CN105698488A - Normal-pressure drying method of non-woven fabric/aluminum silicon aerogel composite heat preserving board - Google Patents

Normal-pressure drying method of non-woven fabric/aluminum silicon aerogel composite heat preserving board Download PDF

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Publication number
CN105698488A
CN105698488A CN201610065564.2A CN201610065564A CN105698488A CN 105698488 A CN105698488 A CN 105698488A CN 201610065564 A CN201610065564 A CN 201610065564A CN 105698488 A CN105698488 A CN 105698488A
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woven fabrics
silicon
constant pressure
aluminium aerogel
aerogel composite
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Inventor
杨卓舒
纪勇
孟宪娴
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Zhuoda New Material Technology Group Co Ltd
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Zhuoda New Material Technology Group Co Ltd
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Priority to CN201610065564.2A priority Critical patent/CN105698488A/en
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26DRYING
    • F26BDRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00Drying solid materials or objects by processes involving the application of heat
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/20Silicates
    • C01B33/32Alkali metal silicates
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece

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

Abstract

The invention provides a normal-pressure drying method of a non-woven fabric/aluminum silicon aerogel composite heat preserving board. At first, non-woven fabric/aluminum silicon wet gel is subjected to solvent replacement and hydrophobic modification, and then the wet gel subjected to hydrophobic modification is dried under normal pressure at a low temperature ranging from 80 DEG C to120 DEG C and then dried for 40 minutes at a high temperature ranging from 300 DEG C to 400 DEG C. A product produced through the normal-pressure drying method is provided, the product yield is high, the production efficiency is high, powder falls from the product slightly, and the product can be popularized industrially. The normal-pressure drying method can be integrated to an assembly line, the whole preparing method is simple and easy to operate, corrosion of strong acid and strong base is avoided, the requirement for equipment is low, and after being popularized, the method is suitable for industrialized production.

Description

A kind of constant pressure and dry method of non-woven fabrics/silicon-aluminium aerogel composite insulation boards
Technical field
The present invention relates to the drying means of a kind of warming plate, be specifically related to the constant pressure and dry method of a kind of non-woven fabrics/silicon-aluminium aerogel composite insulation boards。
Background technology
Aeroge is the material that in solid matter, heat conductivity is minimum, is only slightly higher than vacuum, is approximately 0.013W/m K。Aeroge also has extremely low density, is the minimum solid of the density generally acknowledged in the world, and least density can accomplish 3kg/m3, more slightly higher than the density of air。Therefore aeroge is the insulation material that heat insulation effect is best in the world, density is minimum。
The kind of current aeroge is more, has carbon aerogels, silicon system aeroge, alumina aerogels etc.。The preparing raw material and can adopt tetraethyl orthosilicate or waterglass of silica aerogel, preparation technology can be respectively adopted non-pressure process and supercritical, and its preparation technology is highly developed。The preparation of alumina aerogels, mainly alkoxide process, drying process adopts supercritical process substantially。And the preparation of silica/alumina composite aerogel, rarely having report, even if being prepared into pluralgel, being also adopt alkoxide process to carry out gel。
Inorganic salt method prepares the method for sial composite aerogel, rarely has report, and at present major part aeroge composition is one pack system, for instance silica aerogel is mainly silicon dioxide, aluminum aeroge be mainly composed of aluminium oxide。The raw material of silica aerogel has two kinds, and one is tetraethyl orthosilicate, and one is waterglass, and two kinds of raw materials have different sol gel processings。The raw material major part that alumina aerogels adopts is aluminium-alcohol salt, adopts supercritical process。Therefore, the raw material production cost that tradition prepares alumina aerogels is expensive, and gel process is complicated;If what traditional alumina aerogels preparation adopted is tetraethyl orthosilicate, sol-gel process is also intended to the hydrolysis through raw material and polycondensation, and preparation technology is more complicated。
Inorganic salt method, is adopt two kinds of inorganic salts, according to certain processing compound, as long as according to certain dispensing order, it is possible to easily preparation quality and the good gel of condition。Production process is simple, and former material is cheap, has the prospect that Large scale processes is applied。
Summary of the invention
Simple in order to obtain preparation technology, the composite aerogel that cost is low, it is good and have the constant pressure and dry method of non-woven fabrics/silicon-aluminium aerogel composite insulation boards of some strength that the present invention proposes globality。
In order to achieve the above object, the invention provides employing following technical proposals:
A kind of constant pressure and dry method of non-woven fabrics/silicon-aluminium aerogel composite insulation boards, first non-woven fabrics/sial wet gel is carried out solvent displacement and hydrophobically modified, then wet gel good for hydrophobically modified is carried out at low temperature 80~120 DEG C constant pressure and dry, then dries 40 minutes at high temperature 300~400 DEG C。
First preferred version of the constant pressure and dry method of a kind of non-woven fabrics/silicon-aluminium aerogel composite insulation boards, prepares non-woven fabrics/silicon-aluminium aerogel and comprises the following steps:
(1) preparation sodium metaaluminate aqueous solution;
(2) prepare sial complex sol: under stirring, add in water glass solution preparation in step (1) sodium aluminate solution, stirring mixing 1~2min obtains forerunner's mixed solution;
(3) non-woven fabrics is completely immersed in forerunner's mixed solution, adsorbs full, stand 30min, automatic gel, the sial compound wet gel that the non-woven fabrics obtained strengthens, at room temperature aging 12h;
(4) carrying out solvent displacement, the sial compound wet gel that non-woven fabrics step (3) obtained strengthens immerses alcoholic solution, and through insulation, solvent is replaced, modified, namely obtains non-woven fabrics after drying and strengthens silicon-aluminium aerogel warming plate。
A kind of second preferred version of the constant pressure and dry method of non-woven fabrics/silicon-aluminium aerogel composite insulation boards, the preparation method of waterglass is as follows:
1) magnetic bead in magnetic separation separation of fine coal ash;
2) mechanical grinding;
3) acidleach: at 150 DEG C~220 DEG C, mixes flyash with the sulphuric acid that concentration is 80%~98% with the ratio that solid-to-liquid ratio is 2:1~1:1 of sulphuric acid in flyash, reacts 4~6h;
4) solid-liquid separation: after reactant is cooled to room temperature, it is that 1:2~1:6 preparation adds water by the solid-to-liquid ratio of flyash Yu water, at 75~95 DEG C, after stirring 1~3h, sucking filtration, the filter cake water washing that solid-to-liquid ratio is 2:1~1:2 by flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue;
5) acid leaching residue prepares waterglass: by acid leaching residue and 9%~12% soda lye by the proportions mixed liquor that solid-to-liquid ratio is 1:1~1:2, heat after 6~10h in reactor at 160~200 DEG C, be cooled to room temperature, filter and wash solid slag with water。
3rd preferred version of the constant pressure and dry method of a kind of non-woven fabrics/silicon-aluminium aerogel composite insulation boards, the light transmittance of sial compound wet gel is more than 80%。
A kind of 4th preferred version of the constant pressure and dry method of non-woven fabrics/silicon-aluminium aerogel composite insulation boards, non-woven fabrics is by flaxen fiber, terylene chemical fibre is, chinlon chemical fibre and viscose fibre prepare, and described non-woven fabrics is 50~70% in the mass content of the silicon-aluminium aerogel that described non-woven fabrics strengthens。
5th preferred version of the constant pressure and dry method of a kind of non-woven fabrics/silicon-aluminium aerogel composite insulation boards, solvent displacement adopts ethanol, and hexane equal solvent, described holding temperature is 50~70 DEG C, and described solvent time swap is more than 8 hours。
6th preferred version of the constant pressure and dry method of a kind of non-woven fabrics/silicon-aluminium aerogel composite insulation boards, modified raw material adopts siloxanyl modified liquid, and modification temperature is 50~70 DEG C, and modification time is 7~9h。
7th preferred version of the constant pressure and dry method of a kind of non-woven fabrics/silicon-aluminium aerogel composite insulation boards, it is 0.015~0.022W/ (m K) that non-woven fabrics strengthens the heat conductivity of silicon-aluminium aerogel warming plate, and density is 220~450kg/m3, water absorption rate is less than 3%。
8th preferred version of the constant pressure and dry method of a kind of non-woven fabrics/silicon-aluminium aerogel composite insulation boards, it is the fire prevention of A level that non-woven fabrics strengthens silicon-aluminium aerogel warming plate, and refractory temperature is higher than 650 DEG C。
Compared with immediate prior art, technical scheme provided by the invention has following excellent effect:
1. the invention provides the simple process of a kind of supercritical drying drying method using two kinds of alkaline, inorganic salts to prepare non-woven fabrics enhancing sial composite aerogel;
2. the invention provides the product that supercritical drying drying method produces, product yield is high, and production efficiency is high, and product dry linting is slight, it is possible to carry out industrialization amplification;
3. supercritical drying drying method can be integrated to streamline, it is simple to industrialized production;
4. the raw material of the present invention is sodium metaaluminate, waterglass and non-woven fabrics, and raw materials for production are cheap;
5. the gel method of the present invention be carry out mixture by two kinds of materials after, carry out gel reaction, it is to avoid the complicated approach of other aeroge collosol and gel;
6. whole preparation method is simple and easy to control, corrodes without strong acid and strong base, low for equipment requirements, after method is amplified, is suitable for industrialized production。
Detailed description of the invention
It is described in further detail below in conjunction with specific embodiment, technical scheme is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments。Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention。
Inorganic salt method prepares the process of sial composite aerogel:
First configuring the sodium aluminate solution of certain mass concentration, stirring, until sodium metaaluminate complete hydrolysis;Then, by the requirement of waterglass dilution technique proportioning;When stirring, in the water glass solution after diluted, add the sodium aluminate solution of required amount, after continuing stirring 1~2min, it is ensured that when solution mix homogeneously, stop stirring, stand 5~30min, obtain forerunner's mixed solution。
Non-woven fabrics is completely immersed in forerunner's mixed solution, adsorbs full, stand 30min, automatic gel, the sial compound wet gel that the non-woven fabrics obtained strengthens, at room temperature aging 12h;Then, carry out solvent displacement, the sial compound wet gel that the non-woven fabrics obtained strengthens is immersed alcoholic solution。After solvent has been replaced, adopting siloxanyl modified liquid to be modified, modification temperature is 50~70 DEG C, and modification time is 7~9h。Finally, wet gel good for hydrophobically modified is carried out at low temperature 80~120 DEG C constant pressure and dry, then dries 40 minutes at high temperature 300~400 DEG C, the sial composite aerogel granule that felt strengthens must be stung。
The sodium aluminate solution of configuration, it is necessary to all dissolve, it is not possible to have impurity, solution requires transparent limpid, and sodium aluminate solution requires matching while using, can not long storage time;Waterglass is in the process of dilution, after adding a certain amount of deionized water, and more than magnetic agitation 5min, it is ensured that dilute solution mix homogeneously。
The preparation of waterglass: flyash is through 4 magnetic separation, then through mechanical grinding, mill speed is 1200r/min, the fine powder powder obtained after pulverizing 4min, then with 82% sulphuric acid mix by solid-to-liquid ratio 5:4, and at 200 DEG C react 4h;Reaction end is that 1:3 adds water by the solid-to-liquid ratio of flyash Yu water, is heated to 90 DEG C after being cooled to room temperature, stirs 2h, after sucking filtration obtains filter cake, and is that 1:1 washs by the solid-to-liquid ratio of flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue;By the solid-to-liquid ratio of acid leaching residue Yu solution be 1:1 add concentration be the soda lye of 10.5%, and put into autoclave heat 10h, reaction temperature 180 DEG C;After being cooled to room temperature, filter and with a small amount of water washing solid slag, obtain waterglass。
The preparation of non-woven fabrics: being prepared non-woven fabrics by following component by weight forming, wherein flaxen fiber is 35%, and terylene chemical fibre is 30%, and chinlon chemical fibre is 25%, and viscose fibre is 10%。Properties of product test different technical parameters prepared, is shown in following table。
Technological parameter in each embodiment of table 1 and performance
Above example is only limited in order to technical scheme to be described; those of ordinary skill in the field are to be understood that; the specific embodiment of the present invention can being modified with reference to above-described embodiment or equivalent replacement, these are all being applied within the claims awaited the reply without departing from any amendment or equivalent replacement of spirit and scope of the invention。

Claims (9)

1. the constant pressure and dry method of non-woven fabrics/silicon-aluminium aerogel composite insulation boards, it is characterized in that, non-woven fabrics/sial wet gel good to solvent displacement and hydrophobically modified is carried out constant pressure and dry at low temperature 80~120 DEG C, then dries 40 minutes at high temperature 300~400 DEG C。
2. the constant pressure and dry method of a kind of non-woven fabrics/silicon-aluminium aerogel composite insulation boards according to claim 1, it is characterised in that the preparation of described non-woven fabrics/silicon-aluminium aerogel comprises the following steps:
(1) preparation sodium metaaluminate aqueous solution;
(2) prepare sial complex sol: under stirring, add in water glass solution preparation in step (1) sodium aluminate solution, stirring mixing 1~2min obtains forerunner's mixed solution;
(3) non-woven fabrics is completely immersed in forerunner's mixed solution, adsorbs full, stand 30min, automatic gel, the sial compound wet gel that the non-woven fabrics obtained strengthens, at room temperature aging 12h;
(4) carrying out solvent displacement, the sial compound wet gel that non-woven fabrics step (3) obtained strengthens immerses alcoholic solution, and through insulation, solvent is replaced, modified, namely obtains non-woven fabrics after drying and strengthens silicon-aluminium aerogel warming plate。
3. the constant pressure and dry method of a kind of non-woven fabrics/silicon-aluminium aerogel composite insulation boards according to claim 2, it is characterised in that the preparation method of described waterglass is as follows:
1) magnetic bead in magnetic separation separation of fine coal ash;
2) mechanical grinding;
3) acidleach: at 150 DEG C~220 DEG C, mixes flyash with the sulphuric acid that concentration is 80%~98% with the ratio that solid-to-liquid ratio is 2:1~1:1 of sulphuric acid in flyash, reacts 4~6h;
4) solid-liquid separation: after reactant is cooled to room temperature, it is that 1:2~1:6 preparation adds water by the solid-to-liquid ratio of flyash Yu water, at 75~95 DEG C, after stirring 1~3h, sucking filtration, the filter cake water washing that solid-to-liquid ratio is 2:1~1:2 by flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue;
5) acid leaching residue prepares waterglass: by acid leaching residue and 9%~12% soda lye by the proportions mixed liquor that solid-to-liquid ratio is 1:1~1:2, heat after 6~10h in reactor at 160~200 DEG C, be cooled to room temperature, filter and wash solid slag with water。
4. the constant pressure and dry method of a kind of non-woven fabrics/silicon-aluminium aerogel composite insulation boards according to claim 2, it is characterised in that the light transmittance of described sial compound wet gel is more than 80%。
5. the constant pressure and dry method of a kind of non-woven fabrics/silicon-aluminium aerogel composite insulation boards according to claim 2, it is characterized in that, described non-woven fabrics is by flaxen fiber, terylene chemical fibre is, chinlon chemical fibre and viscose fibre prepare, and described non-woven fabrics is 50~70% in the mass content of the silicon-aluminium aerogel that described non-woven fabrics strengthens。
6. the constant pressure and dry method of a kind of non-woven fabrics/silicon-aluminium aerogel composite insulation boards according to claim 2, it is characterised in that the displacement of described solvent adopts ethanol, and hexane equal solvent, described holding temperature is 50~70 DEG C, and described solvent time swap is more than 8h。
7. the constant pressure and dry method of a kind of non-woven fabrics/silicon-aluminium aerogel composite insulation boards according to claim 2, it is characterised in that described modified raw material adopts siloxanyl modified liquid, and modification temperature is 50~70 DEG C, and modification time is 7~9h。
8. the constant pressure and dry method of a kind of non-woven fabrics/silicon-aluminium aerogel composite insulation boards according to claim 2, it is characterized in that, it is 0.015~0.022W/ (m K) that described non-woven fabrics strengthens the heat conductivity of silicon-aluminium aerogel warming plate, and density is 220~450kg/m3, water absorption rate is less than 3%。
9. the constant pressure and dry method of a kind of non-woven fabrics/silicon-aluminium aerogel composite insulation boards according to claim 2, it is characterised in that it is the fire prevention of A level that described non-woven fabrics strengthens silicon-aluminium aerogel warming plate, and refractory temperature is higher than 650 DEG C。
CN201610065564.2A 2016-01-29 2016-01-29 Normal-pressure drying method of non-woven fabric/aluminum silicon aerogel composite heat preserving board Pending CN105698488A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111893649A (en) * 2020-07-17 2020-11-06 3M创新有限公司 Thermal insulation material, method for preparing thermal insulation material and product prepared from thermal insulation material
CN112524889A (en) * 2020-11-25 2021-03-19 航天特种材料及工艺技术研究所 Drying method of light dimensional ablation aerogel material
CN113083260A (en) * 2021-04-29 2021-07-09 中国科学院城市环境研究所 Aminated polysiloxane-based aerogel composite membrane, preparation method thereof and gas adsorption application

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JPH06191822A (en) * 1992-12-22 1994-07-12 Matsushita Electric Works Ltd Production of aerogel composite material
CN101318659A (en) * 2008-07-04 2008-12-10 绍兴纳诺气凝胶新材料研发中心有限公司 Method for preparing silicon dioxide silica aerogel composite material by drying in atmosphere pressure
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CN101993087A (en) * 2010-11-29 2011-03-30 中煤平朔煤业有限责任公司 Method for preparing water glass by using fly ash
CN103435055A (en) * 2013-06-29 2013-12-11 浙江工业大学 Method for preparing low density silica aerogel under normal pressure
CN103789924A (en) * 2012-10-31 2014-05-14 山东天鼎丰非织造布有限公司 Non-woven fabric

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06191822A (en) * 1992-12-22 1994-07-12 Matsushita Electric Works Ltd Production of aerogel composite material
CN101318659A (en) * 2008-07-04 2008-12-10 绍兴纳诺气凝胶新材料研发中心有限公司 Method for preparing silicon dioxide silica aerogel composite material by drying in atmosphere pressure
CN101698592A (en) * 2009-11-13 2010-04-28 航天特种材料及工艺技术研究所 Silicon-aluminium aerogel composite material and manufacturing method thereof
CN101993087A (en) * 2010-11-29 2011-03-30 中煤平朔煤业有限责任公司 Method for preparing water glass by using fly ash
CN103789924A (en) * 2012-10-31 2014-05-14 山东天鼎丰非织造布有限公司 Non-woven fabric
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111893649A (en) * 2020-07-17 2020-11-06 3M创新有限公司 Thermal insulation material, method for preparing thermal insulation material and product prepared from thermal insulation material
CN111893649B (en) * 2020-07-17 2022-07-26 3M创新有限公司 Thermal insulation material, method for preparing thermal insulation material and product prepared from thermal insulation material
CN112524889A (en) * 2020-11-25 2021-03-19 航天特种材料及工艺技术研究所 Drying method of light dimensional ablation aerogel material
CN113083260A (en) * 2021-04-29 2021-07-09 中国科学院城市环境研究所 Aminated polysiloxane-based aerogel composite membrane, preparation method thereof and gas adsorption application
CN113083260B (en) * 2021-04-29 2023-08-01 中国科学院城市环境研究所 Aminated polysiloxane-based aerogel composite membrane, preparation method and gas adsorption application thereof

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