CN105970357B - A kind of method that electrostatic spinning prepares the porous superfine fibre of forsterite - Google Patents

A kind of method that electrostatic spinning prepares the porous superfine fibre of forsterite Download PDF

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Publication number
CN105970357B
CN105970357B CN201610353800.0A CN201610353800A CN105970357B CN 105970357 B CN105970357 B CN 105970357B CN 201610353800 A CN201610353800 A CN 201610353800A CN 105970357 B CN105970357 B CN 105970357B
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forsterite
pvp
electrostatic spinning
superfine fibre
fibre
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CN105970357A (en
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魏恒勇
崔燚
季文玲
李慧
魏颖娜
卜景龙
于守武
陈越军
王鹏
王合洋
王志发
李成
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Shanxi Aladdin New Material Co ltd
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North China University of Science and Technology
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0015Electro-spinning characterised by the initial state of the material

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Fibers (AREA)

Abstract

The present invention relates to a kind of methods that electrostatic spinning prepares the porous superfine fibre of forsterite, belong to material science and technology field.The fiber producing processes include: by anhydrous magnesium chloride, ethyl orthosilicate and anhydrous methylene chloride by certain molar ratio reaction solution, then by reaction solution heated gelization processing, cause non-hydrolytic sol-gel reaction and synthesize forsterite gel;Dehydrated alcohol and a certain amount of polyvinylpyrrolidone (PVP) are mixed in a certain ratio and obtain PVP ethanol solution, the forsterite gel of synthesis is dissolved in acquisition spinning precursor liquid in PVP ethanol solution;Spinning precursor liquid is prepared by forsterite xerogel/PVP composite fibre using electrostatic spinning process, then obtains the porous superfine fibre of forsterite after high-temperature calcination.The preparation method of the porous superfine fibre of the forsterite is easy to operate, is easy to control, and manufacturing cost is low, and the present invention can provide a kind of new type high temperature heat-barrier material for fields such as space flight military projects.

Description

A kind of method that electrostatic spinning prepares the porous superfine fibre of forsterite
Technical field
The invention belongs to the preparation fields of forsterite fiber, and it is more to prepare forsterite more particularly to a kind of electrostatic spinning The method of hole superfine fibre.
Background technique
Forsterite (Mg2SiO4) be island structure silicate mineral, have that intensity is high, fusing point high (1980 DEG C), chemistry With the features such as mineralogical stabiliser is good, thermal conductivity low (0.8 ~ 1.0w/ (mk)).Forsterite fiber also have lower bulk density and Thermal coefficient (0.44 ~ 0.70w/ (mk)), can be used as asbestos substitute material and is used for a long time under the high temperature conditions, it may also be used for Manufacture electron tube, the insulating parts such as semiconductor devices, such as micro metal ceramic tube and the vacuum-packed shell of transistor or Shell is used in protection.
Currently, centrifugal drying silk is generallyd use and fiber elongation method prepares forsterite fiber, for example, Gao Shengjun is with mass ratio 80% forsterite powder, 20% quartz sand powder are raw material, are uniformly mixed and are placed in electric arc furnaces, are warming up to 1500 ~ 2000 DEG C Melting, gets rid of a mode by melt, through condensers collection cotton, obtains cellucotton Bear-grudge, through needle thorn and 500 ~ 600 DEG C of heat treatments, obtains Forsterite tapetum fibrosum (800 degree of forsterite refractory fibres: China, CN103058637 [P] 2013-04-27).Mu-Tsun Using magnesium methoxide and ethyl orthosilicate as raw material, precursor sol is prepared by hydrolytic sol gel method, is obtained using drawing process Precursor fibre prepares diameter in forsterite fiber (the Hydrolysis and of 20 ~ 30um after 800 DEG C of calcinings condensation of forsterite precursor alkoxides: modification of the molecular gel structure by acetic acid[J].Journal of Non-Crystalline Solids, 2001, 10: 116-130).Li Yuanbing is uniformly mixed and is placed on using dehydroxylation serpentine, useless forsterite, aluminium oxide and chromium oxide as raw material In resistance furnace or electric arc furnaces, directly gets rid of silk after being warming up to 1600 ~ 1800 DEG C of meltings and prepare a kind of forsterite fiber (magnesium olive Mineral wool and preparation method thereof: China, CN105198226 [P] 2015-12-30).It is synthesized using above-mentioned three kinds of fiber-forming processes Forsterite fiber not only complex process, process is not easy to control, and obtained fibre diameter is coarse, is micrometer fibers, and It is solid fibre.
The forsterite solid fibre thermal conductivity of above-mentioned technology preparation is higher, restricts its answering in fields such as space flight military projects With.From insulating mechanism and the analysis of Influential Factors of ceramic fibre it is found that if ceramic fibre diameter is small and fiber in have it is numerous micro- Hole can further decrease the thermal conductivity of ceramic fibre aggregate.Therefore, preparing forsterite porous fibre is to further decrease it The effective ways of thermal conductivity.By adjusting the porous structure of forsterite fiber, it can not only guarantee that fiber has certain machine Tool intensity reduces its bulk density, reduces solid conductive heat.More importantly nano-micro level cavity independent in fiber By the heat transfer campaign of air in abundant restricted room body, it is average that a large amount of existing cavitys can also highly desirable shorten photon conduction Free path reduces gas flowing heat transfer and radiant heat transfer, drops low-fiber thermal coefficient, and especially reduction radiant heat transfer accounts for leading High-temperature heat conductivity, to meet the requirement of modern space flight military project and civilian sciemtifec and technical sphere to heat-barrier material high-temperature heat insulation performance.
Electrostatic spinning technique is to stretch electrically charged precursor solution under the action of electrostatic field force, solvent evaporation Solidification obtains precursor fibre, then obtains ceramic fibre through high-temperature calcination.Using electrostatic spinning technique not only simple process, but also The porous ceramic fiber that diameter is nano-scale can be prepared.Currently, electrostatic spinning technique be successfully applied to prepare magnesia, The solid fibres such as aluminium oxide, titanium dioxide and mullite.However, preparing the porous superfine fibre of forsterite using method of electrostatic spinning And have not been reported, it is an object of that present invention to provide a kind of methods that method of electrostatic spinning prepares the porous superfine fibre of forsterite.
Summary of the invention
The purpose of the present invention is to provide a kind of methods that electrostatic spinning prepares the porous superfine fibre of forsterite, to overcome Deficiency in the heat-proof quality and technology of preparing of existing forsterite solid fibre.
To achieve the above object, the method that electrostatic spinning provided by the invention prepares the porous superfine fibre of forsterite includes Following steps: (1) pressing certain molar ratio reaction solution for anhydrous magnesium chloride, ethyl orthosilicate and anhydrous methylene chloride, then By reaction solution heated gelization processing, causes non-hydrolytic sol-gel reaction and synthesize forsterite gel;It (2) will be anhydrous Ethyl alcohol and a certain amount of polyvinylpyrrolidone (PVP), which are mixed in a certain ratio, obtains PVP ethanol solution, by the magnesium olive of synthesis Stone gel is dissolved in acquisition spinning precursor liquid in PVP ethanol solution;(3) spinning precursor liquid is prepared into using electrostatic spinning process Forsterite xerogel/PVP composite fibre;(4) forsterite xerogel/PVP composite fibre is obtained into magnesium after high-temperature calcination The porous superfine fibre of olivine.
The composition of the reaction solution are as follows: the mass percent of anhydrous magnesium chloride is 3.5% ~ 9.5%, the quality of ethyl orthosilicate Percentage is 0.5 ~ 1.5%, and the mass percent of methylene chloride is 90 ~ 95%;
The temperature control of the reaction solution heated gelization processing are as follows: heating temperature is 110 ~ 130 DEG C, and gelation time is 16~24h;
PVP ethanol solution composition are as follows: the mass percent of dehydrated alcohol be 65 ~ 95%, PVP(molecular weight be 58000 ~ 1300000) mass percent is 5 ~ 35%;
The composition of the spinning precursor liquid are as follows: the mass percent of forsterite gel is the matter of 1 ~ 5%, PVP ethanol solution Measuring percentage is 95 ~ 99%;
It is described to prepare forsterite xerogel/PVP composite fibre electrostatic spinning process parameter are as follows: spinning voltage 10 ~ 25KV, 0.1 ~ 1.5ml/h of charging rate solidify 5 ~ 40cm of distance;
Forsterite xerogel/PVP the composite fibre prepares the temperature of the porous superfine fibre of forsterite through high-temperature calcination Degree control are as follows: calcination temperature is 800 ~ 1200 DEG C, and heating rate is 1 ~ 10 DEG C/min, 0.5 ~ 5h of soaking time.
The forsterite gel that the present invention is prepared by non-hydrolytic sol-gel method, it is hydrolyzed to need not move through metal alkoxide Journey, directly forms gel by the de- alkyl halide polycondensation reaction between reactant, and gel has chemical activity, can dissolve well In spinning solution.The present invention uses the porous superfine fibre of forsterite of non-hydrolytic sol-gel process combination electrostatic spinning preparation Feature are as follows: for average fibre diameter between 300 ~ 500nm, fiber surface is smooth, and diameter distribution is uniform, and fibrous inside has porous knot Structure, pore diameter range are 50 ~ 250nm.Compared with the prior art, the present invention can simplify the preparation process of forsterite fiber, reduce and close At temperature, preparation cost is reduced, the heat-proof quality of fiber improves.The porous superfine fibre of forsterite prepared by the present invention can be used as The high temperature insulating material in the fields such as space flight military project.
Specific embodiment
Embodiment 1
Using 0.29g anhydrous magnesium chloride as presoma, 0.33ml ethyl orthosilicate is oxygen donor, and 15ml anhydrous methylene chloride is Solvent prepares reaction solution, which is put into gelation in 110 DEG C of baking ovens and handles 16h, obtains forsterite xerogel.By matter It measures after percentage measures dehydrated alcohol and polyvinylpyrrolidone (PVP) mixing for 65% and 35% respectively and obtains PVP ethanol solution, The above-mentioned forsterite xerogel that mass percent is 5% is dissolved in the PVP ethanol solution that mass percent is 95% and is obtained Spinning precursor liquid.It is spinning voltage 15KV, charging rate 0.8ml/h by spinning parameter, solidification distance 15cm carries out electrostatic spinning, Needle diameter is 0.8mm, at room temperature, is prepared into forsterite xerogel/PVP composite fibre.Then by the composite fibre with 5 DEG C/heating rate of min calcines and keeps the temperature 1h at 1000 DEG C, obtaining average diameter is 500nm or so, and aperture is 100 ~ 150nm Forsterite fiber.
Embodiment 2
Using 0.29g anhydrous magnesium chloride as presoma, 0.33ml ethyl orthosilicate is oxygen donor, and 15ml anhydrous methylene chloride is Solvent prepares reaction solution, which is put into gelation in 130 DEG C of baking ovens and handles 20h, obtains forsterite xerogel.By matter It measures after percentage measures dehydrated alcohol and polyvinylpyrrolidone (PVP) mixing for 75% and 25% respectively and obtains PVP ethanol solution, The above-mentioned forsterite xerogel that mass percent is 3% is dissolved in the PVP ethanol solution that mass percent is 97% and is obtained Spinning precursor liquid.It is spinning voltage 10KV, charging rate 0.1ml/h by spinning parameter, solidification distance 5cm carries out electrostatic spinning, Needle diameter is 0.8mm, at room temperature, is prepared into forsterite xerogel/PVP composite fibre.Then by the composite fibre with 3 DEG C/heating rate of min calcines and keeps the temperature 5h at 800 DEG C, obtaining average diameter is 450nm or so, and aperture is 50 ~ 150nm's Forsterite fiber.
Embodiment 3
Using 0.15g anhydrous magnesium chloride as presoma, 0.17ml ethyl orthosilicate is oxygen donor, and 15ml anhydrous methylene chloride is Solvent prepares reaction solution, which is put into gelation processing in 130 DEG C of baking ovens and for 24 hours, obtains forsterite xerogel.By matter It measures after percentage measures dehydrated alcohol and polyvinylpyrrolidone (PVP) mixing for 80% and 20% respectively and obtains PVP ethanol solution, The above-mentioned forsterite xerogel that mass percent is 1% is dissolved in the PVP ethanol solution that mass percent is 99% and is obtained Spinning precursor liquid.It is spinning voltage 20KV, charging rate 1.5ml/h by spinning parameter, solidification distance 20cm carries out electrostatic spinning, Needle diameter is 0.8mm, at room temperature, is prepared into forsterite xerogel/PVP composite fibre.Then by the composite fibre with 3 DEG C/heating rate of min calcines and keeps the temperature 0.5h at 800 DEG C, obtaining average diameter is 300nm or so, and aperture is 50 ~ 100nm Forsterite fiber.
Embodiment 4
Using 0.15g anhydrous magnesium chloride as presoma, 0.24ml ethyl orthosilicate is oxygen donor, and 15ml anhydrous methylene chloride is Solvent prepares reaction solution, which is put into gelation processing in 110 DEG C of baking ovens and for 24 hours, obtains forsterite xerogel.By matter It measures after percentage measures dehydrated alcohol and polyvinylpyrrolidone (PVP) mixing for 85% and 15% respectively and obtains PVP ethanol solution, The above-mentioned forsterite xerogel that mass percent is 1% is dissolved in the PVP ethanol solution that mass percent is 99% and is obtained Spinning precursor liquid.It is spinning voltage 25KV, charging rate 1.0ml/h by spinning parameter, solidification distance 30cm carries out electrostatic spinning, Needle diameter is 0.8mm, at room temperature, is prepared into forsterite xerogel/PVP composite fibre.Then by the composite fibre with 3 DEG C/heating rate of min calcines and keeps the temperature 3h at 1200 DEG C, obtaining average diameter is 500nm or so, and aperture is 150 ~ 200nm Forsterite fiber.
Embodiment 5
Using 0.15g anhydrous magnesium chloride as presoma, 0.24ml ethyl orthosilicate is oxygen donor, and 15ml anhydrous methylene chloride is Solvent prepares reaction solution, which is put into gelation processing in 110 DEG C of baking ovens and for 24 hours, obtains forsterite xerogel.By matter It measures after percentage measures dehydrated alcohol and polyvinylpyrrolidone (PVP) mixing for 90% and 10% respectively and obtains PVP ethanol solution, The above-mentioned forsterite xerogel that mass percent is 2% is dissolved in the PVP ethanol solution that mass percent is 98% and is obtained Spinning precursor liquid.It is spinning voltage 15KV, charging rate 1.2ml/h by spinning parameter, solidification distance 40cm carries out electrostatic spinning, Needle diameter is 0.8mm, at room temperature, is prepared into forsterite xerogel/PVP composite fibre.Then by the composite fibre with 3 DEG C/heating rate of min calcines and keeps the temperature 4h at 1100 DEG C, obtaining average diameter is 450nm or so, and aperture is 100 ~ 200nm Forsterite fiber.
Embodiment 6
Using 0.15g anhydrous magnesium chloride as presoma, 0.24ml ethyl orthosilicate is oxygen donor, and 15ml anhydrous methylene chloride is Solvent prepares reaction solution, which is put into gelation in 120 DEG C of baking ovens and handles 20h, obtains forsterite xerogel.By matter It measures after percentage measures dehydrated alcohol and polyvinylpyrrolidone (PVP) mixing for 95% and 5% respectively and obtains PVP ethanol solution, The above-mentioned forsterite xerogel that mass percent is 1% is dissolved in the PVP ethanol solution that mass percent is 99% and is obtained Spinning precursor liquid.It is spinning voltage 15KV, charging rate 1.0ml/h by spinning parameter, solidification distance 10cm carries out electrostatic spinning, Needle diameter is 0.8mm, at room temperature, is prepared into forsterite xerogel/PVP composite fibre.Then by the composite fibre with 1 DEG C/heating rate of min calcines and keeps the temperature 2h at 1000 DEG C, obtaining average diameter is 400nm or so, and aperture is 100 ~ 200nm Forsterite fiber.
Embodiment 7
Using 0.15g anhydrous magnesium chloride as presoma, 0.24ml ethyl orthosilicate is oxygen donor, and 15ml anhydrous methylene chloride is Solvent prepares reaction solution, which is put into gelation in 120 DEG C of baking ovens and handles 16h, obtains forsterite xerogel.By matter It measures after percentage measures dehydrated alcohol and polyvinylpyrrolidone (PVP) mixing for 85% and 15% respectively and obtains PVP ethanol solution, The above-mentioned forsterite xerogel that mass percent is 1% is dissolved in the PVP ethanol solution that mass percent is 99% and is obtained Spinning precursor liquid.It is spinning voltage 15KV, charging rate 1.0ml/h by spinning parameter, solidification distance 25cm carries out electrostatic spinning, Needle diameter is 0.8mm, at room temperature, is prepared into forsterite xerogel/PVP composite fibre.Then by the composite fibre with 5h is calcined and kept the temperature to the heating rate of 10 DEG C/min at 900 DEG C, and obtaining average diameter is 450nm or so, and aperture is 150 ~ 250nm Forsterite fiber.

Claims (7)

1. a kind of method that electrostatic spinning prepares the porous superfine fibre of forsterite, it is characterised in that the preparation method packet of the fiber Include following steps: (1) by anhydrous magnesium chloride, ethyl orthosilicate and anhydrous methylene chloride by certain molar ratio reaction solution, The reaction solution is put into heated gelization in baking oven again to handle, it is solidifying that initiation non-hydrolytic sol-gel reaction synthesizes forsterite Glue;(2) dehydrated alcohol and a certain amount of polyvinylpyrrolidone (PVP) are mixed in a certain ratio and obtain PVP ethanol solution, it will The forsterite gel of synthesis is dissolved in acquisition spinning precursor liquid in PVP ethanol solution;(3) use electrostatic spinning process by spinning Precursor liquid is prepared into forsterite xerogel/PVP composite fibre;(4) by forsterite xerogel/PVP composite fibre through high temperature The porous superfine fibre of forsterite is obtained after calcining;The average fibre diameter is 300~500nm, and fibrous inside has porous knot Structure, pore diameter range are 50~250nm.
2. a kind of method that electrostatic spinning prepares the porous superfine fibre of forsterite as described in claim 1, it is characterised in that Reaction solution composition are as follows: the mass percent of anhydrous magnesium chloride is 3.5%~9.5%, and the mass percent of ethyl orthosilicate is 0.5 ~1.5%, the mass percent of methylene chloride is 90~95%.
3. a kind of method that electrostatic spinning prepares the porous superfine fibre of forsterite as described in claim 1, it is characterised in that Reaction solution heated gelization processing temperature control are as follows: heating temperature be 110~130 DEG C, gelation time be 16~for 24 hours.
4. a kind of method that electrostatic spinning prepares the porous superfine fibre of forsterite as described in claim 1, it is characterised in that PVP ethanol solution composition are as follows: the mass percent that the mass percent of dehydrated alcohol is 65~95%, PVP is 5~35%, PVP Molecular weight is 58000~1300000.
5. a kind of method that electrostatic spinning prepares the porous superfine fibre of forsterite as described in claim 1, it is characterised in that The composition of spinning precursor liquid are as follows: the mass percent of forsterite gel is that the mass percent of 1~5%, PVP ethanol solution is 95~99%.
6. a kind of method that electrostatic spinning prepares the porous superfine fibre of forsterite as described in claim 1, it is characterised in that Prepare forsterite xerogel/PVP composite fibre electrostatic spinning process parameter are as follows: 10~25kV of spinning voltage, charging rate 0.1~1.5ml/h solidifies 5~40cm of distance.
7. a kind of method that electrostatic spinning prepares the porous superfine fibre of forsterite as described in claim 1, it is characterised in that Forsterite xerogel/PVP composite fibre high-temperature calcination prepares the temperature control of the porous superfine fibre of forsterite are as follows: calcining temperature Degree is 800~1200 DEG C, and heating rate is 1~10 DEG C/min, 0.5~5h of soaking time.
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CN112044368B (en) * 2020-08-21 2023-03-10 航天特种材料及工艺技术研究所 Low-density blocky alumina composite aerogel based on non-hydrolytic sol-gel technology and preparation method thereof

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