CN106867019A - One kettle way prepares SiO2The method of cellulose composite aerogel material - Google Patents
One kettle way prepares SiO2The method of cellulose composite aerogel material Download PDFInfo
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- CN106867019A CN106867019A CN201710010005.6A CN201710010005A CN106867019A CN 106867019 A CN106867019 A CN 106867019A CN 201710010005 A CN201710010005 A CN 201710010005A CN 106867019 A CN106867019 A CN 106867019A
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- cellulose
- silicon source
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- inorganic silicon
- sio
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- 239000001913 cellulose Substances 0.000 title claims abstract description 104
- 229920002678 cellulose Polymers 0.000 title claims abstract description 103
- 239000004964 aerogel Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 title claims abstract description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 95
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 53
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 35
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 32
- 239000010703 silicon Substances 0.000 claims abstract description 32
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 31
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 31
- 239000011240 wet gel Substances 0.000 claims abstract description 24
- 239000007864 aqueous solution Substances 0.000 claims abstract description 22
- 235000019795 sodium metasilicate Nutrition 0.000 claims abstract description 21
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 16
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 16
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 13
- PTHCMJGKKRQCBF-UHFFFAOYSA-N Cellulose, microcrystalline Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC)C(CO)O1 PTHCMJGKKRQCBF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 235000010980 cellulose Nutrition 0.000 claims description 73
- 239000000243 solution Substances 0.000 claims description 45
- 239000000835 fiber Substances 0.000 claims description 39
- 235000012239 silicon dioxide Nutrition 0.000 claims description 29
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 15
- 239000004202 carbamide Substances 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 13
- 239000003513 alkali Substances 0.000 claims description 13
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 230000032683 aging Effects 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 9
- 230000001112 coagulating effect Effects 0.000 claims description 7
- 239000000499 gel Substances 0.000 claims description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 6
- 229920000742 Cotton Polymers 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- 229920003043 Cellulose fiber Polymers 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 235000019353 potassium silicate Nutrition 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- 241000218691 Cupressaceae Species 0.000 claims description 3
- 229920000875 Dissolving pulp Polymers 0.000 claims description 3
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 3
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 3
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 3
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- KEZYHIPQRGTUDU-UHFFFAOYSA-N 2-[dithiocarboxy(methyl)amino]acetic acid Chemical compound SC(=S)N(C)CC(O)=O KEZYHIPQRGTUDU-UHFFFAOYSA-N 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 235000011194 food seasoning agent Nutrition 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000001802 infusion Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- ORVGYTXFUWTWDM-UHFFFAOYSA-N silicic acid;sodium Chemical compound [Na].O[Si](O)(O)O ORVGYTXFUWTWDM-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000352 supercritical drying Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 230000000536 complexating effect Effects 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 230000001939 inductive effect Effects 0.000 abstract 1
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract 1
- 239000012774 insulation material Substances 0.000 abstract 1
- 239000011707 mineral Substances 0.000 abstract 1
- 150000007522 mineralic acids Chemical class 0.000 abstract 1
- 239000004627 regenerated cellulose Substances 0.000 abstract 1
- 239000011734 sodium Substances 0.000 description 13
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 9
- 229910052708 sodium Inorganic materials 0.000 description 9
- 206010001497 Agitation Diseases 0.000 description 7
- 238000013019 agitation Methods 0.000 description 7
- 238000006073 displacement reaction Methods 0.000 description 6
- 239000000017 hydrogel Substances 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 229910020489 SiO3 Inorganic materials 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000005191 phase separation Methods 0.000 description 3
- SJRXVLUZMMDCNG-UHFFFAOYSA-N Gossypin Natural products OC1C(O)C(O)C(CO)OC1OC1=C(O)C=C(O)C2=C1OC(C=1C=C(O)C(O)=CC=1)=C(O)C2=O SJRXVLUZMMDCNG-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- SJRXVLUZMMDCNG-KKPQBLLMSA-N gossypin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=C(O)C=C(O)C2=C1OC(C=1C=C(O)C(O)=CC=1)=C(O)C2=O SJRXVLUZMMDCNG-KKPQBLLMSA-N 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000009738 saturating Methods 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000012453 solvate Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/05—Elimination by evaporation or heat degradation of a liquid phase
- C08J2201/0502—Elimination by evaporation or heat degradation of a liquid phase the liquid phase being organic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
Abstract
SiO is prepared the present invention relates to a kind of one kettle way2The method of cellulose composite aerogel material, with cellulose as raw material, green alkalinuria solvent dissolves cellulose；With inorganic silicic acid sodium as silicon source, cellulose is obtained by dispersed with stirring and sodium metasilicate uniformly mixes aqueous solution, the regenerated cellulose wet gel containing silicon source is obtained with reference to sol-gal process；It is reaction dissolvent inductive formation SiO with inorganic acid with cellulose gel as skeleton2, finally by CO2Supercritical drying process system is dried to obtain SiO2Cellulose organo-mineral complexing aeroge.Present invention process simple and fast, feasibility be high and environmental protection, effectively overcomes SiO in infusion process in situ2In cellulose porous network structure the problems such as bad dispersibility, low compound content and poor stable composition, prepared Inorganic whisker aeroge has relatively low thermal conductivity factor, good heat-proof quality, is had a good application prospect in terms of low temperature cold insulation material, middle low temperature heat-insulating heat-preserving material and sorbing material.
Description
Technical field
The invention belongs to high molecular nanometer functional material preparation field, it is related to a kind of one kettle way to prepare SiO2- cellulose is multiple
The method for closing aerogel material.
Background technology
Cellulose aerogels are the class new type natural biomass new materials for growing up in recent years.Cellulose is the earth
The maximum green renewable resource of upper reserves, cellulose aerogels have renewable natural polymer sub-feature and traditional high porosity concurrently
The plurality of advantages of nano inorganic porous material, relative to intensity difference, frangible silica aerogel, with spies such as good toughness, easy processings
Property, therefore cellulose aerogels turn into the new material that a class has a extensive future, Development volue is high, in the branch of Drug controlled release
The electrode material great potential of carbon battery and fuel cell when frame, gas absorbent, heat-barrier material and pyrolysis.
Cellulose aerogels possess many good characteristics, but the polysaccharide aeroge limitation of itself, such as stability be poor, resistance
The features such as combustion property difference, limits its development to a certain extent.Traditional Si O2Although aeroge function admirable, fragility is
It is difficult to overcome.And cellulose-SiO2The characteristics of composite aerogel not only possesses two kinds of aeroges, also show many new excellent
Performance.
Conventional SiO2- cellulose composite aerogel is typically moist cellulose film immersion to tetraethyl orthosilicate/positive silicic acid first
In ester, aerosil is formed in the micropore of cellulose matrix, then in supercritical CO2Middle drying etc., but the method
Silica can be caused in the rapid gel in outer surface of cellulose, so as to block aperture and hinder silica infiltration
To in cellulose matrix, porosity occurs to be badly in need of declining.But directly directly mix cellulose solution and tetraethyl orthosilicate
Method is again inadvisable, and alfali-soluble fibre element solution is metastable state system, and direct and hydrolyzed silane solution can cause cellulose to solidify immediately
It is separated with Ludox.
Aqueous silicic acid sodium is a kind of basic silicate, the pH about 14 of saturated solution；Same pH is 14 alfali-soluble fibre element
Aqueous solution sodium silicate aqueous solution is directly mixed as starting soln, using one kettle way can form uniform and stable mixed solution,
Cellulose self-association of cellulose chain in alcohol bath can cause gelation to generate II fiber type element gel, and sodium silicate solution is dispersed in
In cellulose network structure, then the cellulose of solidification is placed in when in acid rinse bath, sodium metasilicate can be converted into SiO2。
The content of the invention
The purpose of the present invention is directed to existing SiO2Limitation in-cellulose composite aerogel preparation process and one kind is provided
Pot method prepares SiO2The method of-cellulose composite aerogel material, the method is feasible, simple, by using one kettle way, directly will
Inorganic silicon source evenly spread in cellulose gel three-dimensional net structure, it is to avoid duct blocks to be occurred with the phenomenon being separated,
Also can to a certain degree improve SiO simultaneously2The mechanical performance and effect of heat insulation of-cellulose aerogels.
The technical scheme is that：One kettle way prepares SiO2The method of-cellulose composite aerogel material, its specific step
It is rapid as follows：
(1) configuration of cellulose solution
Cellulose fibre is distributed under stirring in alkali urea mixed aqueous solution, is cooled to -20~-5 DEG C after sealing in advance,
Thick solution is obtained with electric blender stirring and dissolving cellulose after taking-up, bubble is then centrifuged off and is obtained clear
Cellulose solution；Wherein the mass fraction of cellulose, alkali, urea and deionized water is respectively (2% -6%) in cellulose solution,
(4%-20%), (10%-20%), (54%-84%)；
(2) configuration of inorganic silicon source-cellulose mixed solution
Inorganic silicon source is dissolved in stirring action, the inorganic silicon source aqueous solution that mass fraction is 1%-7% is obtained；By cellulose
The aqueous solution and inorganic silicon source aqueous solution volume ratio are 1：(0.1-1), the inorganic silicon source aqueous solution is added in cellulose aqueous solution,
After stirring mixing, sonic oscillation removes bubble, forms mixed uniformly inorganic silicon source-cellulose mixed solution；
(3) containing the preparation of inorganic silicon source-cellulose wet gel
Mixed uniformly inorganic silicon source-cellulose mixed solution is poured into mould to be placed in coagulating bath and is regenerated, stood
To the cellulose wet gel containing inorganic silicon source；
(4) preparation of silicon dioxide fiber element wet gel
Cellulose wet gel containing inorganic silicon source is transferred in dilute acid soln, in cellulose gel after it there is neutralization reaction
Inorganic silicon source is induced to form silica in glue hole；
(5) preparation of composite aerogel
It is 6-8 by the pH that silicon dioxide fiber element wet gel distilled water rinses solution processed；Again by silicon dioxide fiber
Hydrogel be transferred to organic solvent carry out solvent put with it is aging obtain silicon dioxide fiber element alcogel；After be transferred to CO2It is super
Treatment is dried in critical drying device, silicon dioxide fiber element composite aerogel is finally given.
Cellulose fibre described in preferred steps (1) is the one kind in cotton pulp cypress, cotton of short staple or microcrystalline cellulose；It is described
Alkali urea mixed aqueous solution in alkali be the one kind in NaOH or lithium hydroxide；Urea is urea or thiocarbamide.
The rotating speed of electric blender is 1000-2000rpm in preferred steps (1), and mixing time is 4-12min；Centrifuge
Rotating speed be 8000-10000rpm, centrifugation time is 5-10min.
Inorganic silicon source described in preferred steps (2) is SODIUM METASILICATE PENTAHYDRATE powder, nine water sodium metasilicate powder, anhydrous sodium metasilicate or
Alkaline waterglass.
Coagulating bath described in preferred steps (3) is methyl alcohol, ethanol, acetone or dilute sulfuric acid.During standing in preferred steps (3)
Between 5-360min.
Dilute acid soln described in preferred steps (4) is hydrochloric acid, nitric acid, sulfuric acid or aqueous acetic acid；The concentration of dilute acid soln
It is 0.5-1mol/L.
Organic solvent described in preferred steps (5) is the one kind or its mixed liquor in methyl alcohol, ethanol or acetone.
CO 2 supercritical seasoning described in preferred steps (5) with carbon dioxide as dried medium, reaction temperature
It it is 40-70 DEG C, pressure is 8~12MPa in autoclave, drying time is 10~20h.
The apparent density 0.092 of silicon dioxide fiber element composite aerogel prepared in preferred steps (5)~
0.143g/cm3, 227.41~264.93m of specific surface area2/ g, bulk thermal conductivity constants are between 0.029~0.038W/mK.
Beneficial effect：
The inventive method and Organic-inorganic composite SiO is obtained as prepared by the one kettle way2- cellulose aerogels material
With following features：
(1) process is simple is effective.This preparation method overcomes SiO in infusion process preparation method2- cellulose aerogels material
Problem of phase separation during material in duct blockage problem and organic silicon source and alfali-soluble fibre element solution.Ludox is logical in infusion process
Cross penetrate into three-dimensional fiber element matrix in realize filling a vacancy porous cellulose gel.This technique has certain limitation, because
For it is a diffusion process, so silica skewness in cellulose matrix, the shadow for easily being prepared by cellulose gel
Ring, and time needed for dipping process is very long.And directly mix organic silicon source and alfali-soluble fibre the element aqueous solution due to and alkali soluble is fine
The plain non-real dissolving of the aqueous solution of dimension, and be in metastable state dissolution system, after adding organic silicon source, it may occur that organic silicon source it is strong
Hydrolysis, water is fought for cellulose so that the hydrogen bond between cellulosic molecule with intramolecular is exposed, so that it is quick that cellulose occurs
Gel and phase separation.And select the sodium metasilicate for being all alkalescence to be mixed directly into as silicon source, after dissolving in alkaline hydrolysis cellulose solution
Metastable state dissolution system will not be destroyed, while also inhibits the appearance of phase separation, well mixed stablizing solution can be formed.Alcohol
After bath gel, under the action of an acid so that sodium metasilicate is converted to the direction of production silica and sodium salt, finally by overcritical
It is dried to obtain SiO2- cellulose composite aerogel.
(2) the cheap wide material sources of the prices of raw materials, the cellulose mainly selected and sodium metasilicate (waterglass) are inexpensively
The industrial raw materials being easy to get, greatly reduce manufacturing cost, it is easy to accomplish large-scale production.And have green ring well concurrently
Protect effect.The cellulose dissolution system of all selections simultaneously is dissolved for green, it is only necessary to which the material such as NaOH and urea just can
Realized to cellulose dissolution in low temperature environment, it is easy and effective.
(3) relative to other aerogel heat-insulating materials, using SiO prepared by one pot of mixing method2- cellulose is combined airsetting
Glue, is generation masterplate with the three-dimensional net structure of cellulose gel, and sodium metasilicate is filled in the hole of cellulose, in acid solution
Catalytic action under generate SiO2Particle, SiO2Condense for larger spheric granules forms the nanometer that agglomerate is attached to cellulose
On fibril, it is to avoid free SiO2Particle occurs, and prepared material surface is smooth, and thickness is controllable, and formability is preferably, prepared
SiO2The microscopic appearance of-cellulose composite aerogel is as shown in scanning electron microscope (SEM) photograph.And prepared SiO2- cellulose is combined gas
Gel still possesses high porosity and than more uniform pore passage structure.
Brief description of the drawings
Fig. 1 is SiO prepared by example 12The sample drawing of-cellulose composite aerogel material；
Fig. 2 is SiO prepared by example 22The X-ray diffraction spectrogram of-cellulose composite aerogel material；
Fig. 3 is SiO prepared by example 22The scanning electron microscopic picture of-cellulose composite aerogel material；
Fig. 4 is SiO prepared by example 32Nitrogen adsorption-the desorption curve of-cellulose composite aerogel.
Specific embodiment
Example 1
1. by the microcrystalline cellulose dispersed with stirring of 2g to alkali urea solution (4.0gLiOH/10gUrea/84gH2O in), dispersion
After be transferred to refrigerator and be cooler than -5 DEG C in advance, stir 4min dissolving fibers under conditions of 2000rpm using motor immediately after taking-up
Element obtains thick solution, 10min removing bubbles is immediately centrifuged under conditions of rotating speed is 8000rpm and obtains clear
Cellulose solution, solvent quality fraction be 2%；Weigh the Na of 16.3g2SiO3·9H2O magnetic agitations are dissolved into 83.7g distillations
The sodium silicate aqueous solution that mass fraction is 7% is obtained in water, is by volume 10 by cellulose solution and sodium silicate solution：1 enters
Row mechanical agitation mixes, and rear sonic oscillation removes bubble, forms mixed uniformly sodium metasilicate-cellulose mixed solution.Again will be equal
Sodium metasilicate-the cellulose mixed solution of even mixing is poured into the middle of mould to be placed in methyl alcohol coagulating bath and regenerated, and is obtained after standing 360min
To the cellulose wet gel containing sodium metasilicate.After ageing, then body will be transferred to after the cellulose wet gel stripping containing sodium metasilicate
Product is 200ML concentration in 0.5mol/L dilution heat of sulfuric acid, silicic acid to be induced in cellulose gel hole after it there is neutralization reaction
Sodium generates silica, then the compound wet gel of silicon dioxide fiber element is spent into acid and generation that distilled water rinsing removing is more than
Salt, now the pH of solution be 7.Silicon dioxide fiber hydrogel is transferred into alcohol solvent again carries out solvent displacement and old
Change, replace 8 times altogether, finally give silicon dioxide fiber element alcogel, silicon dioxide fiber element alcogel is placed in CO2It is super
It is dried treatment in critical drying device, drying temperature is 40 DEG C, pressure is 8MPa in autoclave, drying time is
20h.By supercritical CO2Dry, form organic and inorganic SiO2- cellulose aerogels.The density is 0.092/cm3, specific surface
Product is 227.41m2/ g, bulk thermal conductivity constants 0.032W/mK.Accompanying drawing 1 is prepared SiO in example 12- cellulose is combined airsetting
The sample drawing of glue material.As can be seen that milky of the composite aerogel as pure cellulose aerogels presentation, material in figure
Surfacing, in the absence of the situation of dry linting, also with good mechanical strength.
Example 2
By the cotton pulp cypress cellulose dispersed with stirring of 6g to alkali urea solution (4gLiOH/10gThiourea/80gH2O in), point
Refrigerator being transferred to after dissipating and being cooler than -20 DEG C in advance, 4min is stirred under conditions of 2000rpm using motor immediately after taking-up dissolves fine
Dimension element obtains thick solution, 5min removing bubbles is immediately centrifuged under conditions of rotating speed is 10000rpm and obtains clarifying saturating
Bright cellulose solution, solvent quality fraction is 6%；Weigh the Na of 1.74g2SiO3·5H2O magnetic agitations are dissolved into 98.3g steamings
The sodium silicate aqueous solution that mass fraction is 1% is obtained in distilled water, is by volume 1 by cellulose solution and sodium silicate solution：1 enters
Row mechanical agitation mixes, and sonic oscillation removes bubble, forms mixed uniformly sodium metasilicate-cellulose mixed solution.Again will be uniform
Sodium metasilicate-the cellulose mixed solution of mixing is poured into the middle of mould to be placed in alcohol solidification bath and regenerated, and is contained after standing 60min
There is the cellulose wet gel of sodium metasilicate.After ageing, then by volume is transferred to after the cellulose wet gel stripping containing sodium metasilicate it is
100ML concentration is in 1mol/L dilute hydrochloric acid solutions, induction sodium metasilicate is generated in cellulose gel hole after it there is neutralization reaction
Silica, then the compound wet gel of silicon dioxide fiber element is spent into the salt that distilled water rinsing removes the acid and generation being more than, this
When wash solution pH be 7.Again by silicon dioxide fiber hydrogel be transferred to methanol solvate carry out solvent displacement and it is aging,
Replace 5 times altogether, finally give silicon dioxide fiber element alcogel, silicon dioxide fiber element alcogel is placed in CO2It is super to face
Treatment is dried in boundary's drying device, drying temperature is 40 DEG C, and pressure is 8MPa in autoclave, and drying time is 20h.
By supercritical CO2Dry, form organic and inorganic SiO2- cellulose aerogels.The density is 0.143/cm3, specific surface area is
243.46m2/ g, bulk thermal conductivity constants 0.032W/mK.Fig. 2 is SiO2The scanning electron microscopic picture of-cellulose composite aerogel material,
SiO2It is the agglomerate of larger spheric granules to condense, and is attached in the middle of the three-dimensional net structure of cellulose gel (as figure is got the bid
Shown in note), SiO2It is formed among the pore passage structure of cellulose, not free SiO2Particle occurs.Fig. 3 is SiO2- fine
The plain composite aerogel section energy spectrum diagram of dimension, EDS energy spectrum analysis display Si peaks are probably located in 1.73KeV, and Na peaks are 1.04KeV,
Mainly due to SiO2The sodium salt that generation conversion process is produced.
Example 3
By the short flannel gossypin dispersed with stirring of 3g to alkali urea solution (wherein 4.6gNaOH/15gUrea/77.4gH2O)
In, refrigerator is transferred to after dispersion and is cooler than -15 DEG C in advance, 12min is stirred under conditions of 1000rpm using motor immediately after taking-up
Dissolving cellulose obtains thick solution, 10min removing bubbles is immediately centrifuged under conditions of rotating speed is 8000rpm and obtains
The cellulose solution of clear, solvent quality fraction is about 3% or so；Weigh the anhydrous Na of 3g2SiO3Magnetic agitation is dissolved into
In 97ml distilled water, the sodium silicate aqueous solution that mass fraction is 3% is obtained, by cellulose solution and sodium silicate solution by volume
It is 2：1 carries out the stirring mixing of mechanical mixer agitation tool, and sonic oscillation removes bubble, forms mixed uniformly sodium metasilicate-fiber
Plain mixed solution.Mixed uniformly sodium metasilicate-cellulose mixed solution is poured into the middle of mould is again placed in acetone coagulating bath again
It is raw, obtain the cellulose wet gel containing sodium metasilicate after standing 5min.After ageing, then by the cellulose wet gel containing sodium metasilicate
Be transferred to after wet gel stripping volume for 200ML concentration be lmol/L dilute nitric acid solutions in, occur neutralization reaction after in fiber
Induction sodium metasilicate generation silica in plain gel pore, then the compound wet gel of silicon dioxide fiber element is spent into distilled water rinsing
Acid and the salt of generation that removing is more than, the pH of wash solution is 6.Silicon dioxide fiber hydrogel is transferred to acetone again molten
Agent carries out solvent displacement and aging, displacement 10 times altogether, silicon dioxide fiber element alcogel is finally given, by silica-fibre
The plain alcogel of dimension is placed in CO2Treatment is dried in supercritical drying device, drying temperature is 70 DEG C, pressure in autoclave
It is 12MPa, drying time is 10h.By supercritical CO2Dry, form organic and inorganic SiO2- cellulose aerogels.The density
It is 0.109g/cm3, specific surface area is 264.93m2/ g, bulk thermal conductivity constants 0.029W/mK.Fig. 4 is prepared SiO2- fiber
Nitrogen adsorption-the desorption curve of plain composite aerogel, belongs to the IV types in IUPAC classification, meets the intrinsic essence of porous material special
Levy.
Example 4
By the short flannel gossypin dispersed with stirring of 6g to alkali urea solution (wherein 20gNaOH/20gUrea/54gH2O in), point
Refrigerator being transferred to after dissipating and being cooler than -15 DEG C in advance, 5min is stirred under conditions of 1000rpm using motor immediately after taking-up dissolves fine
Dimension element obtains thick solution, 5min removing bubbles is immediately centrifuged under conditions of rotating speed is 8000rpm and obtains clarifying saturating
Bright cellulose solution, solvent quality fraction is about 3% or so；The alkaline water glass magnetic force stirring and dissolving for weighing 3g is steamed to 97g
In distilled water, the sodium silicate aqueous solution that mass fraction is about 3% is obtained, be by volume 1 by cellulose solution and sodium silicate solution：
After the mixing of 1 mechanical agitation, sonic oscillation removes bubble, forms mixed uniformly sodium metasilicate-cellulose mixed solution.Again will be uniform
Sodium metasilicate-the cellulose mixed solution of mixing is poured into the middle of mould to be placed in dilute sulfuric acid coagulating bath and regenerated, and is obtained after standing 5min
Cellulose wet gel containing sodium metasilicate.After ageing, then volume will be transferred to after the cellulose wet gel stripping containing sodium metasilicate
Be 200ML concentration be lmol/L dilute acetic acid solutions in, occur neutralization reaction after in cellulose gel hole induce sodium metasilicate life
Into silica, then the compound wet gel of silicon dioxide fiber element is spent into the salt that distilled water rinsing removes the acid and generation being more than,
The pH of wash solution is 8.Again by silicon dioxide fiber hydrogel be transferred to alcohol solvent carry out solvent displacement and it is aging, altogether
Meter displacement 7 times, finally gives silicon dioxide fiber element alcogel, and silicon dioxide fiber element alcogel is placed in into CO2It is overcritical
Treatment is dried in drying device, drying temperature is 40 DEG C, and pressure is 8MPa in autoclave, and drying time is 20h.Through
Cross supercritical CO2Dry, form organic and inorganic SiO2- cellulose aerogels.The density is 0.128/cm3, specific surface area is
238.56m2/ g, bulk thermal conductivity constants 0.033W/mK.
Claims (10)
1. one kettle way prepares SiO2The method of-cellulose composite aerogel material, it is comprised the following steps that：
(1) configuration of cellulose solution
Cellulose fibre is distributed under stirring in alkali urea mixed aqueous solution, is cooled to -20~-5 DEG C after sealing in advance, taken out
Thick solution is obtained with electric blender stirring and dissolving cellulose afterwards, the fiber that bubble obtains clear is then centrifuged off
Plain solution；Wherein the mass fraction of cellulose, alkali, urea and deionized water is respectively (2% -6%) in cellulose solution, (4%-
20%), (10%-20%), (54%-84%)；
(2) configuration of inorganic silicon source-cellulose mixed solution
Inorganic silicon source is dissolved in stirring action, the inorganic silicon source aqueous solution that mass fraction is 1%-7% is obtained；It is water-soluble by cellulose
Liquid and inorganic silicon source aqueous solution volume ratio are 1：(0.1-1), the inorganic silicon source aqueous solution is added in cellulose aqueous solution, stirring
After mixing, sonic oscillation removes bubble, forms mixed uniformly inorganic silicon source-cellulose mixed solution；
(3) containing the preparation of inorganic silicon source-cellulose wet gel
Mixed uniformly inorganic silicon source-cellulose mixed solution is poured into mould to be placed in coagulating bath and is regenerated, standing is contained
There is the cellulose wet gel of inorganic silicon source；
(4) preparation of silicon dioxide fiber element wet gel
Cellulose wet gel containing inorganic silicon source is transferred in dilute acid soln, in cellulose gel hole after it there is neutralization reaction
The interior inorganic silicon source of induction forms silica；
(5) preparation of composite aerogel
It is 6-8 by the pH that silicon dioxide fiber element wet gel distilled water rinses solution processed；Again by silicon dioxide fiber element water
Gel be transferred to organic solvent carry out solvent put with it is aging obtain silicon dioxide fiber element alcogel；After be transferred to CO2It is overcritical
Treatment is dried in drying device, silicon dioxide fiber element composite aerogel is finally given.
2. method according to claim 1, it is characterised in that the cellulose fibre described in step (1) is cotton pulp cypress, short
One kind in suede cotton or microcrystalline cellulose；Alkali in described alkali urea mixed aqueous solution is in NaOH or lithium hydroxide
Kind；Urea is urea or thiocarbamide.
3. method according to claim 1, it is characterised in that the rotating speed of electric blender is 1000- in step (1)
2000rpm, mixing time is 4-12min；The rotating speed of centrifuge is 8000-10000rpm, and centrifugation time is 5-10min.
4. method according to claim 1, it is characterised in that the inorganic silicon source described in step (2) is SODIUM METASILICATE PENTAHYDRATE powder
End, nine water sodium metasilicate powder, anhydrous sodium metasilicate or alkaline waterglass.
5. method according to claim 1, it is characterised in that the coagulating bath described in step (3) is methyl alcohol, ethanol, acetone or
Dilute sulfuric acid.
6. method according to claim 1, it is characterised in that the time of repose 5-360min in step (3).
7. method according to claim 1, it is characterised in that the dilute acid soln described in step (4) is hydrochloric acid, nitric acid, sulfuric acid
Or aqueous acetic acid；The concentration of dilute acid soln is 0.5-1mol/L.
8. method according to claim 1, it is characterised in that the organic solvent described in step (5) is methyl alcohol, ethanol or
One kind or its mixed liquor in acetone.
9. method according to claim 1, it is characterised in that CO 2 supercritical seasoning described in step (5) with
Carbon dioxide is dried medium, and reaction temperature is 40-70 DEG C, and pressure is 8~12MPa in autoclave, and drying time is 10
~20h.
10. method according to claim 1, it is characterised in that silicon dioxide fiber element prepared in step (5) is compound
0.092~the 0.143g/cm of apparent density of aeroge3, 227.41~264.93m of specific surface area2/ g, bulk thermal conductivity constants between
0.029~0.038W/mK.
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