CN106007652A - Preparation method of high-temperature-resistant and hydrophobic SiO2 aerogel felt - Google Patents
Preparation method of high-temperature-resistant and hydrophobic SiO2 aerogel felt Download PDFInfo
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- CN106007652A CN106007652A CN201610327897.8A CN201610327897A CN106007652A CN 106007652 A CN106007652 A CN 106007652A CN 201610327897 A CN201610327897 A CN 201610327897A CN 106007652 A CN106007652 A CN 106007652A
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- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 53
- 239000004964 aerogel Substances 0.000 title claims abstract description 39
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910052681 coesite Inorganic materials 0.000 title abstract description 22
- 229910052906 cristobalite Inorganic materials 0.000 title abstract description 22
- 239000000377 silicon dioxide Substances 0.000 title abstract description 22
- 229910052682 stishovite Inorganic materials 0.000 title abstract description 22
- 229910052905 tridymite Inorganic materials 0.000 title abstract description 22
- 235000012239 silicon dioxide Nutrition 0.000 title abstract 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 73
- 230000032683 aging Effects 0.000 claims abstract description 25
- 239000011240 wet gel Substances 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000002253 acid Substances 0.000 claims abstract description 10
- 238000000352 supercritical drying Methods 0.000 claims abstract description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 8
- 239000010703 silicon Substances 0.000 claims abstract description 8
- 238000006073 displacement reaction Methods 0.000 claims abstract description 7
- 239000003513 alkali Substances 0.000 claims abstract description 5
- XTIIITNXEHRMQL-UHFFFAOYSA-N tripotassium methoxy(trioxido)silane Chemical compound [K+].[K+].[K+].CO[Si]([O-])([O-])[O-] XTIIITNXEHRMQL-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 64
- 239000000835 fiber Substances 0.000 claims description 17
- 239000000499 gel Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 6
- XYRAEZLPSATLHH-UHFFFAOYSA-N trisodium methoxy(trioxido)silane Chemical compound [Na+].[Na+].[Na+].CO[Si]([O-])([O-])[O-] XYRAEZLPSATLHH-UHFFFAOYSA-N 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000001117 sulphuric acid Substances 0.000 claims description 4
- 235000011149 sulphuric acid Nutrition 0.000 claims description 4
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052863 mullite Inorganic materials 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000003365 glass fiber Substances 0.000 claims description 2
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims 1
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 239000007783 nanoporous material Substances 0.000 abstract description 2
- 238000003980 solgel method Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract 2
- CAQWNKXTMBFBGI-UHFFFAOYSA-N C.[Na] Chemical compound C.[Na] CAQWNKXTMBFBGI-UHFFFAOYSA-N 0.000 abstract 1
- 239000004115 Sodium Silicate Substances 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000003607 modifier Substances 0.000 abstract 1
- 229910052911 sodium silicate Inorganic materials 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000000084 colloidal system Substances 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 230000035882 stress Effects 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000010793 Steam injection (oil industry) Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials
-
- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
Abstract
The invention belongs to the field of preparation processes of nano porous materials and relates to a preparation method of hydrophobic SiO2 aerogel felt resistant to high temperature (higher than or equal to 350 DEG C). A sol-gel method is adopted, wet gel is prepared from an organic silicon source serving as a silicon source, ethanol serving as a solvent, acid and alkali serving as catalysts as well as methyl sodium silicate and potassium methyl silicate serving as surface modifiers, and the high-temperature-resistant and hydrophobic modified SiO2 aerogel felt is obtained after the wet gel is subjected to aging, solvent displacement, supercritical drying and heat treatment. The prepared high-temperature-resistant and hydrophobic SiO2 aerogel felt can be used for a long time at the high temperature of 350 DEG C or above, keeps the hydrophobic effect and has low density, large specific surface area, high strength, high-temperature resistance, a good hydrophobic property and other excellent performance, and the problems that the hydrophobic property of current hydrophobic SiO2 aerogel disappears at the high temperature of 300 DEG C and the like are solved.
Description
Technical field
The invention belongs to the preparation technology field of nano-porous materials, relate to a kind of high temperature (>=350 DEG C) hydrophobic
SiO2The preparation method of aerogel blanket.Use sol-gel process, prepare high temperature by supercritical drying process
Hydrophobic SiO2Aerogel blanket.
Background technology
SiO2Nano-pore and tridimensional network that aeroge is unique make it have extremely low thermal conductivity, are a kind of good
Good heat-barrier material.Employ new technology and apply new and effective heat-barrier material can effectively reduce heat loss, joint
The about energy；Improve work situation, it is ensured that safety in production simultaneously, improve work efficiency.But modify without surface
SiO2Hydrophilic group-OH and porous structure are contained in aeroge surface, can cause SiO2Aeroge is prone to inhale
Attached water divides, thus causes aerogel structure to cave in, thus limits hydrophilic SiO2The application of aeroge.Mesh
Front commercially available hydrophobic SiO2Aeroge just has volatile substance releasing, hydrophobic performance to disappear at 300 DEG C, has a strong impact on
Aeroge uses in high temperature environments.Therefore the SiO at high temperature remaining to keep hydrophobic performance is prepared2Aeroge
Felt is significant to improving its actual application.
Summary of the invention
The invention aims to improve the deficiencies in the prior art and a kind of hydrophobic SiO of high temperature is provided2Aeroge
The preparation method of felt, the method technique is simple, and the hydrophobic SiO of high temperature prepared2Aerogel blanket, at 350 DEG C
Below still possessing hydrophobic performance, this material can be applied to urban heating network, steam injection as high temperature insulating material
The fields such as flow string.
The technical scheme is that a kind of hydrophobic SiO of high temperature2The preparation method of aerogel blanket, concrete steps
As follows:
(1) by silicon source and ethanol with volume ratio 1:(3～4) 1. mix homogeneously obtain solution；
(2) by ethanol, acid and water with volume ratio 1:(0.01～0.03): (0.2～0.4) mix homogeneously obtains
Solution is 2.；
(3) 3. the solution in step (1) is 1. the most uniformly mixed to get solution with the solution in step (2),
Wherein the volume ratio of solution 1. middle silicon source and solution 2. middle ethanol is 1:(0.5～1.5)；3. solution is sufficiently stirred for,
Stir at temperature 50～60 DEG C；Then continue stirring after cooling, and in solution, add alkali regulation pH extremely
6.5～7, now mixed solution is poured into equipped with the mould of fiber felt is treated its gel；
(4) SiO prepared in step (3)2Wet gel felt adds Ageing solution, seals and be positioned over 50～70 DEG C
Baking oven in aging, and replace Ageing solution, obtain wet gel；
(5) configuration modifying agent and ethanol is with volume ratio 1:(1～10) modified solution, with it to step (4)
The wet gel of aging mistake is modified, modification time 24～60h, modification temperature 20～60 DEG C；
(6) the modified wet gel felt obtained in step (5) is carried out supercritical drying process, after heat treatment
Obtain the hydrophobic SiO of high temperature2Aerogel blanket.
Said method prepares the hydrophobic SiO of high temperature2Aerogel blanket through 350 DEG C of hydrophobic angles of heat treatment is
120 °～130 °, apparent density is 0.18～0.24g/cm3, hydrophobic rate is 95%～99%.
Silicon source described in preferred steps (1) is methyl silicate or tetraethyl orthosilicate；Preferred steps (2)
Described in acid be the one in hydrochloric acid, nitric acid, sulphuric acid, Fluohydric acid. or acetic acid；The concentration of acid is 0.1-1mol/L.
Alkali described in preferred steps (3) is ammonia or sodium hydroxide；Described fiber felt is glass fibre, quartz
One in fiber, mullite fiber or alumina silicate fibre.Ageing solution described in preferred steps (4) is second
One in alcohol, normal hexane, hexamethylene, normal heptane or acetone.
In preferred steps (3), at temperature 50～60 DEG C, the rotating speed of stirring is 300～500rpm, and mixing time is
1～2h；In step (4), the number of times of displacement Ageing solution is 2～6 times, and every 8～12h displacements are once.
Modifying agent described in preferred steps (5) is one or both in potassium methyl silicate or sodium methyl silicate.
Supercritical drying described in preferred steps (6) is CO2Supercritical or Ethanol supercritical；Wherein CO2
Supercritical drying is with CO2As dry medium, reaction temperature is 50～70 DEG C, and in autoclave, pressure is
8～12MPa, drying time is 6～12h；Ethanol supercritical drying is using ethanol as dry medium, reaction temperature
Being 250～270 DEG C, in autoclave, pressure is 8～12MPa, and drying time is 2～2.5h.
Above-mentioned heat treatment temperature is about 350 DEG C, and heat treatment time is 2～3 hours.
Beneficial effect:
High temperature hydrophobically modified SiO prepared by the inventive method2Aerogel blanket has a characteristic that
(1) density is low, the hydrophobic SiO of high temperature prepared by this invention2The apparent density of aerogel blanket is
0.16～0.27g/cm3。
(2) high temperature hydrophobicity is good, hydrophobic SiO prepared by this inventive method2Aerogel blanket is after 350 DEG C of heat treatments
Still keeping preferable hydrophobicity, hydrophobic angle is 120 °～130 °.
(3) structural strength is good, by SiO2Aeroge and fiber felt are combined the SiO of preparation2Aerogel blanket has height
Intensity, can preferably be applied to insulation material aspect.
Accompanying drawing explanation
Fig. 1 is the hydrophobic SiO of high temperature that example 1 prepares2The photo in kind of aerogel blanket；
Fig. 2 is hydrophobic SiO in example 12Infrared figure before and after aerogel blanket high-temperature process, before wherein a is heat treatment
Hydrophobic SiO2The infrared figure of aerogel blanket, b is the hydrophobic SiO of the high temperature after 350 DEG C of heat treatments2Aerogel blanket
Infrared figure；
Fig. 3 is high temperature hydrophobically modified SiO in example 12The hydrophobic angle test figure of aerogel blanket.
Detailed description of the invention
Example 1
Analytical pure tetraethyl orthosilicate and ethanol are mixed homogeneously with the ratio of volume ratio 1:3 and obtains solution 1., ethanol,
2. hydrochloric acid (1mol/L) and water obtain solution with volume ratio 1:0.012:0.23 mix homogeneously, by solution 1. with molten
3. liquid be the most uniformly mixed to get solution, wherein the volume ratio of solution 1. middle tetraethyl orthosilicate and solution 2. middle ethanol
For 1:1.2,3. solution is placed magnetic stirring apparatus, 50 DEG C, under rotating speed 350rpm, be sufficiently stirred for 1.5h,
The most at room temperature addition ammonia continuation stirring and adjusting pH is to 6.5, and plastic emitting before non-gel is poured into and is placed with
The mould of glass mat is sufficiently impregnated with fiber felt, unnecessary colloid is poured out, under room temperature, treat its gel, solidifying
Add in ethanol is placed on the baking oven of 50 DEG C aging after glue in mould, Ageing solution of displacement in every 12 hours, put
Change 4 times.The wet gel felt after aging is placed the surface of the 1:9 volume ratio of ethanol (sodium methyl silicate with) again
In modified solution, being sufficiently impregnated with, in placing 50 DEG C of baking ovens, modified 48h, obtains modified wet gel felt.Again
Utilizing Ethanol supercritical to be dried sample, wherein in still, Stress control controls in 10MPa, temperature
260 DEG C, it is dried 2h, obtains hydrophobically modified SiO2Aerogel blanket.Finally by its heat treatment 2h at 350 DEG C
Obtain high temperature hydrophobically modified SiO2Aerogel blanket.The hydrophobic SiO of high temperature prepared2Aerogel blanket apparent density is
0.2032g/cm2, hydrophobic angle is 126.43 °, and hydrophobic rate is 98.42%.The obtained hydrophobic SiO of high temperature2Gas
The photo in kind of gel felt, as it is shown in figure 1, this composite aerogel felt is complete block, possesses certain mechanical strength,
And hydrophobic performance is good.Hydrophobic SiO in this example2Infrared figure such as Fig. 2 institute before and after aerogel blanket high-temperature process
Show；Obtained high temperature hydrophobically modified SiO2The hydrophobic angle test figure of aerogel blanket is as it is shown on figure 3, show height
SiO after temperature process2Aerogel blanket still has hydrophobic performance, advantageous as a kind of hydrophobic heat-barrier material of high temperature
Use.
Example 2
Analytical pure methyl silicate is mixed homogeneously with the ratio of volume ratio 1:3.2 with ethanol, ethanol, hydrochloric acid
(1mol/L) solution is obtained 2. with volume ratio 1:0.015:0.25 mix homogeneously, by solution 1. with solution 2. with water
Uniformly being mixed to get solution 3., wherein the volume ratio of solution 1. middle methyl silicate and solution 2. middle ethanol is 1:1,
3. solution is placed magnetic stirring apparatus, 55 DEG C, under rotating speed 300rpm, be sufficiently stirred for 1.8h, stop stirring,
The most at room temperature addition ammonia continuation stirring and adjusting pH is to 6.8, and plastic emitting before non-gel is poured into and is placed with
The mould of quartz fiber felt is sufficiently impregnated with fiber felt, unnecessary colloid is poured out, under room temperature, treat its gel, solidifying
Adding in the baking oven of 55 DEG C placed by ethanol aging after glue in mould, Ageing solution of displacement, puts for every eight hours
Change 6 times.The wet gel felt after aging is placed the surface of the 1:4 volume ratio of ethanol (potassium methyl silicate with) again
In modified solution, being sufficiently impregnated with, in placing 30 DEG C of baking ovens, modified 36h, obtains modified wet gel felt.Again
Utilize CO2Sample is dried by critical seasoning, and wherein in still, Stress control controls in 10MPa, temperature
At 55 DEG C, the supercritical drying time is 10h, obtains hydrophobically modified SiO2Aerogel blanket.Finally by it at 350 DEG C
Lower heat treatment 2.5h obtains high temperature hydrophobically modified SiO2Aerogel blanket.The hydrophobic SiO of high temperature prepared2Aerogel blanket
Apparent density is 0.1878g/cm3, hydrophobic angle is 127.26 °, and hydrophobic rate is 98.78%.
Example 3
Analytical pure tetraethyl orthosilicate is mixed homogeneously with the ratio of volume ratio 1:3.8 with ethanol, ethanol, sulphuric acid
(0.2mol/L) and 2. water obtain solution with volume ratio 1:0.025:0.28 mix homogeneously, by solution 1. and solution
The most uniformly being mixed to get solution 3., wherein the volume ratio of solution 1. middle tetraethyl orthosilicate and solution 2. middle ethanol is
1:0.8,3. places magnetic stirring apparatus by solution, 50 DEG C, under rotating speed 450rpm, be sufficiently stirred for 1.2h, stop
Only stirring, the most at room temperature adds sodium hydroxide (1mol/L) and continues stirring and adjusting pH to 7, non-gel
Front plastic emitting, is poured into be placed with in the mould of glass mat and is sufficiently impregnated with fiber felt, is poured out by unnecessary colloid,
Treat its gel under room temperature, add in acetone is placed on the baking oven of 60 DEG C aging after gel in mould, every 12 hours
Replace an Ageing solution, replace 4 times.Again the wet gel felt after aging is placed 1:2.3 (sodium methyl silicate with
The volume ratio of ethanol) surface modification solution in, be sufficiently impregnated with, place modified 60h in 25 DEG C of baking ovens, obtain
Modified wet gel felt.Recycling CO2Sample is dried by supercritical, and wherein in still, Stress control exists
8MPa, temperature controls at 70 DEG C, is dried 8h, obtains hydrophobically modified SiO2Aerogel blanket.Finally by its
At 350 DEG C, heat treatment 3h obtains high temperature hydrophobically modified SiO2Aerogel blanket.The hydrophobic SiO of high temperature prepared2Airsetting
Rubber mat apparent density is 0.1968g/cm3, hydrophobic angle is 123.58 °, and hydrophobic rate is 97.96%.
Example 4
Analytical pure methyl silicate is mixed homogeneously with the ratio of volume ratio 1:4 with ethanol, ethanol, sulphuric acid
(0.2mol/L) solution is obtained 2. with volume ratio 1:0.03:0.3 mix homogeneously, by solution 1. with solution 2. with water
Uniformly being mixed to get solution 3., wherein the volume ratio of solution 1. middle methyl silicate and solution 2. middle ethanol is
1:0.6,3. places magnetic stirring apparatus by solution, 60 DEG C, rotating speed be under 480rpm, be sufficiently stirred for 1h,
Stop stirring, the most at room temperature add sodium hydroxide (1mol/L) continue stirring and adjusting pH to 7, before non-gel
Plastic emitting, is poured in the mould being placed with mullite fiber felt and is sufficiently impregnated with fiber felt, is poured out by unnecessary colloid,
Treat its gel under room temperature, add in acetone is placed on the baking oven of 65 DEG C aging after gel in mould, every 12 hours
Replace an Ageing solution, replace 3 times.Again the wet gel felt after aging is placed 1:1.5 (sodium methyl silicate with
The volume ratio of ethanol) surface modification solution in, be sufficiently impregnated with, place modified 26h in 40 DEG C of baking ovens, obtain
Modified wet gel felt.Sample is dried by recycling Ethanol supercritical, and wherein in still, Stress control exists
8MPa, temperature controls at 250 DEG C, is dried 2.5h, obtains hydrophobically modified SiO2Aerogel blanket.Finally by it
At 350 DEG C, heat treatment 2.5h obtains high temperature hydrophobically modified SiO2Aerogel blanket.The hydrophobic SiO of high temperature prepared2
Aerogel blanket apparent density is 0.2255g/cm3, hydrophobic angle is 125.34 °, and hydrophobic rate is 96.23%.
Claims (9)
1. the hydrophobic SiO of high temperature2The preparation method of aerogel blanket, specifically comprises the following steps that
(1) by silicon source and ethanol with volume ratio 1:(3～4) 1. mix homogeneously obtain solution；
(2) by ethanol, acid and water with volume ratio 1:(0.01～0.03): (0.2～0.4) mix homogeneously obtains
Solution is 2.；
(3) 3. the solution in step (1) is 1. the most uniformly mixed to get solution with the solution in step (2),
Wherein the volume ratio of solution 1. middle silicon source and solution 2. middle ethanol is 1:(0.5～1.5)；3. solution is sufficiently stirred for,
Stir at temperature 50～60 DEG C；Then continue stirring after cooling, and in solution, add alkali regulation pH extremely
6.5～7, now mixed solution is poured into equipped with the mould of fiber felt is treated its gel；
(4) SiO prepared in step (3)2Wet gel felt adds Ageing solution, seals and be positioned over 50～70 DEG C
Baking oven in aging, and replace Ageing solution, obtain wet gel；
(5) configuration modifying agent and ethanol is with volume ratio 1:(1～10) modified solution, with it to step (4)
The wet gel of aging mistake is modified, modification time 24～60h, modification temperature 20～60 DEG C；
(6) the modified wet gel felt obtained in step (5) is carried out supercritical drying process, after heat treatment
Obtain the hydrophobic SiO of high temperature2Aerogel blanket.
Preparation method the most according to claim 1, it is characterised in that prepare the hydrophobic SiO of high temperature2Gas
Gel felt is 120 °～130 ° through 350 DEG C of hydrophobic angles of heat treatment, and apparent density is 0.18～0.24g/cm3, hydrophobic
Rate is 95%～99%.
Preparation method the most according to claim 1, it is characterised in that the silicon source described in step (1) is
Methyl silicate or tetraethyl orthosilicate.
Preparation method the most according to claim 1, it is characterised in that the acid described in step (2) is salt
One in acid, nitric acid, sulphuric acid, Fluohydric acid. or acetic acid；The concentration of acid is 0.1-1mol/L.
Preparation method the most according to claim 1, it is characterised in that the alkali described in step (3) is ammonia
Water or sodium hydroxide；Described fiber felt is glass fibre, quartz fibre, mullite fiber or alumina silicate fibre
In one.
Preparation method the most according to claim 1, it is characterised in that the Ageing solution described in step (4)
For the one in ethanol, normal hexane, hexamethylene, normal heptane or acetone.
Preparation method the most according to claim 1, it is characterised in that temperature 50～60 DEG C in step (3)
The rotating speed of lower stirring is 300～500rpm, and mixing time is 1～2h；In step (4), displacement Ageing solution is secondary
Number is 2～6 times, and every 8～12h displacements are once.
Preparation method the most according to claim 1, it is characterised in that the modifying agent described in step (5)
For one or both in potassium methyl silicate or sodium methyl silicate.
Preparation method the most according to claim 1, it is characterised in that the supercritical described in step (6)
It is dried as CO2Supercritical or Ethanol supercritical；Wherein CO2Supercritical drying is with CO2As dry medium,
Reaction temperature is 50～70 DEG C, and in autoclave, pressure is 8～12MPa, and drying time is 6～12h；Ethanol
Supercritical drying is 250～270 DEG C using ethanol as dry medium, reaction temperature, and in autoclave, pressure is
8～12MPa, drying time is 2～2.5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610327897.8A CN106007652A (en) | 2016-05-17 | 2016-05-17 | Preparation method of high-temperature-resistant and hydrophobic SiO2 aerogel felt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610327897.8A CN106007652A (en) | 2016-05-17 | 2016-05-17 | Preparation method of high-temperature-resistant and hydrophobic SiO2 aerogel felt |
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| CN106747562A (en) * | 2016-12-07 | 2017-05-31 | 河南城建学院 | A kind of Silica Aerogels and preparation method suitable for making superadiabatic visual window |
| CN108221367A (en) * | 2018-03-21 | 2018-06-29 | 青岛纳博科环保科技有限公司 | Hydrophobic modifier for activated carbon fibre and preparation method thereof, hydrophobic active Carbon fibe and preparation method thereof |
| CN108484096A (en) * | 2018-04-01 | 2018-09-04 | 中鸿纳米纤维技术丹阳有限公司 | A kind of nanoscale thermal insulation aeroge of extra-low density |
| CN110029491A (en) * | 2019-04-14 | 2019-07-19 | 泰州浩纳新材料科技有限公司 | A kind of production technology of nano composite heat insulation felt insulation |
| CN110902690A (en) * | 2019-12-25 | 2020-03-24 | 巩义市泛锐熠辉复合材料有限公司 | Method for rapidly preparing hydrophobic silica aerogel by repeatedly increasing and decreasing pressure |
| CN111099912A (en) * | 2019-12-24 | 2020-05-05 | 贵州航天乌江机电设备有限责任公司 | High-temperature-resistant heat-insulation wave-transparent integrated aerogel composite material and preparation process thereof |
| CN111848205A (en) * | 2020-07-13 | 2020-10-30 | 航天特种材料及工艺技术研究所 | Method for preparing high-temperature-resistant aerogel heat-insulating material by normal-pressure drying |
| CN112079618A (en) * | 2020-09-14 | 2020-12-15 | 南京工业大学 | Preparation method of modified silica aerogel heat insulation sheet |
| CN114162827A (en) * | 2021-12-22 | 2022-03-11 | 中国人民解放军国防科技大学 | High-temperature-resistant hydrophobic SiO2Preparation method of aerogel heat insulation composite material |
| CN114804819A (en) * | 2022-06-14 | 2022-07-29 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of high-temperature-resistant aerogel composite material and composite material thereof |
| CN115304350A (en) * | 2022-08-29 | 2022-11-08 | 湖北硅金凝节能减排科技有限公司 | Preparation method of hydrophobic silica aerogel felt |
| CN117468274A (en) * | 2023-12-28 | 2024-01-30 | 淄博华源新材料有限公司 | Glass fiber-aerogel composite fiber paper and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106747562A (en) * | 2016-12-07 | 2017-05-31 | 河南城建学院 | A kind of Silica Aerogels and preparation method suitable for making superadiabatic visual window |
| CN106747562B (en) * | 2016-12-07 | 2019-07-12 | 河南城建学院 | A kind of Silica Aerogels and preparation method suitable for making superadiabatic visual window |
| CN108221367A (en) * | 2018-03-21 | 2018-06-29 | 青岛纳博科环保科技有限公司 | Hydrophobic modifier for activated carbon fibre and preparation method thereof, hydrophobic active Carbon fibe and preparation method thereof |
| CN108484096A (en) * | 2018-04-01 | 2018-09-04 | 中鸿纳米纤维技术丹阳有限公司 | A kind of nanoscale thermal insulation aeroge of extra-low density |
| CN110029491A (en) * | 2019-04-14 | 2019-07-19 | 泰州浩纳新材料科技有限公司 | A kind of production technology of nano composite heat insulation felt insulation |
| CN111099912A (en) * | 2019-12-24 | 2020-05-05 | 贵州航天乌江机电设备有限责任公司 | High-temperature-resistant heat-insulation wave-transparent integrated aerogel composite material and preparation process thereof |
| CN110902690A (en) * | 2019-12-25 | 2020-03-24 | 巩义市泛锐熠辉复合材料有限公司 | Method for rapidly preparing hydrophobic silica aerogel by repeatedly increasing and decreasing pressure |
| CN111848205A (en) * | 2020-07-13 | 2020-10-30 | 航天特种材料及工艺技术研究所 | Method for preparing high-temperature-resistant aerogel heat-insulating material by normal-pressure drying |
| CN112079618A (en) * | 2020-09-14 | 2020-12-15 | 南京工业大学 | Preparation method of modified silica aerogel heat insulation sheet |
| CN114162827A (en) * | 2021-12-22 | 2022-03-11 | 中国人民解放军国防科技大学 | High-temperature-resistant hydrophobic SiO2Preparation method of aerogel heat insulation composite material |
| CN114162827B (en) * | 2021-12-22 | 2023-10-03 | 中国人民解放军国防科技大学 | High-temperature-resistant hydrophobic SiO 2 Preparation method of aerogel heat insulation composite material |
| CN114804819A (en) * | 2022-06-14 | 2022-07-29 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of high-temperature-resistant aerogel composite material and composite material thereof |
| CN115304350A (en) * | 2022-08-29 | 2022-11-08 | 湖北硅金凝节能减排科技有限公司 | Preparation method of hydrophobic silica aerogel felt |
| CN115304350B (en) * | 2022-08-29 | 2023-09-19 | 湖北硅金凝节能减排科技有限公司 | Preparation method of hydrophobic silica aerogel felt |
| CN117468274A (en) * | 2023-12-28 | 2024-01-30 | 淄博华源新材料有限公司 | Glass fiber-aerogel composite fiber paper and preparation method thereof |
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