CN111778649A - Method for quickly preparing nano heat-insulating material through supercritical drying - Google Patents
Method for quickly preparing nano heat-insulating material through supercritical drying Download PDFInfo
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- CN111778649A CN111778649A CN202010561205.2A CN202010561205A CN111778649A CN 111778649 A CN111778649 A CN 111778649A CN 202010561205 A CN202010561205 A CN 202010561205A CN 111778649 A CN111778649 A CN 111778649A
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- 238000000352 supercritical drying Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000011810 insulating material Substances 0.000 title claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 69
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000007788 liquid Substances 0.000 claims abstract description 47
- 239000000835 fiber Substances 0.000 claims abstract description 45
- 238000002360 preparation method Methods 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000011084 recovery Methods 0.000 claims abstract description 7
- 239000000499 gel Substances 0.000 claims description 71
- 238000010438 heat treatment Methods 0.000 claims description 30
- 239000003513 alkali Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000000413 hydrolysate Substances 0.000 claims description 15
- 239000012774 insulation material Substances 0.000 claims description 14
- 239000003292 glue Substances 0.000 claims description 12
- 238000009826 distribution Methods 0.000 claims description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 9
- 230000007062 hydrolysis Effects 0.000 claims description 9
- 238000006460 hydrolysis reaction Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 8
- 239000004964 aerogel Substances 0.000 claims description 8
- 239000000498 cooling water Substances 0.000 claims description 8
- 238000011068 loading method Methods 0.000 claims description 8
- 238000005086 pumping Methods 0.000 claims description 8
- 238000003860 storage Methods 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 108010009736 Protein Hydrolysates Proteins 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 239000001569 carbon dioxide Substances 0.000 claims description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000011240 wet gel Substances 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 239000003365 glass fiber Substances 0.000 claims description 2
- 239000008235 industrial water Substances 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 2
- 239000003921 oil Substances 0.000 claims description 2
- 239000007921 spray Substances 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims 1
- 239000000047 product Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000001879 gelation Methods 0.000 abstract description 4
- 238000005470 impregnation Methods 0.000 abstract description 4
- 239000002918 waste heat Substances 0.000 abstract description 3
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 238000004513 sizing Methods 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 1
- 125000006850 spacer group Chemical group 0.000 description 7
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000002210 supercritical carbon dioxide drying Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B1/00—Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating
- D06B1/02—Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating by spraying or projecting
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B15/00—Removing liquids, gases or vapours from textile materials in association with treatment of the materials by liquids, gases or vapours
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B23/00—Component parts, details, or accessories of apparatus or machines, specially adapted for the treating of textile materials, not restricted to a particular kind of apparatus, provided for in groups D06B1/00 - D06B21/00
- D06B23/20—Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration or distillation
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B9/00—Solvent-treatment of textile materials
- D06B9/06—Solvent-treatment of textile materials with recovery of the solvent
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Silicon Compounds (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a method for quickly preparing a nano heat-insulating material by supercritical drying, which combines liquid preparation, impregnation, gelation and drying together, directly impregnates a fiber felt roll in a drying kettle for molding and curing, and then directly heats up for drying by supercritical methanol or ethanol, thereby realizing the completely closed preparation of the nano heat-insulating material. The method omits the curing and forming step of the fibrofelt, the gel solution is injected into a drying kettle, redundant sizing materials are removed by utilizing the self-adsorption performance of the fibrofelt, supercritical drying is directly carried out after gelation, the process flow is simple, full automation is easy to realize, a large amount of equipment investment is saved, meanwhile, volatilization of a large amount of organic solvents and contact of personnel to volatile matters are avoided, waste heat recovery is carried out in the production process, and energy consumption can be saved to the maximum extent.
Description
Technical Field
The invention relates to a method for quickly preparing a nano heat-insulating material by supercritical drying.
Background
In the preparation process of the silicon oxide nanometer thermal insulation material, the currently known preparation method of the nanometer thermal insulation material generally adopts the compounding of aerogel and fiber felt fiber, then the soaking and aging are carried out after the addition of a spacer, or the hydrophobic modification process is carried out again, and then the supercritical carbon dioxide drying is carried out. The commonly adopted method for compounding the fiber felt with the gel liquid is a gel bath whole roll soaking method for gel, or an unreeling-dipping-heating curing-spacer-added reeling method.
After the gel tank dipping method impregnated fiber coiled material, a large amount of gel liquid formed block aerogel around the fibrofelt, add the spacer after the rewinding broken, dropped, formed a large amount of useless gel, and operation engineering needs a large amount of personnel to unreel, peels off unnecessary gel, and the rewinding adds work such as spacer, and the process is loaded down with trivial details, extravagant a large amount of gel liquid, forms a large amount of waste water to washing of equipment simultaneously.
If the unreeling-dipping-heating curing-composite forming-spacer adding reeling method is adopted, a long-distance production line device is needed so as to add the spacer after the gelling process is finished, and meanwhile, a large amount of solvent solution is volatilized due to the fact that gel liquid is exposed in a large area in a gel spraying dipping section and a wet gel felt is exposed in a reeling and spacer adding section, explosive mixed gas or toxic gas is easily formed, the formed mixed gas easily enters heating equipment, and great risk potential exists, so that the development of a closed aerogel production device is obviously very important.
The existing drying modes of the aerogel include a supercritical drying mode for preparing the nano heat-insulating material and a normal-pressure drying mode for preparing the nano heat-insulating material. Wherein supercritical carbon dioxide drying mode need be incessantly to carbon dioxide heat, cooling, compression, and equipment is complicated, and the energy consumption is high, and pressurization, replacement drying, pressure release time are long, and is high to operating personnel's requirement, are difficult to accomplish the automation, and the water in the wet gel felt is difficult to be drawed out by carbon dioxide, consequently great increase nanometer thermal insulation material's manufacturing cost. The nanometer heat-insulating material prepared by normal-pressure drying is gradually eliminated because the gel generates pore shrinkage and gel cracking in the drying process, the performance of the prepared nanometer heat-insulating material cannot meet the use requirement, the drying time is long, and the solution recovery rate is low.
With the progress of sealing technology and the development of automation technology, the safety of high-temperature supercritical alcohol drying is greatly improved, and the supercritical alcohol drying does not need to replace a solvent, and the drying of the gel can be completed only by heating the alcohol in the gel to the supercritical state and slowly releasing the alcohol solvent under the state of maintaining the supercritical condition. The supercritical ethanol drying does not need separation equipment, can complete the separation of drying only by a condenser and a condensate collecting tank, and has simple equipment and convenient operation.
Disclosure of Invention
The invention aims to provide a method for quickly preparing a nano heat-insulating material by supercritical drying, which combines liquid preparation, impregnation, gelation and drying together to realize completely closed preparation of the nano heat-insulating material, adopts an automatic roll loading and unloading technology to completely realize unmanned operation, and has the advantages of simple equipment structure, low energy consumption, easy recovery of supercritical ethanol steam waste heat, easy recovery of ethanol, safety, environmental protection and the like.
The technical scheme of the invention is as follows: a method for quickly preparing a nano heat-insulating material by supercritical drying is characterized by comprising the following steps:
step 1, hoisting and adding a fibrofelt coiled material fixed on a coiled material loading and unloading tray into a supercritical drying kettle, connecting a material distribution pipeline with a material inlet pipe inside the drying kettle by using a quick-connection clamp, and covering a kettle cover of the drying kettle;
step 3, spraying the mixed gel liquid on the top of a fiber felt roll in a cloth pipeline on the top of a supercritical drying kettle, adsorbing the gel liquid on the fiber felt due to capillary effect of the fiber felt to wet the fiber felt, pumping redundant gel liquid after the fiber felt roll is soaked into a gel liquid collecting tank by using negative pressure, circularly pumping the redundant gel liquid into the drying kettle again by using a gel liquid circulating pump to continuously spray, completely soaking the fiber felt, and finally using the redundant gel liquid for preparing aerogel particles;
step 4, after the fiber felt is impregnated by the gel liquid, heating the drying kettle by a heating device, stopping heating when the temperature is raised to 60 ℃, and preserving the heat for 1-3 hours to completely gel and solidify the wet gel fiber felt to obtain an alcohol gel fiber felt; then, continuously heating to 250-300 ℃ above the supercritical temperature, wherein the heating speed is stabilized at 1-2 ℃/min, detecting and safely discharging a device for detecting and adjusting the pressure of the drying kettle and maintaining the pressure of the drying kettle at 7-15 MPa, keeping the temperature for 30min after the temperature reaches 250-300 ℃, and starting pressure relief;
and 5, before pressure relief, firstly introducing condensed water into the condenser to circularly cool the water in the condenser, then opening the pressure relief valve of the drying kettle, keeping the temperature above the supercritical temperature in the pressure relief process, flushing the drying kettle by using inert gas nitrogen or carbon dioxide to cool to normal pressure after the pressure relief is finished, opening the kettle cover of the drying kettle after the internal and external pressures are balanced, and using hoisting equipment to hoist the finished nano heat-insulating material.
The hydrolysate consists of water, alcohol, an organic silicon source and acid; the dilute alkali solution comprises one or more of ammonia water, sodium hydroxide, potassium hydroxide and calcium hydroxide.
The acid comprises one or more of oxalic acid, acetic acid, hydrochloric acid, sulfuric acid, phosphoric acid and ammonium fluoride.
The organic silicon source is one or a mixture of methyl orthosilicate, ethyl orthosilicate, methyltrimethoxysilane and ethyltriethoxysilylalkoxysilane.
The complete equipment required for realizing the method comprises a hydrolysis device, an alkali preparation device, a pipeline mixer, a supercritical drying device and a glue solution circulating device according to a process route;
the hydrolysis device consists of a hydrolysate preparation tank, a first delivery pump and a first flowmeter, and is used for preparing hydrolysate, metering and delivering the hydrolysate to the pipeline mixer;
the alkali preparation device consists of an alkali preparation tank, a second delivery pump and a second flowmeter, is used for preparing dilute alkali liquor, is metered and delivered to the pipeline mixer, and mixes the hydrolysis liquid and the dilute alkali liquor in a specified proportion to form gel liquid for impregnating the fiber felt;
the supercritical drying device consists of a drying kettle condenser, a recovery tank and a delivery pump, and is used for impregnating, gelling and drying coiled fiber felts and condensing and recovering alcohol in a supercritical state;
the glue solution circulating device comprises a basket filter, a glue solution collecting tank, a glue solution circulating pump and a water circulating vacuum pump, wherein the water circulating vacuum pump provides a negative pressure for the glue solution collecting tank to absorb gel solution which is not soaked at the bottom of the drying kettle, the basket filter filters glass fiber yarns in the gel solution, and the glue solution circulating pump pumps the gel solution in the gel collecting tank into the drying kettle again to soak the fiber felt.
The drying kettle cover adopts a kettle cover quick-opening device for quick loading and unloading.
Drying kettle around have heating device, adopt the heating methods to have electrical heating or conduction oil heating, the top has gel liquid cloth pipeline to be used for spouting the even fibre felt coil stock top of following of gel liquid, cloth pipeline and the inside inlet pipe of drying kettle adopt the clamp connection, the quick dismantlement of being convenient for does not influence the business turn over of fibrofelt and nanometer thermal insulation material.
The condenser is connected with a cooling water supply pipe and a cooling water return pipe, and is cooled by cold water or industrial water to cool supercritical ethanol or methanol steam, the liquid alcohol is recovered by a condensate collecting tank, and the recovered liquid alcohol is conveyed to a subsequent alcohol storage tank by a third centrifugal pump.
And a detection device and a safety discharge device are arranged at an outlet at the top of the drying kettle, wherein the discharge device is a spring type safety valve, and an outlet of the safety valve is connected with the condenser.
The method omits the curing and forming step of the fibrofelt, the gel solution is injected into a drying kettle, redundant sizing materials are removed by utilizing the self-adsorption performance of the fibrofelt, supercritical drying is directly carried out after gelation, the process flow is simple, full automation is easy to realize, a large amount of equipment investment is saved, meanwhile, volatilization of a large amount of organic solvents and contact of personnel to volatile matters are avoided, waste heat recovery is carried out in the production process, and energy consumption can be saved to the maximum extent.
Drawings
FIG. 1 is a schematic flow chart of a method for rapidly preparing a nano heat-insulating material by supercritical drying.
Fig. 2 is a schematic view of a fiber felt roll loading and unloading device.
Fig. 3 is a schematic view of a fiber mat roll.
The reference numbers illustrate: 1-hydrolysate preparation tank, 2-first delivery pump, 3-first flowmeter, 4-alkali preparation tank, 5-second delivery pump, 6-second flowmeter, 7-pipeline mixer, 8-supercritical drying kettle, 9-heating device, 10-material distribution pipeline, 11-kettle cover, 12-detection and safety discharge device, 13-fiber felt coiled material, 14-condenser, 15-cooling water supply pipe, 16-cooling water return pipe, 17-condensate collection tank, 18-third delivery pump, 19-basket filter, 20-gel liquid collection tank, 21-water circulation vacuum pump, 22-gel liquid circulation pump, 23 coiled material loading and unloading tray, and 24 hoisting ring.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention is further described below with reference to the accompanying drawings and specific embodiments, but the present invention is not limited by the examples. Given the illustrated embodiments of this invention, those skilled in the art will readily appreciate that many modifications and substitutions can be made without departing from the scope of this invention.
Example 1
Referring to fig. 1 and 2, the invention provides a method for rapidly preparing a nano heat-insulating material by supercritical drying, and the whole process flow comprises the steps of preparing hydrolysate, preparing alkali liquor, mixing gel liquor, spraying and impregnating, circularly impregnating, heating and gelling, heating and drying, and finishing drying from front to back.
And (3) hoisting and adding the fiber felt coiled material 13 fixed on the coiled material loading and unloading tray 23 into the supercritical drying kettle 8, connecting the material distribution pipeline 10 with the feeding pipe of the drying kettle by using a quick-connection clamp, and covering the kettle cover 11 of the drying kettle.
Mixing ethyl orthosilicate and methyltriethoxysilane according to a molar ratio of 1:1, adding the mixture serving as an organic silicon source, ethanol, water and oxalic acid into a hydrolysate preparation tank 1 according to a molar ratio of 1:20:4:0.02, stirring, heating to 50 ℃, keeping the temperature constant for 4 hours, pumping by a first conveying pump 2, metering by a first flow meter 3, pumping an ethanol solution of 1mol/L diluted ammonia water mixed with an alkali preparation tank 4 by a second conveying pump 5, metering by a second flow meter 6, feeding the ethanol solution into a pipeline mixer 7 according to a flow rate of 15:1, feeding the mixed gel solution into a drying kettle 8 which is provided with a material distribution pipeline 10 and a fiber felt coiled material 13 in advance, spraying the gel solution above the fiber felt coiled material 13 to impregnate the fiber felt, and adsorbing the gel solution on the fiber felt due to a capillary effect to wet the fiber felt; the redundant gel liquid is collected below the drying kettle 8 and filtered by a basket filter 19;
the water circulation vacuum pump 21 provides a certain negative pressure for the gel liquid collecting tank 20 to pump the gel liquid at the bottom of the drying kettle to the gel liquid collecting tank 20, the gel liquid is conveyed to the drying kettle distribution pipeline 10 through the gel liquid circulating pump 22 to be continuously sprayed to completely impregnate the fiber felt, and finally redundant liquid is used for preparing aerogel particles after the impregnation is completed.
And starting the heating device 9 in the drying kettle 8 to work, heating the drying kettle 8 to 60 ℃, gradually starting the gel of the fiber felt coiled material 13 subjected to gel impregnation in the heating process of the drying kettle, and keeping the drying kettle at 60 ℃ for 2-3 hours to ensure that the gel is complete. And continuously heating to 270 ℃, wherein the heating speed is stabilized at 1-2 ℃/min, the temperature is 270 ℃, the pressure is kept for 1h at 10MPa, a condenser 14 is filled with cooling water through a cooling water supply pipe 15, a valve between the drying kettle and the condenser is opened to start pressure relief, the temperature is kept unchanged in the pressure relief process, the pressure is slowly relieved until the pressure is normal pressure, nitrogen is filled into the drying kettle 8 to reduce the temperature to 50 ℃, the drying kettle 8 is opened, a material distribution pipeline 10 is disassembled, and the dried nano heat insulation material is hoisted.
The ethanol collected by the condensate collection tank 17 is delivered to an ethanol storage tank by a third delivery pump 18. The dried nano heat insulating material coil is integrated with the coil mounting and dismounting tray 23, and as shown in fig. 2 and 3, after the lifting ring 24 on the coil mounting and dismounting tray 23 is removed, the coil mounting and dismounting tray 23 is directly pulled out, and the nano heat insulating material can be directly packaged.
Wherein the hydrolysate preparation tank 1 is provided with a stirring system and a heating jacket device for maintaining the hydrolysis temperature between 40 ℃ and 60 ℃.
The configured hydrolysate is conveyed by using a first centrifugal pump 2, the flow of the hydrolysate is measured by using a first flowmeter 3, the rotating speed of the centrifugal pump is adjusted, and the starting and stopping of the centrifugal pump are controlled.
The configured alkali liquor is conveyed by using a second centrifugal pump 5, the flow of the alkali liquor is measured by using a second flowmeter 6, the rotating speed of the centrifugal pump is adjusted, and the starting and stopping of the centrifugal pump are controlled.
Wherein the alkali preparation tank 4 is provided with a stirrer and is used for mixing one or more of ammonia water, sodium hydroxide, potassium hydroxide, calcium hydroxide and the like with water, methanol, ethanol and the like.
Wherein the pipeline mixer 7 is one of static pipeline mixers and is used for mixing the hydrolysate and the alkali liquor to form gel, and the inner core of the pipeline mixer is easy to be drawn out so as to be convenient for cleaning.
Wherein the basket filter 19 adopts 10-100 mesh meshes to filter the gel liquid, and the top of the filter is provided with an observation hole for observing the condition of the gel liquid, so that the redundant gel liquid can be timely discharged, and the gel in the pipeline can be prevented. And the waste gas pumped out by the water circulation vacuum pump 21 is conveyed to a waste gas washing tower for washing and purifying and then is discharged.
Example 2
The difference from the embodiment 1 is that the mixed silicon source is replaced by methyl orthosilicate and methyltrimethoxysilane which are mixed according to the proportion of 1:1, the catalyst acid is replaced by mixed acid of hydrochloric acid and hydrofluoric acid with the molar ratio of 1:2, and after the ethanol is replaced by methanol, the reaction is carried out according to the proportion of the silicon source: alcohol: water: mixing the acid with the molar ratio of 1:18:4.5:0.02 to form a hydrolysate, keeping the hydrolysis temperature between 40 and 55 ℃, keeping other conditions basically unchanged, and changing ethanol supercritical drying into methanol supercritical drying. The produced aerogel has better elasticity and lower heat conductivity coefficient.
Example 3
Different from the first embodiment, the fiber felt and the spacer (the hexagonal mesh made of the PP material) with the thickness of 5mm are rolled together, so that larger gaps are formed between layers of the fiber felt, the heat preservation time at the supercritical temperature is shortened to 30min, and the drying speed is accelerated. After drying, the nano heat insulation material needs to be rewound and the spacer is recycled, and the prepared nano heat insulation material has a stable surface structure and good appearance quality. Meanwhile, the method is also suitable for preparing the nano heat-insulating material by changing supercritical alcohol drying into supercritical carbon dioxide drying.
The above examples are specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any basic modifications such as changing the supercritical vertical storage tank to the horizontal type, connecting multiple supercritical drying storage tanks in series and parallel to form a large-scale production, and forming a completely unmanned and automated modification are within the scope of the present invention.
Claims (9)
1. A method for quickly preparing a nano heat-insulating material by supercritical drying is characterized by comprising the following steps:
step 1, hoisting and adding a fibrofelt coiled material (13) fixed on a coiled material loading and unloading tray (23) into a supercritical drying kettle (8), connecting a material distribution pipeline (10) with a feeding pipe inside the drying kettle by using a quick-connection hoop, and covering a kettle cover (11) of the drying kettle;
step 2, adding an organic silicon source, alcohol, water and acid from a storage tank area into a hydrolysate preparation tank (1) according to the molar ratio of 1: 0.5-2: 15-30: 0.01-0.05, stirring for 3-6 hours at the temperature of 40-60 ℃ to complete hydrolysis, mixing with diluted alkali liquor prepared from an alkali preparation tank (4) according to a fixed volume ratio of 22-12: 1 after pumping and metering, continuously conveying to a pipeline mixer (7) for mixing, and feeding mixed gel liquid into a supercritical drying kettle (8);
step 3, spraying the mixed gel liquid on the top of a fiber felt coiled material (13) in a material distribution pipeline (10) at the top of a supercritical drying kettle, adsorbing the gel liquid on the fiber felt due to capillary effect of the fiber felt to wet the fiber felt, pumping redundant gel liquid after the fiber felt coiled material (13) is soaked to a gel liquid collection tank (20) by using negative pressure, circularly pumping the gel liquid into the drying kettle again by a gel liquid circulating pump (22) to continuously spray, completely soaking the fiber felt, and finally using the redundant gel liquid to prepare aerogel particles;
step 4, after the fiber felt is impregnated by the gel liquid, heating the drying kettle (8) through a heating device (9), stopping heating when the temperature is raised to 60 ℃, and preserving the heat for 1-3 hours to completely gel and solidify the wet gel fiber felt to obtain the alcohol gel fiber felt; then, continuously heating to 250-300 ℃ above the supercritical temperature, wherein the heating speed is stabilized at 1-2 ℃/min, detecting and safely discharging a device (12) for detecting and adjusting the pressure of the drying kettle and maintaining the pressure of the drying kettle at 7-15 MPa, preserving the temperature for 30min after the temperature reaches 250-300 ℃, and starting to discharge the pressure;
and 5, before pressure relief, firstly introducing condensed water into the condenser (14) to circularly cool water in the condenser (14), then opening the pressure relief valve of the drying kettle, keeping the temperature above the supercritical temperature in the pressure relief process, flushing the drying kettle (8) by using inert gas nitrogen or carbon dioxide to cool to normal pressure after pressure relief is finished, opening the kettle cover (11) of the drying kettle after the internal pressure and the external pressure are balanced, and hoisting the finished product of the nano heat-insulating material by using hoisting equipment.
2. The supercritical drying rapid preparation method of nano heat insulation material according to claim 1, wherein the hydrolysate is composed of water, alcohol, organic silicon source, and acid; the dilute alkali solution comprises one or more of ammonia water, sodium hydroxide, potassium hydroxide and calcium hydroxide.
3. The supercritical drying rapid preparation method of nano thermal insulation material as claimed in claim 2, wherein the acid comprises one or more of oxalic acid, acetic acid, hydrochloric acid, sulfuric acid, phosphoric acid, ammonium fluoride.
4. The supercritical drying method for rapidly preparing nanometer heat insulating material according to claim 2, wherein the organic silicon source is one or more of methyl orthosilicate, ethyl orthosilicate, methyltrimethoxysilane and ethyltriethoxysilylalkoxysilane.
5. The supercritical drying rapid preparation method of nanometer heat insulation material as claimed in claim 1, characterized in that the complete sets of equipment required for realizing the method comprise a hydrolysis device, an alkali preparation device, a supercritical drying device, a glue solution circulating device according to the process route;
the hydrolysis device consists of a hydrolysate preparation tank (1), a first delivery pump (2) and a first flow meter (3), and is used for preparing hydrolysate, metering and delivering the hydrolysate to a pipeline mixer (7);
the alkali preparation device consists of an alkali preparation tank (4), a second delivery pump (5) and a second flowmeter (6), is used for preparing dilute alkali liquor, is metered and delivered to a pipeline mixer (7), and mixes the hydrolysate and the dilute alkali liquor in a specified proportion to form gel liquid for impregnating the fiber felt;
the supercritical drying device consists of a drying kettle (8), a condenser (14), a recovery tank (17) and a delivery pump (18), and is used for dipping, gelling and drying coiled fiber felts and condensing and recovering alcohol in a supercritical state;
the glue solution circulating device comprises a basket filter (19), a glue solution collecting tank (20), a glue solution circulating pump (22) and a water circulating vacuum pump (21), wherein the water circulating vacuum pump (21) provides a negative pressure for the glue solution collecting storage tank (20) to absorb gel solution which cannot be impregnated at the bottom of the drying kettle, the basket filter (19) filters glass fiber yarns in the gel solution, and the glue solution circulating pump (22) pumps the gel solution in the gel collecting tank (20) into the drying kettle again to impregnate the fiber mat.
6. The supercritical drying rapid preparation method of nanometer thermal insulation material as claimed in claim 5, characterized in that the drying still kettle cover (11) adopts a kettle cover quick-opening device for quick loading and unloading.
7. The supercritical drying rapid preparation method of nanometer thermal insulation material as claimed in claim 5, characterized in that the drying kettle (8) is surrounded by a heating device (9) which is heated by electricity or heat-conducting oil in a heating manner, the top is provided with a gel liquid distribution pipeline (10) for uniformly spraying gel liquid from the top of the fiber felt roll (13), and the distribution pipeline (10) is connected with the feeding pipe inside the drying kettle by a clamp, so as to facilitate rapid disassembly without affecting the inlet and outlet of the fiber felt and the nanometer thermal insulation material.
8. The supercritical drying rapid preparation method of nano heat insulating material according to claim 5, wherein the condenser (14) is connected with a cooling water supply pipe (15) and a cooling water return pipe (16), and is cooled by cold water or industrial water, supercritical ethanol or methanol vapor is cooled, and liquid alcohol is recovered by using a condensate collecting tank (17), and the recovered liquid alcohol is transferred to a subsequent alcohol storage tank by using a third centrifugal pump (18).
9. The supercritical drying rapid preparation method of nanometer heat insulation material as claimed in claim 5, characterized in that the outlet at the top of the drying kettle (8) is provided with a detection device and a safety relief device (12), wherein the relief device is a spring-type safety valve, and the outlet of the safety valve is connected with the condenser (14).
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| CN112411187A (en) * | 2020-11-23 | 2021-02-26 | 天津工业大学 | Preparation method of nano-cellulose aerogel composite fabric |
| CN113829545A (en) * | 2021-09-27 | 2021-12-24 | 江西宏柏新材料股份有限公司 | Roll type production device and method for aerogel composite material |
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