CN111188188A - Preparation method of hydrophobic precipitated silica composite material - Google Patents
Preparation method of hydrophobic precipitated silica composite material Download PDFInfo
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- CN111188188A CN111188188A CN202010034397.1A CN202010034397A CN111188188A CN 111188188 A CN111188188 A CN 111188188A CN 202010034397 A CN202010034397 A CN 202010034397A CN 111188188 A CN111188188 A CN 111188188A
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- precipitated silica
- hydrophobic
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 151
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 61
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 50
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000011268 mixed slurry Substances 0.000 claims abstract description 20
- 239000003607 modifier Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 7
- 238000013329 compounding Methods 0.000 claims abstract description 5
- 239000000835 fiber Substances 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 7
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- 239000004917 carbon fiber Substances 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- DRUOQOFQRYFQGB-UHFFFAOYSA-N ethoxy(dimethyl)silicon Chemical compound CCO[Si](C)C DRUOQOFQRYFQGB-UHFFFAOYSA-N 0.000 claims description 4
- 239000003365 glass fiber Substances 0.000 claims description 4
- 229920000620 organic polymer Polymers 0.000 claims description 4
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 3
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
- MDLRQEHNDJOFQN-UHFFFAOYSA-N methoxy(dimethyl)silicon Chemical compound CO[Si](C)C MDLRQEHNDJOFQN-UHFFFAOYSA-N 0.000 claims description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 3
- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 claims description 3
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 3
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 3
- 238000007306 functionalization reaction Methods 0.000 abstract description 2
- 239000002002 slurry Substances 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 12
- 238000009413 insulation Methods 0.000 description 7
- 239000011148 porous material Substances 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 5
- 239000007858 starting material Substances 0.000 description 5
- 239000004964 aerogel Substances 0.000 description 4
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- 239000004965 Silica aerogel Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 238000002715 modification method Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- -1 feed Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000003605 opacifier Substances 0.000 description 1
- 239000010451 perlite Substances 0.000 description 1
- 235000019362 perlite Nutrition 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 239000010455 vermiculite Substances 0.000 description 1
- 235000019354 vermiculite Nutrition 0.000 description 1
- 229910052902 vermiculite Inorganic materials 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
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- 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
-
- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
-
- 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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
-
- 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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention belongs to the field of preparation of new materials, and particularly relates to a preparation method of a hydrophobic precipitated silica composite material. The method comprises the steps of mixing and stirring the aqueous precipitated silica slurry, the silane coupling agent and the hydrophobic modifier to prepare a mixed slurry, compounding the mixed slurry and the fibrofelt, and drying to obtain the hydrophobic precipitated silica composite material. According to the method, the hydrophobic functionalization of the precipitated silica is realized by adding the modifier into the slurry, the damage to the structure of the precipitated silica product caused by adding the modifier into a modifier solution is avoided, the flexibility is better, the environment friendliness is better, and the method is suitable for the industrial hydrophobic modification of the precipitated silica. The obtained hydrophobic precipitated silica composite material has an apparent density of 0.08 to0.20g/cm3The thermal conductivity is 0.024-0.032W/(m.K), and the water contact angle is 100-135 deg.
Description
Technical Field
The invention belongs to the field of preparation of new materials, and particularly relates to a preparation method of a hydrophobic precipitated silica composite material.
Background
Silica aerogel has structural features of low density, high specific surface area, large porosity, etc., and gives it excellent thermal insulation properties, but the high cost of silica aerogel limits its wide range of applications.
The cost of the precipitated silicon dioxide is far lower than that of the silicon oxide aerogel, only less than five percent of the silicon oxide aerogel is used, the precipitated silicon dioxide is used for a heat-insulating material, large-area popularization is facilitated, and the cost of engineering application can be reduced by matching the precipitated silicon dioxide with the silicon oxide aerogel. The precipitated silica is a nano silica material prepared from water glass and inorganic acid, is generally used in the industries of tire reinforcement, plastic filler, daily chemicals, feed, coating and the like, and is rarely mentioned as a heat insulation material.
Patent 201080007741.2 reports heat insulating materials and molded articles thereof containing precipitated silica with product components of precipitated silica, opacifiers, binders and particulate insulating fillers (vermiculite, perlite, powdered coal, silica, etc.), but does not describe hydrophobic precipitated silica composite articles and related solutions.
Patents 201710893609.X and 201110178448.9 provide a hydrophobic modification method of precipitated silica, the main technical route of which is to react a solution containing a hydrophobic modifier with precipitated silica to achieve hydrophobicity of the precipitated silica, and which is a post-modification method that destroys the structure of the precipitated silica.
Disclosure of Invention
The invention aims to provide a preparation method of a hydrophobic precipitated silica composite material. The method has no damage to the structure of the precipitated silica, and the hydrophobic precipitated silica composite material can be used for heat insulation, sound insulation or vacuum heat insulation board core materials.
The technical scheme of the invention is as follows: a preparation method of hydrophobic precipitated silica composite material is characterized by comprising the following steps:
mixing and stirring the water-based precipitated silica slurry, the silane coupling agent and the hydrophobic modifier to prepare mixed slurry, then compounding the mixed slurry with the fibrofelt, and finally drying to obtain the hydrophobic precipitated silica composite material.
The apparent density of the hydrophobic precipitated silica composite material prepared by the invention is 0.08 to0.20g/cm3The thermal conductivity is 0.024-0.032W/(m.K), and the water contact angle is 100-135 deg.
Preferably, the mass solid content of the aqueous precipitated silica slurry is 5-25%. (more preferably, the bulk density of the precipitated silica powder after spray drying of the aqueous precipitated silica slurry is 0.10 to 0.15g/cm3Pore volume of 1.5-2.0 cm3G, dry SiO basis2The content mass fraction is 92-98%. )
Preferably, the silane coupling agent is one of 3-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, N-aminoethyl-gamma-aminopropyltriethoxysilane or N-aminoethyl-gamma-aminopropyltrimethoxysilane.
Preferably, the hydrophobic modifier is one of methyltriethoxysilane, methyltrimethoxysilane, dimethylmethoxysilane or dimethylethoxysilane.
The mixed slurry comprises the following components in parts by volume: 85-95 parts of precipitated silica slurry, 1-5 parts of silane coupling agent and 3-10 parts of hydrophobic modifier.
Preferably, the mixing and stirring temperature is 20-60 ℃, and the stirring time is 5-30 minutes.
Preferably, the fiber felt is one of a glass fiber felt, a carbon fiber felt, an organic polymer fiber felt, a pre-oxidized fiber felt or a ceramic fiber felt; the density of the fiber felt is 0.05-0.15 g/cm3。
Preferably, the composite mode of the mixed slurry and the fiber felt is one of dipping and spraying.
Preferably, the drying is one of freeze drying, reduced pressure drying or atmospheric drying.
Has the advantages that:
the hydrophobic precipitated silica composite material has the following characteristics:
(1) the method has the advantages that the precipitated silica slurry is used as an initiator, the hydrophobic functionalization of the precipitated silica is realized by adding the modifier into the slurry, the damage to the structure of the precipitated silica product caused by adding the modifier into a modifier solution is avoided, the flexibility is better, the environment friendliness is better, and the method is suitable for large-scale industrial production.
(2) The composite material formed by compounding the precipitated silica slurry and the fibrofelt is used for heat insulation, so that the precipitated silica powder is prevented from being used for forming required heat insulation, the cost is greatly reduced compared with heat insulation materials such as aerogel, and the heat insulation performance is obviously improved compared with the fibrofelt.
Drawings
FIG. 1 is a graph of the hydrophobic effect of the hydrophobic precipitated silica composite prepared in example 3;
FIG. 2 is a graph showing the hydrophobic effect of the hydrophobic precipitated silica powder in the hydrophobic precipitated silica composite prepared in example 3.
Detailed Description
Example 1
An aqueous precipitated silica slurry having a mass solid content of 20% was used as a starting material (the precipitated silica slurry was spray-dried to obtain a precipitated silica powder having a bulk density of 0.12g/cm3Pore volume of 1.7cm3G, dry SiO basis2Content mass fraction 96%), and mixing 90 parts of the precipitated silica slurry with 5 parts of 3-aminopropyltriethoxysilane and 5 parts of methyltriethoxysilane at 20 deg.C for 30 min to obtain mixed slurry, and mixing the mixed slurry with a density of 0.10g/cm3The glass fiber felt is soaked and compounded, and then is frozen and dried to obtain the hydrophobic precipitated silicon dioxide composite material. The apparent density of the hydrophobic precipitated silica composite material is 0.18g/cm3The thermal conductivity at normal temperature and normal pressure is 0.024W/(m.K), the water contact angle is 100 degrees, and the thermal conductivity of the composite material relative to the glass fiber felt (0.038W/(m.K) under the same test condition) is obviously improved.
Example 2
An aqueous precipitated silica slurry having a mass solid content of 25% was used as a starting material (the precipitated silica slurry was spray-dried to obtain a precipitated silica powder having a bulk density of 0.15g/cm3Pore volume of 1.5cm3G, dry SiO basis2Content 98%) 90 portions of precipitated silica slurry, 3 portions of 3-aminopropyl trimethoxy silane and 7 portions of methyl trimethoxy silane are stirred for 5 minutes at 20 ℃ to prepare mixed slurry, and the mixed slurry and density are 0.10g/cm3Carbon fiber ofAnd (4) soaking and compounding the felt, and then drying under reduced pressure to obtain the hydrophobic precipitated silica composite material. The apparent density of the hydrophobic precipitated silica composite material is 0.20g/cm3The thermal conductivity at normal temperature and normal pressure is 0.028W/(m.K), the water contact angle is 100 degrees, and the thermal conductivity of the composite material is obviously improved compared with that of the carbon fiber felt (0.041W/(m.K) under the same test condition).
Example 3
An aqueous precipitated silica slurry having a mass solid content of 5% was used as a starting material (the bulk density of the precipitated silica powder after spray-drying of the precipitated silica slurry was 0.10g/cm3Pore volume of 2.0cm3G, dry SiO basis2Content mass fraction of 92%), using 85 portions of precipitated silica slurry, 5 portions of N-aminoethyl-gamma-aminopropyltriethoxysilane and 10 portions of dimethylethoxysilane to stir for 15 minutes at 60 ℃ to prepare mixed slurry, mixing the mixed slurry with density of 0.05g/cm3The organic polymer fiber felt is soaked and compounded, and then is frozen and dried to obtain the hydrophobic precipitated silicon dioxide composite material. The apparent density of the hydrophobic precipitated silica composite material is 0.08g/cm3The thermal conductivity at normal temperature and normal pressure is 0.030W/(m.K), the water contact angle is 135 degrees, and the thermal conductivity of the composite material relative to the organic polymer fiber felt (0.055W/(m.K) under the same test condition) is obviously improved.
Referring to the drawings, fig. 1 is a graph showing the hydrophobic effect of the hydrophobic precipitated silica composite prepared in this example, which exhibits good water non-wetting characteristics, indicating that the hydrophobic modifier plays its role.
Referring to the accompanying drawings, fig. 2 is a graph of the hydrophobic effect of the hydrophobic precipitated silica powder prepared by the example, the precipitated silica powder in the precipitated silica composite material shows good hydrophobic effect, and the water contact angle of the precipitated silica powder is about 135 degrees, which shows that the method provided by the invention can also prepare the hydrophobic modified precipitated silica powder.
Example 4
An aqueous precipitated silica slurry having a mass solid content of 20% was used as a starting material (the precipitated silica slurry was spray-dried to obtain a precipitated silica powder having a bulk density of 0.12g/cm3Pore volume of 1.7cm3/gDry basis SiO2Content mass fraction 96%), mixing 95 parts of the precipitated silica slurry with 1 part of N-aminoethyl-gamma-aminopropyltrimethoxysilane and 4 parts of dimethylmethoxysilane at 40 ℃ for 20 minutes to prepare a mixed slurry, and mixing the mixed slurry with a density of 0.15g/cm3The ceramic fiber felt is sprayed and compounded and then dried under normal pressure to obtain the hydrophobic precipitated silica composite material. The apparent density of the hydrophobic precipitated silica composite material is 0.18g/cm3The thermal conductivity at normal temperature and normal pressure is 0.032W/(m.K), the water contact angle is 125 degrees, and the thermal conductivity of the composite material (0.046W/(m.K) under the same test condition) is obviously improved compared with that of the ceramic fiber felt.
Example 5
An aqueous precipitated silica slurry having a mass solid content of 15% as a starting material (the precipitated silica slurry after spray-drying has a bulk density of precipitated silica powder of 0.12g/cm3Pore volume of 1.8cm3G, dry SiO basis294 percent by mass), mixing 94 parts of the precipitated silica slurry, 3 parts of 3-aminopropyltriethoxysilane and 3 parts of dimethylethoxysilane at 20 ℃ for 30 minutes to prepare mixed slurry, and mixing the mixed slurry with the density of 0.10g/cm3And after the pre-oxidized fiber felt is sprayed and compounded, freezing and drying to obtain the hydrophobic precipitated silicon dioxide composite material. The apparent density of the hydrophobic precipitated silica composite material is 0.15g/cm3The thermal conductivity at normal temperature and normal pressure is 0.028W/(m.K), the water contact angle is 105 degrees, and the thermal conductivity of the composite material is obviously improved compared with that of the pre-oxidized fiber felt (0.040W/(m.K) under the same test condition).
Claims (10)
1. The preparation method of the hydrophobic precipitated silica composite material is characterized by comprising the following steps:
mixing and stirring the water-based precipitated silica slurry, the silane coupling agent and the hydrophobic modifier to prepare mixed slurry, then compounding the mixed slurry with the fibrofelt, and finally drying to obtain the hydrophobic precipitated silica composite material.
2. The method according to claim 1, wherein the hydrophobic precipitated silica composite has an apparent density of 0.08-0.20 g/cm3The thermal conductivity is 0.024-0.032W/(m.K), and the water contact angle is 100-135 deg.
3. The method according to claim 1, wherein the aqueous precipitated silica slurry has a mass solid content of 5 to 25%.
4. The method according to claim 1, wherein the silane coupling agent is one of 3-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, N-aminoethyl- γ -aminopropyltriethoxysilane, and N-aminoethyl- γ -aminopropyltrimethoxysilane.
5. The method of claim 1, wherein the hydrophobic modifier is one of methyltriethoxysilane, methyltrimethoxysilane, dimethylmethoxysilane, or dimethylethoxysilane.
6. The preparation method according to claim 1, wherein the mixed slurry comprises the following components in parts by volume: 85-95 parts of precipitated silica slurry, 1-5 parts of silane coupling agent and 3-10 parts of hydrophobic modifier.
7. The preparation method according to claim 1, wherein the temperature of the mixing and stirring is 20 to 60 ℃ and the stirring time is 5 to 30 minutes.
8. The preparation method according to claim 1, wherein the fiber mat is one of a glass fiber mat, a carbon fiber mat, an organic polymer fiber mat, a pre-oxidized fiber mat or a ceramic fiber mat; the density of the fiber felt is 0.05-0.15 g/cm3。
9. The method of claim 1, wherein the mixed slurry is combined with the fiber mat by one of dipping and spraying.
10. The method of claim 1, wherein the drying is one of freeze drying, drying under reduced pressure, or drying under atmospheric pressure.
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| US20110206471A1 (en) * | 2009-11-25 | 2011-08-25 | Cabot Corporation | Aerogel Composites and Methods for Making and Using Them |
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- 2020-01-14 CN CN202010034397.1A patent/CN111188188A/en active Pending
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Application publication date: 20200522 |
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