drying process 5 times.It is last freeze-dried, produce a kind of toughness SiO coated using PVP2Airsetting glue fiber. The obtained toughness SiO coated using PVP2Aeroge pulp freeness is 483.2m2/ g, most probable pore size 8nm, fiber It can knot.The obtained toughness SiO coated using PVP2It is as shown in Figure 1 that airsetting glue fiber fastens thing figure；It is obtained to use PVP The toughness SiO of coating2The SEM figures of aeroge fiber surface morphology are as shown in Figure 2；The obtained toughness SiO coated using PVP2Gas Gelatinous fibre hole pattern SEM figures are as shown in Figure 3.
Embodiment 2
Using modulus as 3, the KP1 of 35 Baume degrees is spinning solution, using 0.2mol/L dilution heat of sulfuric acid as solidification Bath, carries out reaction wet spinning.The orthosilicic acid formed in coagulating bath/sodium metasilicate fiber is rolled up with 0.5m/s winding speed 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.Entered using ethanol Row solvent is replaced, and is dried at normal temperatures.Fiber is immersed after drying in the 5wt% PVP aqueous solution after 5min, taking-up, repetition Immerse PVP and drying process 4 times.It is last freeze-dried, produce the toughness SiO coated using PVP2Airsetting glue fiber.It is made Using PVP coat toughness SiO2Aeroge pulp freeness is 352.4m2/ g, most probable pore size 7nm, fiber bendable It is bent.
Embodiment 3
Using modulus as 3, the KP1 of 35 Baume degrees is spinning solution, using 0.8mol/L dilution heat of sulfuric acid as solidification Bath, carries out reaction wet spinning.The orthosilicic acid formed in coagulating bath/potassium silicate fiber is rolled up with 1m/s winding speed 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.Carried out using ethanol molten Agent is replaced, and is dried at normal temperatures.Fiber is immersed after drying in the 15wt% PVP aqueous solution after 5min, taking-up, repeat to immerse PVP and drying process 3 times.It is last freeze-dried, produce the toughness SiO coated using PVP2Airsetting glue fiber.It is obtained to make The toughness SiO coated with PVP2Aeroge pulp freeness is 316.4m2/ g, most probable pore size 8nm, fiber can knot.
Embodiment 4
Using nine water sodium metasilicate directly heat solution as spinning solution, using 0.4mol/L dilute hydrochloric acid solution as coagulating bath, Carry out reaction wet spinning.Orthosilicic acid/the silicate fiber formed in coagulating bath is wound with 2m/s winding speed.Volume The watery 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.Solvent is carried out using ethanol to put Change, and dry at normal temperatures.Fiber is immersed after drying in the 10wt% PVP aqueous solution after 5min, taking-up, repeat to immerse PVP And drying process 2 times.It is last freeze-dried, produce the toughness SiO coated using PVP2Airsetting glue fiber.Obtained use The toughness SiO of PVP coatings2Aeroge pulp freeness is 182.9m2/ g, most probable pore size 10nm, fiber are flexible.
Embodiment 5
Using nine water sodium metasilicate directly heat solution as spinning solution, using 1.2mol/L dilute hydrochloric acid solution as coagulating bath, Carry out reaction wet spinning.Orthosilicic acid/the silicate fiber formed in coagulating bath is wound with 1m/s winding speed.Volume The watery 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.Solvent is carried out using ethanol to put Change, and dry at normal temperatures.Fiber is immersed after drying in the 10wt% PVP aqueous solution after 5min, taking-up, repeat to immerse PVP And drying process 5 times.It is last freeze-dried, produce the toughness SiO coated using PVP2Airsetting glue fiber.Obtained use The toughness SiO of PVP coatings2Aeroge pulp freeness is 207.7m2/ g, most probable pore size 10nm, fiber are flexible.
Embodiment 6
Viscosity 0.01PaS, silicon content 12wt% colloidal sol is hydrolyzed into as spinning solution using tetraethyl orthosilicate plus watery hydrochloric acid, Using 12mol/L acetum as coagulating bath, reaction wet spinning is carried out.The orthosilicic acid formed in coagulating bath/silicate is fine Dimension is wound with 1m/s winding speed.The oxalic acid that fiber after winding immerses 0.005mol/L is aged for 10 days, is realized From orthosilicic acid fiber to SiO2Fiber changes, while forms a large amount of holes.After ageing, fiber is washed with deionized, until It is neutral.Solvent displacement is carried out using ethanol, and is dried at normal temperatures.Fiber is immersed in the 10wt% PVP aqueous solution after drying After 5min, take out, repeat to immerse PVP and drying process 5 times.Most produce the toughness coated using PVP through supercritical drying afterwards SiO2Airsetting glue fiber.The obtained toughness SiO coated using PVP2Aeroge pulp freeness is 384.1m2/ g, most probable Aperture is 4nm, and fiber can knot.
Embodiment 7
Viscosity 0.05PaS, silicon content 18wt% colloidal sol are hydrolyzed into as spinning using MTES plus watery hydrochloric acid Silk stock solution, using 15mol/L acetum as coagulating bath, carry out reaction wet spinning.Orthosilicic acid/the silicon that will be formed in coagulating bath Silicate fiber is wound with 1m/s winding speed.The oxalic acid that fiber after winding immerses 0.1mol/L is aged for 5 days, real Now from orthosilicic acid fiber to SiO2Fiber changes, while forms a large amount of holes.After ageing, fiber is washed with deionized, directly To neutrality.The solvent in fiber is replaced using absolute ethyl alcohol, and is dried at normal temperatures.Fiber is immersed 10wt%'s after drying In the PVP aqueous solution after 5min, take out, repeat to immerse PVP and drying process 5 times, through supercritical drying, produce and coated using PVP Toughness SiO2Airsetting glue fiber.The obtained toughness SiO coated using PVP2Aeroge pulp freeness is 592.5m2/ g, Most probable pore size is 4nm, and fiber can knot.
Embodiment 8
Viscosity 0.1PaS, silicon content 22wt% colloidal sol are hydrolyzed into as spinning using MTMS plus watery hydrochloric acid Stoste, using 15mol/L acetum as coagulating bath, carry out reaction wet spinning.Orthosilicic acid/the silicic acid that will be formed in coagulating bath Salt fiber is wound with 1m/s winding speed.The oxalic acid that fiber after winding immerses 0.1mol/L is aged for 5 days, is realized From orthosilicic acid fiber to SiO2Fiber changes, while forms a large amount of holes.After ageing, fiber is washed with deionized, until It is neutral.The solvent in fiber is replaced using absolute ethyl alcohol, and is dried at normal temperatures.Fiber is immersed to 10wt% PVP after drying In the aqueous solution after 5min, take out, repeat to immerse PVP and drying process 5 times, through supercritical drying, produce using the tough of PVP coatings Property SiO2Airsetting glue fiber.The obtained toughness SiO coated using PVP2Aeroge pulp freeness is 629.4m2/ g, most may be used Several apertures are 4nm, and fiber can knot.
Embodiment 9
Viscosity 0.08PaS, silicon content 20wt% colloidal sol are hydrolyzed into as spinning using phenyltrimethoxysila,e plus watery hydrochloric acid Silk stock solution, using 15mol/L glacial acetic acid solution as coagulating bath, carry out reaction wet spinning.By the orthosilicic acid formed in coagulating bath/ Silicate fiber is wound with 1m/s winding speed.The oxalic acid that fiber after winding immerses 0.1mol/L is aged for 5 days, Realize from orthosilicic acid fiber to SiO2Fiber changes, while forms a large amount of holes.After ageing, fiber is washed with deionized, It is until neutral.The solvent in fiber is replaced using absolute ethyl alcohol, and is dried at normal temperatures.Fiber is immersed 10wt%'s after drying In the PVP aqueous solution after 5min, take out, repeat to immerse PVP and drying process 5 times, through supercritical drying, produce and coated using PVP Toughness SiO2Airsetting glue fiber.The obtained toughness SiO coated using PVP2Aeroge pulp freeness is 536.4m2/ g, Most probable pore size is 4nm, and fiber can knot.

Claims (4)

  1. A kind of 1. toughness SiO of PVP coatings2The preparation method of airsetting glue fiber, including：
    (1) silicate is configured to spinning solution；Wherein, silicate is sodium silicate, KP1 or nine water sodium metasilicate, spinning The specification of stoste is：Sodium silicate, the modulus of KP1 are 2~3, and Baume degrees is 35~50, and nine water sodium metasilicate directly heat Into solution without solubilizer again；
    (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 0.8mol/L dilution heat of sulfuric acid, concentration are 0.4mol/L~1.2mol/L be 12mol/L~ 15mol/L acetic acid；
    (3) spinning solution in step (1) is added in coagulating bath, carries out reaction wet spinning, part generates the former silicon of solid phase Acid, obtain orthosilicic acid/silicate fiber；
    (4) orthosilicic acid in step (3)/silicate fiber is wound, is then immersed in normal temperature in aged solution and is aged 2~10 days； Wherein, aged solution be concentration be 0.005mol/L~0.1mol/L dilution heat of sulfuric acid, concentration be 0.01mol/L~ 0.2mol/L dilute hydrochloric acid solution or concentration is 0.005mol/L~0.1mol/L oxalic acid；
    (5) fiber after being aged in step (4) is washed with deionized to neutrality, using ethanol progress solvent displacement, and Dried under normal temperature；
    (6) after dried fiber in step (5) being immersed into concentration for 5min in the 5wt%~15wt% PVP aqueous solution, take Go out, repeat to immerse PVP, dry, obtain the toughness SiO of PVP coatings2Airsetting glue fiber.
  2. A kind of 2. toughness SiO of PVP coatings according to claim 12The preparation method of airsetting glue fiber, it is characterised in that The condition of reaction wet spinning is normal temperature and pressure in the step (3).
  3. A kind of 3. toughness SiO of PVP coatings according to claim 12The preparation method of airsetting glue fiber, it is characterised in that The speed of winding is 0.1~2m/s in the step (4).
  4. A kind of 4. toughness SiO of PVP coatings according to claim 12The preparation method of airsetting glue fiber, it is characterised in that Dried in the step (6) as freeze-drying or supercritical drying.
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