CN115259167A - Vacuum continuous modification process and device - Google Patents
Vacuum continuous modification process and device Download PDFInfo
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- CN115259167A CN115259167A CN202210876669.1A CN202210876669A CN115259167A CN 115259167 A CN115259167 A CN 115259167A CN 202210876669 A CN202210876669 A CN 202210876669A CN 115259167 A CN115259167 A CN 115259167A
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- Prior art keywords
- vacuum
- inert gas
- modifier
- kettle
- tank
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- 238000012986 modification Methods 0.000 title claims abstract description 65
- 230000004048 modification Effects 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000003607 modifier Substances 0.000 claims abstract description 136
- 239000011261 inert gas Substances 0.000 claims abstract description 130
- 239000007788 liquid Substances 0.000 claims abstract description 100
- 238000000926 separation method Methods 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 9
- 238000011084 recovery Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000005086 pumping Methods 0.000 claims description 12
- 238000009833 condensation Methods 0.000 claims description 8
- 230000005494 condensation Effects 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000002274 desiccant Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
- 239000000499 gel Substances 0.000 description 35
- 230000002209 hydrophobic effect Effects 0.000 description 17
- 239000003054 catalyst Substances 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 10
- 239000004964 aerogel Substances 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 8
- 239000003921 oil Substances 0.000 description 8
- 239000002904 solvent Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 239000003513 alkali Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 5
- -1 alkyl alkoxy silane Chemical compound 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 229910000077 silane Inorganic materials 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000002738 chelating agent Substances 0.000 description 2
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 2
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 0.000 description 2
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 2
- 125000001165 hydrophobic group Chemical group 0.000 description 2
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000000352 supercritical drying Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 2
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 description 1
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 1
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 1
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 description 1
- HXLAEGYMDGUSBD-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propan-1-amine Chemical compound CCO[Si](C)(OCC)CCCN HXLAEGYMDGUSBD-UHFFFAOYSA-N 0.000 description 1
- ZYAASQNKCWTPKI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-amine Chemical compound CO[Si](C)(OC)CCCN ZYAASQNKCWTPKI-UHFFFAOYSA-N 0.000 description 1
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 description 1
- KNTKCYKJRSMRMZ-UHFFFAOYSA-N 3-chloropropyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)CCCCl KNTKCYKJRSMRMZ-UHFFFAOYSA-N 0.000 description 1
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- ZMAPKOCENOWQRE-UHFFFAOYSA-N diethoxy(diethyl)silane Chemical compound CCO[Si](CC)(CC)OCC ZMAPKOCENOWQRE-UHFFFAOYSA-N 0.000 description 1
- VSYLGGHSEIWGJV-UHFFFAOYSA-N diethyl(dimethoxy)silane Chemical compound CC[Si](CC)(OC)OC VSYLGGHSEIWGJV-UHFFFAOYSA-N 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- CTLDFURRFMJGON-UHFFFAOYSA-N dimethoxy-methyl-(3-piperazin-1-ylpropyl)silane Chemical compound CO[Si](C)(OC)CCCN1CCNCC1 CTLDFURRFMJGON-UHFFFAOYSA-N 0.000 description 1
- WEHWNAOGRSTTBQ-UHFFFAOYSA-N dipropylamine Chemical compound CCCNCCC WEHWNAOGRSTTBQ-UHFFFAOYSA-N 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 229940102253 isopropanolamine Drugs 0.000 description 1
- 229940018564 m-phenylenediamine Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- NHBRUUFBSBSTHM-UHFFFAOYSA-N n'-[2-(3-trimethoxysilylpropylamino)ethyl]ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCNCCN NHBRUUFBSBSTHM-UHFFFAOYSA-N 0.000 description 1
- YLBPOJLDZXHVRR-UHFFFAOYSA-N n'-[3-[diethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CCO[Si](C)(OCC)CCCNCCN YLBPOJLDZXHVRR-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 150000002835 noble gases Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 1
- IWICDTXLJDCAMR-UHFFFAOYSA-N trihydroxy(propan-2-yloxy)silane Chemical compound CC(C)O[Si](O)(O)O IWICDTXLJDCAMR-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000011240 wet gel Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/159—Coating or hydrophobisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/04—Silica-rich materials; Silicates
- C04B14/06—Quartz; Sand
- C04B14/064—Silica aerogel
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Civil Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a vacuum continuous modification process and a device, wherein a gel material is placed in a vacuum kettle, the vacuum kettle is vacuumized and then heated, the gel is in a vacuum high-temperature environment, a modifier liquid is rapidly gasified after entering the vacuum high-temperature environment in the vacuum kettle and is filled in the vacuum kettle, when the pressure in the vacuum kettle is 0.05-0.09MPa, suction is stopped, the gel material is in the vacuum kettle filled with the modifier gas, then modification is carried out for 3-6h, the gaseous modifier can be attached to the surface of the gel for modification, the vacuum kettle is broken by introducing inert gas from the upper part of the vacuum kettle, the inert gas is continuously injected to take away the rest of the modifier, the inert gas enters a condenser for gas-liquid separation, the separated inert gas is pumped into an inert gas pressure tank, the modifier liquid enters a modifier liquid tank after being liquefied, compared with the traditional surface modification solution, the use amount of the modifier is greatly saved, and the use amount of the modifier is increased.
Description
Technical Field
The invention relates to the technical field of aerogel, in particular to a vacuum continuous modification process and a vacuum continuous modification device.
Background
As a high-porosity super-porous material, the surface of the traditionally prepared silicon dioxide aerogel contains more hydroxyl groups, so that the hydrophilicity is too good, and the weather resistance is poor. The structural instability of hydrophilic aerogels limits their range of applications, which is one of the reasons for the large number of studies on hydrophobic aerogels. The surface of the aerogel is modified by soaking with a hydrophobic agent, and the surface of the hydrophobically modified aerogel is completely changed into hydrophobicity.
CN201680003854.2 relates to a method for preparing highly hydrophobic silica aerogel, which reduces the preparation time by performing surface modification and solvent replacement simultaneously in a single step, wherein the surface modification is achieved by soaking in a surface modification solution. The preparation process has the following problems that a large amount of surface modification solution is required to be used, the surface modification solution is prepared by a surface modifier and a solvent, the concentration of the surface modification solution cannot reach the concentration required by reuse after the surface modification solution is modified once, the surface modification solution after being soaked has high proportion of waste, and is not beneficial to continuous production in actual production.
Disclosure of Invention
In view of the above, the invention aims to provide a vacuum continuous modification process, which effectively solves the problems of large usage amount and low utilization rate of surface modification solution in the existing gel modification process.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a vacuum continuous modification process comprises the following steps;
opening a vacuum kettle, putting gel to be modified into the vacuum kettle, and then sealing the vacuum kettle;
step two, performing vacuum pumping operation in the vacuum kettle by using a vacuum pump to ensure that the vacuum pressure in the vacuum kettle is lower than a set value;
step three, heating the vacuum kettle after vacuumizing is finished, and heating the vacuum kettle to a temperature at which the liquid modifier for later use can be gasified;
opening a valve between the vacuum kettle and the modifier liquid tank, pressing the liquid modifier in the modifier liquid tank into the vacuum kettle under the action of pressure difference, stopping suction when the pressure in the vacuum kettle reaches a certain pressure, and modifying the gel to be modified;
step five, after the modification is finished, opening an inert gas valve between an inert gas pressure tank and a vacuum kettle, opening a condensation valve between the vacuum kettle and a condenser, and introducing inert gas into the vacuum kettle to break vacuum;
step six, the inert gas carrying the residual modifier in the vacuum kettle circulates to a condenser for gas-liquid separation, the liquid modifier obtained by separation flows back to a modifier liquid tank through a pipeline, and the inert gas obtained by separation is conveyed to an inert gas pressure tank for recycling;
and seventhly, circulating the inert gas until the residual modifier is completely recovered, closing an inert gas valve and a condensation valve, opening the vacuum kettle, and taking out the modified gel.
Further, in the second step, the vacuum pressure in the vacuum kettle after the vacuumizing operation is not higher than-0.07 MPa.
And in the fourth step, stopping sucking the modifier liquid when the vacuum pressure in the vacuum kettle reaches-0.05 to-0.01 MPa, and keeping the modification time for 3 to 6 hours.
And in the seventh step, the circulation time of the inert gas is 30 to 120min.
Further, the inert gas pressure tank is used for supplying inert gas with constant pressure into the modified vacuum kettle to break vacuum, and the inert gas pressure tank is communicated with a dryer for containing a drying agent and used for drying the recovered inert gas.
Further, the inert gas pressure tank is communicated with the inert gas supply tank through a pressure regulating valve, and the constant pressure in the inert gas pressure tank is maintained, wherein the constant pressure is the normal pressure.
Further, the upper part of the vacuum kettle is communicated with an inert gas pressure tank, the lower part of the vacuum kettle is communicated with a modifier liquid tank, modifier liquid enters the vacuum kettle from the lower part, and the liquid modifier is gasified at high temperature in vacuum and is filled in the vacuum kettle; inert gas enters the vacuum kettle from the upper part to break vacuum, and takes the modifier out of the vacuum kettle downwards, and the temperature of the vacuum kettle is raised by the vacuum kettle in a heat conduction oil heating mode.
Furthermore, a plurality of vacuum kettles are arranged, an upper branch pipe and a lower branch pipe are arranged above and below each vacuum kettle, a liquid outlet main pipe is arranged at an outlet of the modifier liquid tank, a recovery main pipe is arranged at a recovery port of the condenser, the liquid outlet main pipe and the recovery main pipe are respectively communicated with each lower branch pipe through a three-way valve, a suction port of the vacuum pump is provided with a vacuum pumping main pipe, an inert gas main pipe is arranged at an outlet of the inert gas pressure tank, and the vacuum pumping main pipe and the inert gas main pipe are respectively communicated with each upper branch pipe through the three-way valve; so that a plurality of vacuum kettles can work independently.
Further, the vacuum continuous modification device comprises a modifier liquid tank, a condenser, an inert gas pressure tank, an inert gas supply tank, a dryer, a vacuum pump and at least one vacuum kettle; an air pressure meter and a temperature sensor which are used for respectively detecting the internal pressure, the air pressure and the temperature are arranged in the inner cavity of the vacuum kettle; the upper part of the vacuum kettle is provided with a vacuumizing pipe and an inert gas pipe, the vacuumizing pipe is communicated with a vacuum pump, the inert gas pipe is communicated with an inert gas pressure tank, and a valve is arranged on a pipeline to control the opening and the closing; the lower part of the vacuum kettle is provided with a liquid inlet pipe and a recovery pipe, the liquid inlet pipe is communicated with a modifier liquid tank, the recovery pipe is communicated with a recovery port of the condenser, and a valve is arranged on a pipeline to control the opening and the closing; the modifier liquid tank is communicated with a liquid phase outlet of the condenser through a pipeline, the inert gas pressure tank is communicated with a gas phase outlet of the condenser through a pipeline, and the inert gas pressure tank is provided with a pressure gauge and is connected with a dryer and an inert gas supply tank.
Furthermore, the vacuum kettles are provided with a plurality of vacuum kettles, the upper part and the lower part of each vacuum kettle are respectively provided with an upper branch pipe and a lower branch pipe, the liquid inlet pipe and the recovery pipe are respectively communicated with each lower branch pipe through a three-way valve, and the vacuumizing pipe and the inert gas pipe are respectively communicated with each upper branch pipe through the three-way valve.
The beneficial effects of the above technical scheme are: according to the invention, a gel material is placed in a vacuum kettle, the vacuum kettle is vacuumized and then heated, so that a gel is in a vacuum high-temperature environment, a modifier liquid can be automatically sucked in due to a negative pressure environment in the vacuum kettle, the modifier liquid is rapidly gasified after entering the vacuum high-temperature environment in the vacuum kettle and is filled in the vacuum kettle, the suction is stopped when the pressure in the vacuum kettle is within minus 0.05 to minus 0.01MPa, the vacuum kettle is sealed, so that the gel material is in the vacuum kettle filled with the modifier gas, and then modification is carried out for 3 to 6 hours, in the process, the gaseous modifier can be attached to the surface of the gel for modification, and the gel material is fast in molecular motion and high in modification efficiency at a vacuum high temperature, so that the gel material is soaked in a traditional surface modification solution, the dosage of the modifier is greatly saved, and the utilization rate of the modifier is improved.
Meanwhile, the residual modifier in the vacuum kettle is recovered, inert gas is introduced from the upper part of the vacuum kettle to break the vacuum, the inert gas is continuously injected and takes away the residual modifier, the residual modifier enters a condenser to be subjected to gas-liquid separation, the separated inert gas is pumped into an inert gas pressure tank, and the liquefied modifier enters a modifier liquid tank to recycle the inert gas and the modifier.
Meanwhile, the modifier is selected to be pure, and an alkali catalyst is not required to be added, so that the modifier can be recycled after being modified once, the problem that the proportion is not uniform due to the loss of the modifier after modification is avoided, and the modifier can be continuously recycled.
Therefore, the invention provides a vacuum continuous modification process, which realizes the surface modification of gel through a plurality of tank bodies, modifies the gel by adopting a gaseous modifier, takes away the residual modified liquid by utilizing inert gas, and can recycle the modifier by gas-liquid separation in a condenser without interruption; the gas phase modifier has high permeation efficiency and good modification effect, and greatly improves the utilization rate of the modification liquid.
Drawings
FIG. 1 is a process flow diagram of the present invention;
reference numerals: the device comprises a vacuum kettle 1, a modifier liquid tank 2, a condenser 3, an inert gas pressure tank 4, an inert gas supply tank 5, a dryer 6, a vacuum pump 7, a pump 8, a pressure gauge 9, a temperature sensor 10 and a three-way valve 11.
Detailed Description
The invention is described in further detail below with reference to the following figures and embodiments:
in embodiment 1, this embodiment aims to provide a vacuum continuous modification process, which is mainly used for modifying gel, and aims to solve the problems that the surface modification solution in the existing gel modification process is large in dosage and low in utilization rate, and the surface modification solution is prepared by a surface modifier and a solvent, and the concentration of the surface modification solution cannot reach the concentration required for reuse after being modified once.
As shown in fig. 1, a vacuum continuous modification process in the present embodiment comprises at least one vacuum tank 1, a modifier liquid tank 2, a condenser 3, an inert gas pressure tank 4, an inert gas supply tank 5, a dryer 6, and a vacuum pump 7 in configuration; in this embodiment, a vacuum kettle is taken as an example for explanation, the vacuum kettle 1 is provided with two kettle walls, heat conducting oil and a heating wire are arranged in the two kettle walls at intervals, the heat conducting oil can be introduced into the kettle walls at intervals for heating, the heating wire is used for heating the temperature to be higher than the boiling point of the selected modifier, and a barometer 9 and a temperature sensor 10 for respectively detecting the internal pressure and the temperature are arranged in the inner cavity of the vacuum kettle 1; the upper part of the vacuum kettle 1 is provided with a vacuum tube and an inert gas tube, wherein the vacuum tube is communicated with a vacuum pump 7, the inert gas tube is communicated with an inert gas pressure tank 4, a valve is arranged on a pipeline to control the opening and closing of the inert gas pressure tank, the lower part of the vacuum kettle is provided with a liquid inlet tube and a recovery tube, the liquid inlet tube is communicated with a modifier liquid tank 2, the recovery tube is communicated with a recovery port of a condenser 3, and the valve is arranged on the pipeline to control the opening and closing of the liquid inlet tube and the recovery tube.
Certainly, as another embodiment, the evacuation pipe and the inert gas pipe may be an integrated pipe, and are connected to the inert gas pressure tank and the vacuum pump through the three-way valve 11, respectively, the liquid inlet pipe and the recovery pipe are connected to the modifier liquid tank and the condenser through the three-way valve, respectively, and in implementation, the three-way valve is an electromagnetic three-way valve, so as to achieve the purpose of electric control or automatic control of the controller. The condenser 3 is a device capable of taking away heat of the gaseous modifier to convert the gaseous modifier into liquid, and can be a water cooling type condenser or an air cooling type condenser, wherein the water cooling type condenser adopts a shell-and-tube type or a sleeve-type condenser, and the air cooling type condenser can adopt a coiled tube type condenser. The condenser can also be selected as the existing air-cooled condenser to carry out surface heat exchange. A gas-liquid separator can be additionally arranged between the condenser 3 and the modifier liquid tank 2, which is beneficial to further separation of inert gas and liquid modifier obtained by condensation.
Structurally, modifier liquid tank 2 is through the liquid phase export intercommunication of pipeline with condenser 3, and inert gas overhead tank 4 is through the gaseous phase export intercommunication of pipeline (being equipped with the pump additional) with condenser 3, is provided with the manometer on the inert gas overhead tank 4 to be connected with desicator 6 and inert gas supply tank 5, utilize inert gas supply tank 5 to come to continuously provide gas for inert gas overhead tank, go on inert gas overhead tank, utilize desicator 6 to carry out the drying to inert gas overhead tank inside gas. The dryer 6 may be an adsorption dryer, and the inert gas is dried for the second time by using the characteristic of the adsorbent (activated alumina, silica gel, molecular sieve, etc.) to adsorb liquid.
The modifier liquid tank 2 is used for containing a modifier and is communicated with the vacuum kettle 1 to supply modifier liquid to the vacuum kettle 1 after vacuumizing, a liquid adding port for supplementing the modifier is reserved in the modifier liquid tank 2, the modifier is selected to be pure modifier in the embodiment and is gasified in a high-temperature vacuum environment to modify the surface of the gel, the gasified modifier has fast molecular motion, an alkali catalyst does not need to be added, the mode is pure solvent gas phase modification, the components of the modifier are single, the recycled modifier can be directly used, and the problem of the proportion of the existing modifier solution is not considered.
When the vacuum continuous modification process is used, the vacuum continuous modification process comprises the following steps;
step one, opening a vacuum kettle 1, putting gel to be modified into the vacuum kettle 1, and then sealing the vacuum kettle 1;
secondly, performing vacuum pumping operation in the vacuum kettle 1 by using a vacuum pump to ensure that the vacuum pressure in the vacuum kettle 1 is lower than a set value;
step three, heating the vacuum kettle 1 after vacuumizing is finished, and heating the vacuum kettle 1 to a temperature at which the liquid modifier to be used can be gasified, wherein the temperature at which the liquid modifier can be gasified refers to the temperature (range) at which the liquid modifier is converted into the gaseous modifier under the negative pressure state in the vacuum kettle 1; the heat conduction oil heating mode of the vacuum kettle 1 is heating through a heat conduction oil circulation heating mode, a flow guide pipeline for heat conduction oil circulation is arranged on the outer wall of the vacuum kettle, and the heated heat conduction oil circulates outside the vacuum kettle through the flow guide pipeline so as to conduct contact type conduction heating on the vacuum kettle.
In terms of the selection of the modifier, the modifier in this embodiment may be hexamethyldisilazane, the corresponding vacuum pressure after vacuum pumping is-0.075 MPa, the gasification temperature is higher than 120 ℃, preferably 120 to 130 ℃, and within this temperature range, the hexamethyldisilazane can be completely gasified; the modifier can also be dimethyl dimethoxy silane, the vacuum pressure after vacuum pumping is-0.085 MPa, the gasification temperature is higher than 120 ℃, preferably 120 to 130 ℃, and the methyl dimethoxy silane can be completely gasified within the temperature range.
Opening a valve between the vacuum kettle 1 and the modifier liquid tank 2, keeping the interior of the modifier liquid tank 2 at normal pressure, pressing the liquid modifier in the modifier liquid tank 2 into the vacuum kettle 1 under the action of pressure difference, gasifying the pressed modifier in a vacuum high-temperature environment, allowing the modifier liquid to enter the vacuum kettle 1 from the lower part, gasifying the modifier liquid at vacuum high temperature, filling the vacuum kettle 1, stopping suction when the vacuum pressure in the vacuum kettle 1 reaches-0.05 to-0.01 MPa, closing the valve, and keeping the modification time for 3-6 hours;
the inert gas pressure tank 4 is communicated with an inert gas supply tank 5 through a pressure regulating valve, and the inert gas pressure tank 4 is replenished with inert gas lost by taking out the modified material, and the constant pressure in the inert gas pressure tank 4 is maintained, and the constant pressure is normal pressure.
The inert gas is a chemically inert gas, and in this embodiment, the inert gas is nitrogen. In other embodiments, the inert gas may be one of the noble gases.
Step five, firstly, the condenser 3 is started, and the cooling medium in the condenser 3 circulates in advance; opening an inert gas valve between the inert gas pressure tank 4 and the vacuum kettle 1, introducing inert gas into the vacuum kettle 1 to break vacuum, wherein the inert gas pressure tank 4 is used for supplying constant-pressure inert gas into the modified vacuum kettle 1 to break vacuum; opening a condensation valve between the vacuum kettle 1 and the condenser 3, and communicating the inert gas pressure tank 4 with a dryer 6 for containing the molecular sieve for drying the recovered inert gas; the upper part of the vacuum kettle 1 is communicated with an inert gas pressure tank 4, and the lower part of the vacuum kettle is communicated with a modifier liquid tank 2; the inert gas enters the vacuum kettle 1 from the upper part to break vacuum, and the modifier is taken out of the vacuum kettle 1 downwards.
Step six, at this time, the circulation path of the inert gas is as follows: inert gas pressure tank 4-vacuum kettle 1-condenser 3-inert gas pressure tank 4. Circulating inert gas carries residual modifier remained in the vacuum kettle 1 to circulate to a condenser 3 for gas-liquid separation, the liquid modifier obtained by separation flows back to a modifier liquid tank 2 through a pipeline, the inert gas obtained by separation is pressurized and conveyed to an inert gas pressure tank 4 through a pump 8 for recycling, and a gas one-way valve is arranged between the inert gas pressure tank 4 and the pump 8 to ensure the circulating flow direction of the inert gas; and in the fourth step, the residual modifier in the vacuum kettle is the modifier which does not participate in the gel modification reaction in the vacuum kettle after the modification time is over.
And seventhly, circulating until the residual modifier is completely recovered, closing the inert gas valve and the condensation valve, opening the vacuum kettle, and taking out the modified gel.
In this embodiment, the gel is a wet gel that can be prepared as a sol-solution gel of an aerogel.
Example 2, this example increases the number of vacuum vessels in addition to example 1.
The vacuum kettle in this embodiment is provided with a plurality of, 3 are shown in fig. 1, upper and lower branch pipes are arranged on each vacuum kettle, a liquid outlet main pipe is arranged at the outlet of the modifier liquid tank, a recovery port recovery main pipe of the condenser is arranged, the liquid outlet main pipe and the recovery main pipe are respectively communicated with each lower branch pipe through a three-way valve, a suction port of the vacuum pump is provided with a vacuum pumping main pipe, an inert gas pressure tank outlet is provided with an inert gas main pipe, and the vacuum pumping main pipe and the inert gas main pipe are respectively communicated with each upper branch pipe through the three-way valve.
In the embodiment, a plurality of vacuum kettles are connected in parallel, gel to be modified can be placed in the vacuum kettles simultaneously or in batches, the vacuum kettles 1 are vacuumized by a vacuum pump 7, heating is carried out by heating oil in the vacuum kettle separation layer, the inner cavities of the vacuum kettles are heated to the boiling temperature of the used modifier, and the structure can be obtained by a pressure gauge and a temperature sensor on the vacuum kettles; opening a valve between the vacuum kettle 1 and the modifier liquid tank 2, sucking the liquid in the modifier liquid tank 2 into the vacuum kettle 1, and keeping the modification time of 3-6 h; opening valves between an inert gas pressure tank 4 and a vacuum kettle 1 and between the vacuum kettle 1 and a condenser 3, breaking vacuum through inert gas, circulating the inert gas through a circulating passage of the inert gas pressure tank 4-the vacuum kettle 1-the condenser 3-a booster pump-the inert gas pressure tank 4, circulating the inert gas carrying a modifier into the condenser 3, carrying out gas-liquid separation, returning the separated liquid modifier into a modifier liquid tank 2 through a pipeline, conveying the separated inert gas into the inert gas pressure tank 4 through an additional pump for circulation until the residual modifier is completely recovered, closing the valves between the inert gas pressure tank 4 and the vacuum kettle 1 and between the vacuum kettle 1 and the condenser 3, opening the vacuum kettle 1, and taking out modified gel.
The modifier used in the conventional soaking process is a liquid modifier, and the modifier is prepared by blending an alcohol solvent, an alkali catalyst and a modifier, wherein the alcohol solvent is used as a diluting and dissolving solvent, the alkali catalyst is used for accelerating the modification speed, and the modifier in the embodiment is selected as a pure modifier as a distinguishing part, and the alkali catalyst is not required to be added, so that the modifier can be repeatedly recycled, the problem that the proportion is uneven due to the loss of the modifier after modification is avoided, and the modifier can be continuously recycled is solved.
In this example, the modifying agent was hexamethyldisilazane and methyldimethoxysilane.
In the fourth step of reagent pressure mapping in this embodiment, the liquid modifier in the modifier liquid tank 2 is sucked into the vacuum kettle 1, and the sucked modifier is gasified in a vacuum high-temperature environment, which is the vacuum pressure in the vacuum kettle 1.
In order to verify the hydrophobic modification effect of the present invention, three experiments were performed with hexamethyldisilazane and dimethyldimethoxysilane as modifiers, and the hydrophobic ratio was tested. The hydrophobic rate test is carried out according to the hydrophobic test method (GB/T10299-2011) of the heat insulating material, and the hydrophobic rate of the obtained modified gel is 99.2% -99.8%.
Therefore, in the embodiment, under the condition that the alkali catalyst is not added, by means of the vacuum high-temperature environment in the vacuum kettle 1, the liquid modifier entering the vacuum kettle 1 is quickly gasified, the gasified modifier is used for modifying the gel in the vacuum high-temperature environment, and experiments prove that the pure modifier has a better modification effect, so that the requirements of people can be met, compared with the traditional process, a novel modification process is provided, the utilization rate of the modifier is greatly improved, and the work efficiency of modification is also improved.
In this embodiment, the gel is a gel or gel-fiber material composite (e.g., a gel mat) prepared from a silica sol. The preparation method of the silica sol comprises the following steps: uniformly mixing a silicon source, ethanol and water, adding a catalyst, and uniformly stirring to obtain a silicon dioxide sol; wherein the silicon-based material is obtained by mixing silicon source, ethanol, water = 1: 2 to 60: 0.05 to 30 in molar ratio; the silicon source is one or more of ethyl orthosilicate, methyl orthosilicate, butyl orthosilicate, isopropyl orthosilicate and alkyl alkoxy silane; the alkyl alkoxy silane comprises one or more of methyl trimethoxy silane, dimethyl dimethoxy silane, methyl triethoxy silane, dimethyl diethoxy silane, vinyl triethoxy silane, propyl trimethoxy silane and propyl triethoxy silane; the catalyst comprises an alkaline catalyst, wherein the alkaline catalyst is one or a combination of two of sodium hydroxide, potassium hydroxide, ammonia water, ammonium fluoride, ammonium bicarbonate, sodium carbonate, sodium bicarbonate, ethanolamine, diethanolamine, methylamine, dimethylamine, ethylamine, diethylamine, propylamine, dipropylamine, isopropanolamine, aniline, o-phenylenediamine, m-phenylenediamine and p-phenylenediamine.
In other embodiments, when the liquid modifier is a hydrophobic modification reagent, the hydrophobic gel can be prepared by regulating the type of the hydrophobic modifier, the vacuumizing pressure, the reagent pressure, the heating temperature of the vacuum kettle and the modification time, and the hydrophobic rate of the obtained hydrophobic gel is 99-99.8% according to a hydrophobic rate test and a thermal insulation material hydrophobic test method (GB/T10299-2011). Wherein the liquid hydrophobizing agent comprises one or more of hydrophobic alkoxysilanes, hexamethyldisiloxane and hexamethyldisilazane; the molecular formula of the alkoxy silane is R3mSi（OR4）（4-m）Wherein R is3Is a hydrophobic group, R4Is alkyl, m is the number of hydrophobic groups, 4-m is the number of alkyl, and the value of m is an integer between 1 and 3. Specifically, the hydrophobic agent comprises methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, propyltrimethoxysilane, chlorineAny one or more of propyl triethoxysilane, chloropropyl trimethoxysilane, chloropropyl methyldimethoxysilane, dimethyldiethoxysilane, diethyldimethoxysilane, diethyldiethoxysilane, trimethylchlorosilane and hexamethyldisiloxane.
In other implementations, other liquid hydrophilic modifiers that vaporize at high temperatures under vacuum may be used. The liquid hydrophilic modifier is hydrophilic alkoxy silane with the molecular formula of R1nSi（OR2）（4-n）(ii) a Wherein R is1Is a hydrophilic group, R2Is alkyl, n is the number of hydrophilic groups, 4-n is the number of alkyl, and n is an integer between 1 and 3. Specifically, the hydrophilic agent comprises any one or more of 3-aminopropylmethyldimethoxysilane, 3-aminopropylmethyldiethoxysilane, aminoethylaminopropylmethyldiethoxysilane, diethylenetriaminopropyltrimethoxysilane, gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-piperazinylpropylmethyldimethoxysilane, gamma-glycidyloxypropyltrimethoxysilane and gamma-N-butyl-gamma-aminopropyltrimethoxysilane.
In other embodiments, the gel is a gel or gel-fiber material composite (e.g., a gel mat) prepared from an alumina sol or a silicon aluminum composite sol. Wherein, the preparation steps of the alumina sol comprise: an aluminum source, a chelating agent, alcohol, water and an aluminum sol are mixed by a catalyst according to a molar ratio of 1: (0.001 to 0.06): (4 to 32): (0.6 to 4): (0.0001 to 1), mixing to obtain aluminum sol catalyzed by a gel catalyst; the preparation method of the silicon-aluminum composite sol comprises the following steps: (1) preparing silica sol: firstly, mixing one or more organic silicon sources, water and alcohol according to a molar ratio of 1: (4 to 50): (2 to 10), adding a hydrolysis catalyst, and after uniform mixing, hydrolyzing a silicon source to form silica sol; (2) preparing an aluminum sol: an aluminum source, a chelating agent, alcohol and water are mixed according to a molar ratio of 1: (0.001 to 0.06): (4 to 32): (0.6 to 4): (0.0001 to 1), and mixing to obtain an aluminum sol; and (3) mixing the silica sol and the aluminum sol according to the molar ratio of silicon: aluminum = (1 to 8): (1 to 8) pouring the mixture into a container, and mixing and stirring the mixture for 10 to 30min to obtain silicon-aluminum composite sol; and (4) adding a gel catalyst into the silicon-aluminum composite sol.
In other embodiments, the modified gel is further dried (to obtain the aerogel) before being modified, and then modified (to the aerogel). The drying method comprises drying under normal pressure, and CO2Supercritical drying, ethanol supercritical drying, etc.
Claims (10)
1. A vacuum continuous modification process is characterized by comprising the following steps;
opening a vacuum kettle, putting gel to be modified into the vacuum kettle, and then sealing the vacuum kettle;
step two, carrying out vacuum-pumping operation in the vacuum kettle;
step three, after the vacuumizing is finished, heating the vacuum kettle to a temperature at which the liquid modifier for standby can be gasified;
opening a valve between the vacuum kettle and the modifier liquid tank, pressing the liquid modifier in the modifier liquid tank into the vacuum kettle under the action of pressure difference, stopping sucking when the pressure in the vacuum kettle reaches a certain pressure, and modifying the gel to be modified;
step five, after the modification is finished, opening an inert gas valve between an inert gas pressure tank and the vacuum kettle, opening a condensation valve between the vacuum kettle and a condenser, and introducing inert gas into the vacuum kettle to break vacuum;
step six, the inert gas carrying the residual modifier in the vacuum kettle is circulated to a condenser for condensation and gas-liquid separation, the liquid modifier obtained by separation flows back to a modifier liquid tank through a pipeline, and the inert gas obtained by separation is conveyed to an inert gas pressure tank for recycling;
and seventhly, circulating the inert gas until the residual modifier is completely recovered, closing an inert gas valve and a condensation valve, opening the vacuum kettle, and taking out the modified gel.
2. The vacuum continuous modification process of claim 1, wherein: in the second step, after the vacuum pumping operation, the vacuum pressure in the vacuum kettle is not higher than-0.07 MPa.
3. The vacuum continuous modification process of claim 1, wherein: in the fourth step, when the vacuum pressure in the vacuum kettle reaches-0.05 to-0.01 MPa, a valve between the vacuum kettle and the modifier liquid tank is closed, and the modification time is kept for 3 to 6 hours.
4. The vacuum continuous modification process of claim 1, wherein: and seventhly, the circulation time of the inert gas is 30 to 120min.
5. The vacuum continuous modification process of claim 1, wherein: the inert gas pressure tank is used for supplying inert gas with constant pressure into the vacuum kettle after modification to break vacuum, and the inert gas pressure tank is communicated with a dryer for containing a drying agent and is used for drying the recovered inert gas.
6. The vacuum continuous modification process of claim 5, wherein: the inert gas pressure tank is communicated with the inert gas supply tank through a pressure regulating valve, and maintains constant pressure in the inert gas pressure tank, wherein the constant pressure is normal pressure.
7. The vacuum continuous modification process of any one of claims 1 to 6, wherein: the upper part of the vacuum kettle is communicated with an inert gas pressure tank, the lower part of the vacuum kettle is communicated with a modifier liquid tank, modifier liquid enters the vacuum kettle from the lower part, and the liquid modifier is gasified at high temperature in vacuum and is filled in the vacuum kettle; inert gas enters the vacuum kettle from the upper part to break vacuum, and takes the modifier out of the vacuum kettle downwards, and the temperature of the vacuum kettle is raised by the vacuum kettle in a heat conduction oil heating mode.
8. The vacuum continuous modification process of claim 7, wherein: the device comprises a plurality of vacuum kettles, a modifier liquid tank, a condenser, a vacuum pump, a vacuum tank, a vacuum master pipe, an inert gas pressure tank and a vacuum pump, wherein the vacuum kettles are provided with a plurality of vacuum kettles, the upper part and the lower part of each vacuum kettle are respectively provided with an upper branch pipe and a lower branch pipe, the outlet of the modifier liquid tank is provided with a liquid outlet master pipe, the recovery port of the condenser is provided with a recovery master pipe, the liquid outlet master pipe and the recovery master pipe are respectively communicated with each lower branch pipe through a three-way valve, the suction port of the vacuum pump is provided with a vacuum pumping master pipe, the outlet of the inert gas pressure tank is provided with an inert gas master pipe, and the vacuum pumping master pipe and the inert gas master pipe are respectively communicated with each upper branch pipe through the three-way valve; so that a plurality of vacuum kettles can work independently.
9. A vacuum continuous modification device is characterized by comprising a modifier liquid tank, a condenser, an inert gas pressure tank, an inert gas supply tank, a dryer, a vacuum pump and at least one vacuum kettle; an air pressure gauge and a temperature sensor which are used for respectively detecting the internal pressure and the temperature are arranged in the inner cavity of the vacuum kettle; the upper part of the vacuum kettle is provided with a vacuumizing pipe and an inert gas pipe, the vacuumizing pipe is communicated with a vacuum pump, the inert gas pipe is communicated with an inert gas pressure tank, and a valve is arranged on a pipeline to control the opening and the closing; the lower part of the vacuum kettle is provided with a liquid inlet pipe and a recovery pipe, the liquid inlet pipe is communicated with a modifier liquid tank, the recovery pipe is communicated with a recovery port of the condenser, and a valve is arranged on a pipeline to control the opening and the closing; the modifier liquid tank is communicated with a liquid phase outlet of the condenser through a pipeline, the inert gas pressure tank is communicated with a gas phase outlet of the condenser through a pipeline, and the inert gas pressure tank is provided with a pressure gauge and is connected with a dryer and an inert gas supply tank.
10. The vacuum continuous modification apparatus according to claim 9, wherein a plurality of vacuum vessels are provided, each vacuum vessel is provided with an upper branch pipe and a lower branch pipe at the upper and lower sides thereof, the liquid inlet pipe and the recovery pipe are respectively communicated with each lower branch pipe through a three-way valve, and the evacuation pipe and the inert gas pipe are respectively communicated with each upper branch pipe through a three-way valve.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20180370809A1 (en) * | 2016-03-24 | 2018-12-27 | Lg Chem, Ltd. | System for preparing silica aerogel |
| CN113247911A (en) * | 2021-06-10 | 2021-08-13 | 绍兴文理学院 | Modification method of silicon dioxide aerogel |
| CN114751718A (en) * | 2022-04-01 | 2022-07-15 | 巩义市泛锐熠辉复合材料有限公司 | Method for preparing hydrophobic silica aerogel felt under normal pressure |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20180370809A1 (en) * | 2016-03-24 | 2018-12-27 | Lg Chem, Ltd. | System for preparing silica aerogel |
| CN113247911A (en) * | 2021-06-10 | 2021-08-13 | 绍兴文理学院 | Modification method of silicon dioxide aerogel |
| CN114751718A (en) * | 2022-04-01 | 2022-07-15 | 巩义市泛锐熠辉复合材料有限公司 | Method for preparing hydrophobic silica aerogel felt under normal pressure |
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