CN107266774A - A kind of aerogel composite and preparation method thereof - Google Patents
A kind of aerogel composite and preparation method thereof Download PDFInfo
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- CN107266774A CN107266774A CN201610214830.3A CN201610214830A CN107266774A CN 107266774 A CN107266774 A CN 107266774A CN 201610214830 A CN201610214830 A CN 201610214830A CN 107266774 A CN107266774 A CN 107266774A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
Abstract
The invention discloses a kind of aerogel composite and preparation method thereof, it is characterised in that is mainly made up of aerogel powder and PUR, and the aerogel powder is nano-porous structure in the PUR.The preparation method of the aerogel composite of the present invention comprises the following steps：（1）The aerogel powder is mixed with the PUR powder, mechanical agitation；（2）To step（1）Dry mixture carry out it is hot-forming.Aerogel powder is nano-porous structure in the aerogel composite of the present invention, and with excellent thermal and insulating performance and mechanical property, market application foreground is huge.
Description
Technical field
The present invention relates to a kind of insulation material, more particularly to a kind of aerogel composite and preparation method thereof, belong to the fields such as lightweight, thermal insulation, acoustic material.
Background technology
Aeroge be it is a kind of by nano-scale particle accumulation form, the lightweight solid material with nanoscale hole hole, with high porosity, specific surface area, extremely low density and solid content, chemical inertness and noninflammability, excellent lightweight, insulation, fire prevention, sound insulation, damping energy absorption characteristics are shown, the civil area such as the military fields such as defence and military, security anti-terrorism and green building, heat transmission, public transport, finance device protection is can be widely applied to.
However, just because of the intrinsic defect of aeroge, such as low intensity, fragility is big, therefore, on the premise of aeroge nano-porous structure is not destroyed, aeroge is combined with other materials, it is expected to improve the mechanical property of aeroge and composite.
The content of the invention
For above-mentioned technical problem, the present invention proposes a kind of aerogel composite and preparation method thereof.
A kind of aerogel composite, is mainly made up of aerogel powder and PUR, and the aerogel powder is nano-porous structure in the PUR.
In one of the embodiments, the PUR is the one or more in ethylene-vinyl acetate copolymer powder, ethylene ethyl acrylate copolymer powder, polyvinyl alcohol powder, polyethylene powder, polyvinyl chloride powder, polyurethane powder.
A kind of preparation method of aerogel composite, comprises the following steps：
（1）The aerogel powder is mixed with the PUR powder, mechanical agitation；
（2）To step（1）Dry mixture carry out it is hot-forming.
In one of the embodiments, the step（1）Phase-changing energy storage material, fire retardant, other insulation materials can also be added.
In one of the embodiments, the phase-changing energy storage material is the one or more in the inorganic water and salt, higher aliphatic hydrocarbon, polyalcohol, multi-hydroxy carboxy acid of microcapsule coated；The fire retardant is carbon forming agent, foaming agent, catalyst；The carbon forming agent is the one or more in pentaerythrite, starch, dipentaerythritol, erythrol, sorbierite, inositol；The foaming agent is the one or more in melamine, urea, polyamide, dicyandiamide, chlorinated paraffin, polyureas, melamine, glycine；The catalyst is the one or more in APP, ammonium hydrogen carbonate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium sulfate, formic acid；The fire retardant also includes the one or more in magnesium hydroxide, modified magnesium hydroxide, aluminium hydroxide, modified aluminium hydroxide, borax.
In one of the embodiments, the step（1）The preceding hydrophobically modified step including aerogel powder.
In one of the embodiments, the hydrophobically modified is to carry out hydrophobically modified to aerogel powder in closed hydrophobic modifier gaseous environment.
In one of the embodiments, the hydrophobic modifier be trim,ethylchlorosilane, HMDS, HMDO, MTMS, MTES, dimethyldimethoxysil,ne, dimethyldiethoxysilane, γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-（The oxygen of 2,3- epoxies third）Propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, N-（β-aminoethyl）One or more mixtures in-gamma-aminopropyl-triethoxy-silane.
In one of the embodiments, the step（2）In hot-forming temperature be 50 ~ 300 DEG C, pressure is 0.01 ~ 100MPa, and processing time is 10 ~ 300min.
A kind of thermal conductivity factor of above-mentioned aerogel composite is 0.015 ~ 0.035 W/mK, with excellent mechanical property, and surface not dry linting, application prospect is extensive.
Embodiment
In order to facilitate the understanding of the purposes, features and advantages of the present invention, the embodiment below to the present invention is described in detail.Many details are elaborated in the following description to fully understand the present invention.But the invention can be embodied in many other ways as described herein, those skilled in the art can make similar improvements without departing from the spirit of the invention, therefore the present invention is not limited to the specific embodiments disclosed below.
A kind of embodiment of the aerogel composite of the present invention, is mainly made up of aerogel powder and PUR, and the aerogel powder is nano-porous structure in the PUR.
In this way, the aerogel composite of the present invention provides the performance such as insulation, heat-insulated, sound insulation by filler of aerogel powder, mechanical property is provided by matrix of PUR.
In the present embodiment, the PUR is the one or more in ethylene-vinyl acetate copolymer powder, ethylene ethyl acrylate copolymer powder, polyvinyl alcohol powder, polyethylene powder, polyvinyl chloride powder, polyurethane powder.
In this way, different PURs has different physical and chemical performance and mechanical property, a kind of PUR or a variety of PURs is selected to compound according to application demand so that aerogel composite performance and application variation.
A kind of preparation method of aerogel composite, comprises the following steps：
（1）The aerogel powder is mixed with the PUR powder, mechanical agitation；
（2）To step（1）Dry mixture carry out it is hot-forming.
In addition, step（1）The mass ratio of middle aerogel powder and PUR powder can be 1:(0.1 ~ 10), step（1）In can also add the insulation materials such as glass bead, expanded perlite, ceramic fine bead, expanded polystyrene particle, polyurathamc particle, the particle diameter of aerogel powder can be 0.01 ~ 20mm, and the particle diameter of PUR powder can be 10 ~ 200 μm；Step（2）In by using technique, so that PUR has certain viscosity and mobility, by regulating and controlling hot pressing parameterses, adjust the viscosity of PUR, PUR is controlled to enter the porous speed of aerogel powder nano surface, so that aerogel powder has good interface cohesion with PUR, and ensure that the most nano-porous structure of aeroge retains.
In this way, the preparation method technique of the aerogel composite of the present invention is simple, and it is practical, it is cheap, it is adapted to industrialized production.
In one of the embodiments, the step（1）Phase-changing energy storage material, fire retardant can also be added.
In one of the embodiments, the phase-changing energy storage material is the one or more in the inorganic water and salt, higher aliphatic hydrocarbon, polyalcohol, multi-hydroxy carboxy acid of microcapsule coated；The fire retardant is carbon forming agent, foaming agent, catalyst；The carbon forming agent is the one or more in pentaerythrite, starch, dipentaerythritol, erythrol, sorbierite, inositol；The foaming agent is the one or more in melamine, urea, polyamide, dicyandiamide, chlorinated paraffin, polyureas, melamine, glycine；The catalyst is the one or more in APP, ammonium hydrogen carbonate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium sulfate, formic acid；The fire retardant also includes the one or more in magnesium hydroxide, modified magnesium hydroxide, aluminium hydroxide, modified aluminium hydroxide, borax.
So, phase-changing energy storage material can be absorbed or be discharged a large amount of heat energy by phase transformation, with energy storage effect, when the aerogel composite of the present invention is used for building masonry wall, architecture indoor temperature can be adjusted, comfortable quality of building is improved, the energy is saved, also, the linear contraction value of aerogel composite of the present invention can be reduced by adding phase-changing energy storage material；Carbon forming agent, foaming agent and catalyst are added into aerogel composite so that aerogel composite meets fire expansion, Surface Creation foam layer of charcoal, trap heat is transmitted to base material；Due to the dehydration endothermic reaction can occur when magnesium hydroxide, aluminium hydroxide, borax etc. are heated, therefore into aerogel composite, addition magnesium hydroxide, aluminium hydroxide, borax etc. can extend the time that heat is transmitted to base material, improve fire endurance.
In the present embodiment, the step（1）The preceding hydrophobically modified step including aerogel powder.
So, because in existing aeroge preparation method, precursor, displacement solvent and drying process have significant effect to the hydrophobicity of aeroge, if the surface of aeroge and the contact angle of water are more than 90 °, hydrophobically modified can not be carried out in advance, directly carry out surface hydrophilic modification；If the surface of aeroge and the contact angle of water are less than 90 °, need to carry out hydrophobically modified in advance.
In the present embodiment, the hydrophobically modified is to carry out hydrophobically modified to aerogel powder in closed hydrophobic modifier gaseous environment.
So, hydrophobically modified, the modified effect except significantly improving aerogel powder are carried out to aerogel powder in closed hydrophobic modifier gaseous environment, it is ensured that inside nano-porous structure is not destroyed outer during follow-up hydrophilic modifying, modification efficiency and production efficiency are also significantly improved, production cost is reduced.
In the present embodiment, the hydrophobic modifier be trim,ethylchlorosilane, HMDS, HMDO, MTMS, MTES, dimethyldimethoxysil,ne, dimethyldiethoxysilane, γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-（The oxygen of 2,3- epoxies third）Propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, N-（β-aminoethyl）One or more mixtures in-gamma-aminopropyl-triethoxy-silane.
In this way, different hydrophobic modifiers has different reactivities from aeroge, the present invention improves modification efficiency and modified effect by selecting one or more hydrophobic modifiers to be modified aerogel powder.
In the present embodiment, the step（2）In hot-forming temperature be 50 ~ 300 DEG C, pressure is 0.01 ~ 100MPa, and processing time is 10 ~ 300min.
In this way, by carrying out hot-forming processing to the dry blend that aerogel powder and PUR powder are constituted so that aerogel powder is bonded together by PUR, retains the nano-porous structure of aeroge, improves the mechanical property of aerogel composite.
The thermal conductivity factor of above-mentioned aerogel composite is 0.015 ~ 0.035 W/mK, with excellent mechanical property, not dry linting, and application prospect is extensive.
It is specific embodiment part below.
Embodiment 1
SiO is prepared using following steps2Aerogel composite：
（1）Pending SiO is detected using contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 55 °, are then 56 μm of SiO by particle diameter2Aerogel powder is positioned in vacuum furnace, the HMDS after weighing is positioned in vacuum furnace with container, heating and gasifying, and hydrophobically modified 1.5h obtains hydrophobic SiO2Aerogel powder, hydrophobic SiO is detected with contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 147 °；
（2）In mass ratio 1:1 by step（1）Aerogel powder, aluminium hydroxide powder mixed with EVA hot-melt adhesive powder, mechanical agitation 30min, stir speed (S.S.) be 1500 turns/min；
（3）To step（2）Dry mixture hot-pressing processing, temperature be 105 DEG C, pressure is 1MPa, and the time is 20min, obtains SiO2Aerogel composite.Table 1 is SiO made from the present embodiment2The performance indications of aerogel composite.
The SiO of table 12The performance indications of aerogel composite
Embodiment 2
SiO is prepared using following steps2Aerogel composite：
（1）Pending SiO is detected using contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 45 °, then by SiO of the particle diameter for 12mm2Aerogel powder is positioned in vacuum furnace, the trim,ethylchlorosilane after weighing is positioned in vacuum furnace with container, heating and gasifying, and hydrophobically modified 1.5h obtains hydrophobic SiO2Aerogel powder, hydrophobic SiO is detected with contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 146 °；
（2）In mass ratio 1:0.5 weighs step（1）Obtained SiO2Aerogel powder, microcapsule coated octadecane and EAA PUR mechanical agitation 10min, stir speed (S.S.) are 1500 turns/min；
（3）To step（2）Dry mixture hot-pressing processing, temperature be 110 DEG C, pressure is 0.1MPa, and the time is 20min, obtains SiO2Aerogel composite.Table 2 is SiO made from the present embodiment2The performance indications of aerogel composite.
The SiO of table 22The performance indications of aerogel composite
Embodiment 3
SiO is prepared using following steps2Aerogel composite：
（1）Pending SiO is detected using contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 45 °, then by SiO of the particle diameter for 0.1mm2Aerogel powder is positioned in vacuum furnace, the HMDS after weighing is positioned in vacuum furnace with container, heating and gasifying, and hydrophobically modified 1.5h obtains hydrophobic SiO2Aerogel powder, hydrophobic SiO is detected with contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 141 °；
（2）In mass ratio 1:1 weighs step（1）SiO2Aerogel powder and the mixing of PU PURs, mechanical agitation 30min, stir speed (S.S.) is 1000 turns/min；
（3）To step（2）Dry mixture carry out hot-pressing processing, temperature be 190 DEG C, pressure is 20MPa, and the time is 15min, obtains SiO2Aerogel composite.Table 3 is SiO made from the present embodiment2The performance indications of aerogel composite.
The SiO of table 32The performance indications of aerogel composite
Embodiment 4
SiO is prepared using following steps2Aerogel composite：
（1）The SiO that pending particle diameter is 77 μm is detected using contact angle measurement2Aerogel powder surface and the contact angle of water, testing result are 140 °, then the SiO2Aerogel powder has hydrophobicity；
（2）In mass ratio 1:0.8 weighs step（1）SiO2Aerogel powder and the mixing of PVA PURs, mechanical agitation 30min, stir speed (S.S.) is 1500 turns/min；
（3）To step（2）Dry mixture carry out hot-pressing processing, temperature be 100 DEG C, pressure is 10MPa, and the time is 15min, obtains SiO2Aerogel composite.Table 4 is SiO made from the present embodiment2The performance indications of aerogel composite.
The SiO of table 42The performance indications of aerogel composite
Above-described embodiment is the present invention preferably embodiment; but embodiments of the present invention are simultaneously not restricted to the described embodiments; other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification; equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (9)
1. a kind of aerogel composite, it is characterised in that be mainly made up of aerogel powder and PUR, the aerogel powder is nano-porous structure in the PUR.
2. a kind of aerogel composite according to claim 1, characterized in that, the PUR is the one or more in ethylene-vinyl acetate copolymer powder, ethylene ethyl acrylate copolymer powder, polyvinyl alcohol powder, polyethylene powder, polyvinyl chloride powder, polyurethane powder.
3. the preparation method of the aerogel composite according to foregoing any claim, it is characterised in that comprise the following steps：
（1）The aerogel powder is mixed with the PUR powder, mechanical agitation；
（2）To step（1）Dry mixture carry out it is hot-forming.
4. a kind of preparation method of aerogel composite according to claim 3, it is characterised in that the step（1）Phase-changing energy storage material, fire retardant, other insulation materials can also be added.
5. a kind of preparation method of aerogel composite according to claim 4, it is characterised in that the phase-changing energy storage material is the one or more in the inorganic water and salt, higher aliphatic hydrocarbon, polyalcohol, multi-hydroxy carboxy acid of microcapsule coated；The fire retardant is carbon forming agent, foaming agent, catalyst；The carbon forming agent is the one or more in pentaerythrite, starch, dipentaerythritol, erythrol, sorbierite, inositol；The foaming agent is the one or more in melamine, urea, polyamide, dicyandiamide, chlorinated paraffin, polyureas, melamine, glycine；The catalyst is the one or more in APP, ammonium hydrogen carbonate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium sulfate, formic acid；The fire retardant also includes the one or more in magnesium hydroxide, modified magnesium hydroxide, aluminium hydroxide, modified aluminium hydroxide, borax.
6. a kind of preparation method of aerogel composite according to claim 3, it is characterised in that the step（1）The preceding hydrophobically modified step including aerogel powder.
7. a kind of preparation method of aerogel composite according to claim 6, it is characterised in that the hydrophobically modified step is to carry out hydrophobically modified to aerogel powder in closed hydrophobic modifier gaseous environment.
8. a kind of preparation method of aerogel composite according to claim 7, characterized in that, the hydrophobic modifier be trim,ethylchlorosilane, HMDS, HMDO, MTMS, MTES, dimethyldimethoxysil,ne, dimethyldiethoxysilane, γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-（The oxygen of 2,3- epoxies third）Propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, N-（β-aminoethyl）One or more in-gamma-aminopropyl-triethoxy-silane.
9. a kind of preparation method of aerogel composite according to claim 3, it is characterised in that the step（2）In hot-forming temperature be 50 ~ 300 DEG C, pressure is 0.01 ~ 100MPa, and processing time is 10 ~ 300min.
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| CN109385254A (en) * | 2018-11-26 | 2019-02-26 | 同济大学 | A kind of graphene elastomeric polymer phase change composite material and preparation method thereof |
| CN111154167A (en) * | 2019-03-18 | 2020-05-15 | 罗瑞尔纳米合成材料(江苏)有限公司 | Heat-insulating polyethylene composite material and preparation method thereof |
| CN111269557A (en) * | 2020-04-14 | 2020-06-12 | 烟台恒诺新材料有限公司 | Preparation method of hollow nano microsphere modified high-molecular heat-insulation material |
| CN111619192A (en) * | 2019-02-27 | 2020-09-04 | 南通市通州区先锋誉佳衬布厂 | Composite material containing aerogel, composite fabric and preparation method of composite material |
| CN111825901A (en) * | 2019-04-15 | 2020-10-27 | 江苏泛亚微透科技股份有限公司 | Silicon dioxide aerogel flexible elastic heat insulation composite material and preparation method thereof |
| WO2021057846A1 (en) * | 2019-09-26 | 2021-04-01 | 广州恩沣新材料科技有限公司 | Aerogel eva light-weight breathable and thermal insulation composite material and preparation method therefor |
| CN112796114A (en) * | 2020-12-04 | 2021-05-14 | 卿星 | Method for modifying textile through low-temperature melting and bonding of composite powder |
| CN114804818A (en) * | 2022-05-24 | 2022-07-29 | 巩义市泛锐熠辉复合材料有限公司 | Low-cost aerogel composite material and preparation method thereof |
| CN116120620A (en) * | 2023-03-07 | 2023-05-16 | 北京清冠科技有限公司 | Preparation method of low-density aerogel/polyvinyl chloride foam composite material |
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| CN111619192A (en) * | 2019-02-27 | 2020-09-04 | 南通市通州区先锋誉佳衬布厂 | Composite material containing aerogel, composite fabric and preparation method of composite material |
| CN111154167A (en) * | 2019-03-18 | 2020-05-15 | 罗瑞尔纳米合成材料(江苏)有限公司 | Heat-insulating polyethylene composite material and preparation method thereof |
| CN111825901A (en) * | 2019-04-15 | 2020-10-27 | 江苏泛亚微透科技股份有限公司 | Silicon dioxide aerogel flexible elastic heat insulation composite material and preparation method thereof |
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| CN111269557A (en) * | 2020-04-14 | 2020-06-12 | 烟台恒诺新材料有限公司 | Preparation method of hollow nano microsphere modified high-molecular heat-insulation material |
| CN112796114A (en) * | 2020-12-04 | 2021-05-14 | 卿星 | Method for modifying textile through low-temperature melting and bonding of composite powder |
| CN114804818A (en) * | 2022-05-24 | 2022-07-29 | 巩义市泛锐熠辉复合材料有限公司 | Low-cost aerogel composite material and preparation method thereof |
| CN114804818B (en) * | 2022-05-24 | 2023-04-11 | 巩义市泛锐熠辉复合材料有限公司 | Low-cost aerogel composite material and preparation method thereof |
| CN116120620A (en) * | 2023-03-07 | 2023-05-16 | 北京清冠科技有限公司 | Preparation method of low-density aerogel/polyvinyl chloride foam composite material |
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