CN113462078A - Aerogel composite foaming sheet, preparation method and application - Google Patents

Aerogel composite foaming sheet, preparation method and application Download PDF

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CN113462078A
CN113462078A CN202110795922.6A CN202110795922A CN113462078A CN 113462078 A CN113462078 A CN 113462078A CN 202110795922 A CN202110795922 A CN 202110795922A CN 113462078 A CN113462078 A CN 113462078A
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aerogel
sheet
foaming
foamed sheet
parts
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张鑫
魏琼
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Hubei Xiangyuan New Material Technology Inc
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Hubei Xiangyuan New Material Technology Inc
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Abstract

The invention discloses an aerogel composite foaming sheet, a preparation method and application, and belongs to the field of aerogel materials. When the wet gel composite foaming sheet is prepared, the prepared aerogel sol is uniformly sprayed on the section of the foaming sheet, the foaming sheet is kept stand for 5 to 10 hours at the temperature of between 50 and 70 ℃ to convert the aerogel sol into gel, so that the wet gel composite foaming sheet is obtained, and the prepared wet gel composite foaming sheet is dried in a drying device at the temperature of between 80 and 100 ℃ for 10 to 60 minutes, so that the aerogel composite foaming sheet is obtained. The invention can solve the problems of poor mechanical property, higher brittleness, infirm combination between composite layers and unsatisfactory heat and moisture insulation effect of the existing aerogel felt.

Description

Aerogel composite foaming sheet, preparation method and application
Technical Field
The invention belongs to the field of aerogel materials, and particularly relates to an aerogel composite foaming sheet, a preparation method and application.
Background
The aerogel is a continuous open pore, high porosity (80-99.9%), low density (-0.03 g/cm)3) The novel nano material has the advantages that the unique space network structure of the aerogel is filled with air, the heat conductivity coefficient is extremely low, and the novel nano material has a very wide application prospect in the field of heat preservation and insulation. The skeleton that constitutes aerogel network structure is thinner, receives the fracture of easy fracture when exogenic action, so aerogel mechanical properties is poor, and the fragility is higher, and the in-service use receives the restriction.
The skeleton that constitutes aerogel network structure is thinner, receives the fracture of easy fracture when exogenic action, so aerogel mechanical properties is poor, and the fragility is higher, and the in-service use receives the restriction, uses aerogel and other material composite maximum performance aerogel advantage that insulates against heat, is the development trend that the aerogel was used.
At present, the commercially available aerogel heat insulation product is mainly aerogel felt, is formed by compounding aerogel and fiber serving as a reinforcing structure, and has the following problems in the application process:
1. the fiber structure is far larger than the pore size of the aerogel, so that aerogel powder is easy to fall off from the surface, and the product cannot be well attached to other materials;
2. in order to enable the sol to permeate into the material in the preparation process, the material structure is mostly a through hole structure, and the hydrophobic modification can not effectively isolate water vapor. Once water enters the heat insulation device during use, the heat insulation effect is remarkably reduced.
In view of the above-mentioned deficiencies in the prior art, there is a need for an aerogel composite material and a preparation method with a simple process, which can fully exert the excellent properties of aerogel materials.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an aerogel composite foaming sheet, a preparation method and application, and aims to solve the problems that the existing aerogel felt is poor in mechanical property, high in brittleness, not firm in combination between composite layers and not ideal in heat insulation and moisture insulation effects.
In order to achieve the above object, the present invention provides an aerogel composite foamed sheet, which comprises a foamed sheet layer and an aerogel layer, wherein the aerogel layer is attached to a cutting plane of the foamed sheet layer, the foamed sheet is a closed-cell foamed sheet, and the cutting plane naturally forms a large number of concave cell grid structures after being cut, so that the surface area of the cutting plane can be greatly increased.
Further, the foamed sheet has an average pore diameter of 30 to 300. mu.m.
Further, the number of open cells per square centimeter on the cutting surface of the foamed sheet is 103To 106And (4) respectively.
Further, the proportion of the number of the cells with the diameter of less than 10 microns and the diameter of more than 300 microns on the section plane of the foaming sheet in the total number of the cells is less than 50%, and the proportion of the number of the cells with the diameter of 30 microns to 300 microns on the section plane of the foaming sheet in the total cells is more than 50%.
Furthermore, the volume occupied by the open cells on the cutting surface of the foamed sheet per square centimeter is 10-4cm3～10-3cm3。
Further, the aerogel sol is uniformly attached to a cut surface of the foamed sheet, which is attached theretoHas a mass of 5g/m2～100g/m2。
According to the second aspect of the present invention, there is also provided a method for preparing an aerogel composite foamed sheet, comprising the step S3:
uniformly spraying the prepared aerogel sol on a section of a foaming sheet, standing for 5-10 h at the temperature of 50-70 ℃ to convert the aerogel sol into gel to obtain a wet gel foaming sheet composite material, and drying the prepared wet gel foaming sheet composite material in a drying device at the temperature of 80-100 ℃ for 10-60 min to obtain the aerogel composite foaming sheet.
Further, the method also comprises the following steps:
s1: preparing a foamed sheet, specifically, weighing 50-90 parts by weight of resin, 1-10 parts by weight of foaming agent, 0.1-0.5 part by weight of opacifier, 1-3 parts by weight of flame retardant and 1-5 parts by weight of white carbon black, uniformly mixing in an internal mixer at 120-160 ℃ to prepare the sheet, irradiating the prepared sheet to generate crosslinking, foaming at a high temperature of 200-280 ℃, cooling to obtain the foamed sheet, cutting the foamed sheet into thin foamed sheets with a specified thickness by using cutting equipment,
s2: the preparation method comprises the steps of weighing 5-10 parts by weight of an aerogel silicon source, 10-35 parts by weight of deionized water and 10-35 parts by weight of ethanol, uniformly stirring in a stirring kettle, adding an acidic catalyst to adjust the pH value to 3-4, continuously stirring for 10-60 min, adding an alkaline catalyst to adjust the pH value to 7-8, and continuously stirring uniformly to prepare the aerogel sol.
Further, in step S1, the resin is selected from one or more of the following: one or more of polystyrene, polyurethane, polyvinyl chloride, polyethylene, polypropylene, ethylene-vinyl acetate copolymer, ethylene propylene diene monomer, nitrile butadiene rubber, natural rubber, polyvinyl formal, cellulose acetate, polymethyl methacrylate, polychlorinated or sulfonated polyethylene, polycarbonate, polyimide. The foaming agent is selected from azodimethyl phthalein amine (foaming agent AC), N '-dinitrosopentamethylenetetramine (foaming agent H), 4' -oxybis-benzenesulfonylhydrazide (OBSH), sodium bicarbonate, and ureaOne or more opacifiers including SiC and Al2O3、TiO2、ZrO2One or more of them. The flame retardant is Sb2O3、Al(OH)3、Mg(OH)2One or more of red phosphorus, expandable graphite and ammonium polyphosphate. The white carbon black is one or more of hydrophobic white carbon black and hydrophilic white carbon black. The silicon source is one or more of Tetraethoxysilane (TEOS), methyl orthosilicate (TMOS), Methyltriethoxysilane (MTES), methyltrimethoxysilane (MTMS), Polysiloxane (PEDS), silsesquioxane (POSS) and Trimethylchlorosilane (TMCS). The acid catalyst is 0.5-1 mol/L hydrochloric acid, and the alkaline catalyst is 10-20% ammonia water by mass concentration.
According to a third aspect of the present invention, there is also provided a use of the aerogel composite foamed sheet as described above, in the field of heat preservation and insulation in the building field, or in the field of heat insulation in the electronic equipment field.
Generally, compared with the prior art, the above technical solution conceived by the present invention has the following beneficial effects:
(1) the foamed sheet is a closed-cell foamed sheet, the closed-cell foamed sheet has an independent cell structure, and the cells are separated by a wall membrane, so that the foamed sheet has excellent buffering, sound-insulating and heat-insulating properties and can effectively isolate water vapor. The foaming sheet needs to be cut into a thin foaming sheet with a specified thickness in parallel to the surface, then the thin foaming sheet is subjected to a compounding process with aerogel, and the cut foaming sheet is compounded with the aerogel to prepare the aerogel composite foaming sheet. The sectioning surface naturally forms a large number of concave cellular grid structures after being sectioned, so that the surface area of the sectioning surface can be greatly increased, the combination of the foaming sheet and the aerogel is naturally and tightly realized by adopting the natural structure, meanwhile, the cellular grid structure is used as a toughening framework of the aerogel layer, the aerogel layer formed in the cellular grid structure can be protected from being easily damaged in the production and use processes, the combination between composite layers is firm, and the composite foaming sheet is more durable in use.
(2) The average pore diameter of the foamed sheet is preferably from 30 μm to 300. mu.m, in this range of pore diameters, on the one hand, owing to the porosity of the foamed sheet layerThe structure can be fine play the buffering effect, receives the exogenic action and can protect aerogel and the cotton composite bed structure of bubble not destroyed. On the other hand, due to the independent cell structure, the heat conductivity of air in the cell is very low, and the heat insulation performance is good. The number of open cells per square centimeter on the section surface of the foamed sheet is 103An6The number of the cells per unit area influences the diameter of the cells and the surface area of a cell wall film, the more the number of the cells in the unit area is, the larger the surface area of the cell wall combined with the aerogel is, the more compact the combination between the cells is, but the too large number of the cells in the unit area can cause the undersize of the average cell diameter, the aerogel sol is not favorably permeated into the cells, the number of the open cells per square centimeter on the section surface of the foaming sheet is 103An6In addition, the aerogel and the foaming sheet can be well combined.
(3) The proportion of the number of the cells with the diameter of less than 10 microns and the diameter of more than 300 microns on the section plane of the foaming sheet in the total cells is less than 50%, the proportion of the number of the cells with the diameter of 30 microns-300 microns on the section plane of the foaming sheet in the total cells is more than 50%, the cells with the too small diameter are not beneficial to the permeation of aerogel sol, when the diameter of the cells is too large, aerogel in the cells is easy to break and fall off in the using process, the proportion of the number of the cells with the diameter of less than 10 microns and the diameter of more than 300 microns in the total cells needs to be limited in a proper range, and when the diameter of the cells is 30 microns-300 microns, the aerogel sol is beneficial to rapidly permeate and soak into the cells.
(4) The volume of the open cells on the cutting plane of the foamed sheet per square centimeter is 10-4cm3～10-3cm3The volume occupied by the open cells influences the quality of the foamed sheet material capable of compounding the aerogel, the volume occupied by the open cells is too small, the quality of the foamed sheet material compounded aerogel is low, and the heat conductivity coefficient of the foamed sheet material is too high to meet the heat insulation requirement. The open cells occupy too large a volume, and too much sol enters the interior of the cells to affect the drying speed of the aerogel.
(5) The method for preparing the aerogel foaming sheet material has the advantages of mature technology, convenient material obtaining, low cost, controllable spraying amount and easy actual engineering production.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing an aerogel composite foamed sheet according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides an aerogel composite foaming sheet which comprises a foaming sheet layer and an aerogel layer, wherein the aerogel layer is attached to the cutting surface of the foaming sheet layer. The foamed sheet is a closed-cell foamed sheet, the closed-cell foamed sheet has an independent cell structure, and the cells are separated by a wall membrane, so that the foamed sheet has excellent buffering, sound-insulating and heat-insulating properties and can effectively isolate water vapor. The average pore diameter of the foamed sheet is preferably 30 to 300. mu.m. In the pore diameter range, on one hand, the porous structure of the foaming sheet layer can well play a role in buffering, and the aerogel and foam composite layer structure can be protected from being damaged when the porous structure of the foaming sheet layer is acted by external force. On the other hand, due to the independent cell structure, the heat conductivity of the air in the cell is very small, and the cell has good heat insulation performance.
The foaming sheet needs to be cut into a thin foaming sheet with a specified thickness in parallel to the surface, then the thin foaming sheet is subjected to a compounding process with aerogel, and the cut foaming sheet is compounded with the aerogel to prepare the aerogel composite foaming sheet. The foam sheet material cutting plane has a large amount of sunken cell structures, greatly increased the surface area of cutting plane, made the combination of bubble cotton and aerogel inseparabler, its cell grid structure can regard as the skeleton of toughening of aerogel simultaneously, the protection aerogel that forms in cell grid structure makes it difficult destroyed in production and use.
As a preferable mode of the present invention, the number of open cells per square centimeter in the cut surface of the foamed sheet is 103To 106The number of cells per unit area affects the diameter and cell walls of the cellsThe greater the surface area of the film, the greater the number of cells per unit area, the greater the surface area of the cell walls associated with the aerogel, and the tighter the association between the two. However, too much number of cells per unit area will result in too small average cell diameter, which is not favorable for aerogel sol to permeate into the cells, and the number of cells opened per square centimeter on the section plane of the foamed sheet is 103To 106In addition, the aerogel and the foaming sheet can be well combined.
As a preferable mode of the present invention, the number of cells having a diameter of less than 10 μm and a diameter of more than 300 μm in a cross-sectional plane of the foamed sheet should be less than 50% in the total cells, and the number of cells having a diameter of 30 μm to 300 μm in a cross-sectional plane of the foamed sheet should be more than 50% in the total cells. The cells with too small diameters are not beneficial to the permeation of aerogel sol, and when the cell diameters are too large, the aerogel in the cells is easy to be damaged and fall off in the using process. The ratio of the number of cells having a diameter of less than 10 μm and a diameter of more than 300 μm to the total cells needs to be limited to a suitable range, and the cells having a diameter of 30 to 300 μm facilitate rapid infiltration of the aerogel sol into the interior of the cells.
As a preferable mode of the present invention, the volume occupied by the open cells per square centimeter section of the foamed sheet is 10-4cm3-10-3cm3The volume of the open cells affects the quality of the composite aerogel of the foamed sheet, and the mass of the composite aerogel of the foamed sheet is small when the volume of the open cells is too small, so that the thermal conductivity coefficient of the composite sheet is too high to meet the heat insulation requirement; the open cells occupy too large a volume, and too much sol enters the interior of the cells to affect the drying speed of the aerogel.
Fig. 1 is a schematic flow chart of a method for preparing an aerogel composite foamed sheet according to the present invention, and it can be seen that the method for preparing an aerogel composite foamed sheet according to the present invention specifically includes the following steps:
a: a foamed sheet was prepared as follows,
weighing 50-90 parts of resin, 1-10 parts of foaming agent, 0.1-0.5 part of light-shading agent, 1-3 parts of flame retardant and 1-5 parts of white carbon black in parts by weight; the method comprises the following steps of uniformly mixing the materials in an internal mixer set to be 120-160 ℃ to prepare a sheet, irradiating the prepared sheet to be crosslinked, foaming at a high temperature of 200-280 ℃, cooling to obtain a foamed sheet, and cutting the foamed sheet into a thin foamed sheet with a specified thickness by using cutting equipment.
B: the aerogel sol was prepared as follows,
weighing 5-10 parts of aerogel silicon source, 10-35 parts of deionized water and 10-35 parts of ethanol in parts by weight, uniformly stirring in a stirring kettle, adding an acidic catalyst to adjust the pH to 3-4, continuously stirring for 10-60 min, adding an alkaline catalyst to adjust the pH to 7-8, and continuously stirring uniformly to prepare aerogel sol.
C: and uniformly spraying the prepared aerogel sol on a section of the foaming sheet, standing for 5-10 hours at the temperature of 50-70 ℃ to convert the aerogel sol into gel, and thus obtaining the wet gel foaming sheet composite material.
D: and drying the prepared wet gel foaming sheet composite material to obtain the aerogel composite foaming sheet, wherein the drying mode of the wet gel foaming sheet composite material is drying for 10-60 min in a drying device at the temperature of 80-100 ℃.
As a preferable scheme of the invention, the resin is one or more of polystyrene, polyurethane, polyvinyl chloride, polyethylene, polypropylene, ethylene-vinyl acetate copolymer, ethylene propylene diene monomer, nitrile butadiene rubber, natural rubber, polyvinyl formal, cellulose acetate, polymethyl methacrylate, polychlorinated or sulfonated polyethylene, polycarbonate and polyimide; the foaming agent is one or more of azodicarbonamide (foaming agent AC), N '-dinitrosopentamethylenetetramine (foaming agent H), 4' -oxo-diphenyl sulfonyl hydrazide (OBSH), baking soda and urea; the opacifier is SiC or Al2O3、TiO2、ZrO2One or more of the above; the flame retardant is Sb2O3、Al(OH)3、Mg(OH)2One or more of red phosphorus, expandable graphite and ammonium polyphosphate; the white carbon black is one or more of hydrophobic white carbon black and hydrophilic white carbon black.
As a preferable scheme of the invention, the silicon source is one or more of Tetraethoxysilane (TEOS), methyl orthosilicate (TMOS), Methyltriethoxysilane (MTES), methyltrimethoxysilane (MTMS), Polysiloxane (PEDS), silsesquioxane (POSS) and Trimethylchlorosilane (TMCS); the acidic catalyst is 0.5-1 mol/L hydrochloric acid; the alkaline catalyst is ammonia water with the concentration of 10-20%.
As a preferred scheme of the invention, the aerogel sol is uniformly sprayed on the section of the foamed sheet, and the spraying amount is 5-100 g/m2. Too little sol spraying amount can cause that the finished product can not meet the heat insulation requirement, and too much sol spraying amount can cause unnecessary waste.
The aerogel composite foaming sheet can be applied to heat preservation and insulation in the field of buildings and heat insulation in the field of electronic equipment.
In order to illustrate the process of the present invention in more detail, the following specific examples are provided for further details.
Example 1
A preparation method of an aerogel composite foaming sheet comprises the following steps:
a preparation of foamed sheet
Weighing 80 parts of polypropylene resin, 5 parts of foaming agent AC and TiO in parts by weight20.5 part of ammonium polyphosphate, 4 parts of hydrophilic fumed silica; the preparation method comprises the following steps of uniformly mixing the materials in an internal mixer with the temperature of 153 ℃ to prepare a sheet, irradiating and crosslinking the prepared sheet, foaming at the high temperature of 260 ℃, cooling to obtain a closed-cell foamed sheet, and slitting the foamed sheet into a thin foamed sheet with the specified thickness of 1mm parallel to the surface by using slitting equipment.
b, preparing aerogel sol
Weighing 5 parts of aerogel silicon source, 10 parts of deionized water and 10 parts of ethanol in parts by weight, uniformly stirring in a stirring kettle, adding 1mol/L hydrochloric acid to adjust the pH value to 3.5, continuously stirring for 30min, adding 20% ammonia water to adjust the pH value to 7.0, and continuously stirring uniformly to prepare aerogel sol.
And c, uniformly spraying the prepared aerogel sol on the section of the foaming sheet, standing for 5 hours at the temperature of 50 ℃ to convert the aerogel sol into gel, and thus obtaining the wet gel foaming sheet composite material.
And d, placing the prepared wet gel foamed sheet composite material in a 90 ℃ oven to dry for 20min under normal pressure to obtain the aerogel composite foamed sheet.
The foamed sheet has an apparent density of 0.091g/cm2The average pore diameter of the section is 97 μm, the thickness of the aerogel composite foamed sheet is 1.0mm, and the thermal conductivity is 0.021 W.m-1·K-1。
Example 2
A preparation method of an aerogel composite foaming sheet comprises the following steps:
a, preparing a foaming sheet:
weighing 75 parts of polypropylene resin, 3 parts of foaming agent sodium bicarbonate and Al in parts by weight2O30.5 part of Mg (OH)21 part of hydrophilic fumed silica 4 parts; the preparation method comprises the following steps of uniformly mixing the materials in an internal mixer with the temperature of 153 ℃ to prepare a sheet, carrying out irradiation crosslinking on the prepared sheet, foaming at the high temperature of 280 ℃, cooling to obtain a closed-cell foamed sheet, and using a sectioning device to section the foamed sheet into a thin foamed sheet with the specified thickness of 0.8mm in parallel with the surface.
b, preparing aerogel sol:
weighing 6 parts of aerogel silicon source, 10 parts of deionized water and 25 parts of ethanol in parts by weight, uniformly stirring in a stirring kettle, adding 1mol/L hydrochloric acid to adjust the pH value to 4.0, continuously stirring for 30min, adding 20% ammonia water to adjust the pH value to 7.5, and continuously stirring uniformly to prepare aerogel sol.
And c, uniformly spraying the prepared aerogel sol on the section of the foaming sheet, standing for 5 hours at the temperature of 50 ℃ to convert the aerogel sol into gel, and thus obtaining the wet gel foaming sheet composite material.
And d, placing the prepared wet gel foamed sheet composite material in a drying oven at 100 ℃ and drying for 10min under normal pressure to obtain the aerogel composite foamed sheet.
The foamed sheet had an apparent density of 0.133g/cm2The average pore diameter of the dissected plane is 67 μmThe thickness of the gel composite foaming sheet is 0.8mm, and the thermal conductivity is 0.030 W.m-1·K-1。
Example 3
A preparation method of an aerogel composite foaming sheet comprises the following steps:
a, preparing a foaming sheet:
weighing 60 parts of polypropylene resin, 10 parts of foaming agent AC, 0.5 part of SiC, 3 parts of expandable graphite and 5 parts of hydrophilic fumed silica in parts by weight; the preparation method comprises the following steps of uniformly mixing the materials in an internal mixer with the temperature of 153 ℃ to prepare a sheet, irradiating and crosslinking the prepared sheet, foaming at the high temperature of 200 ℃, cooling to obtain a closed-cell foamed sheet, and slitting the foamed sheet into a thin foamed sheet with the specified thickness of 1.2mm by using slitting equipment in parallel with the surface.
b, preparing aerogel sol:
weighing 8 parts of aerogel silicon source, 10 parts of deionized water and 35 parts of ethanol in parts by weight, uniformly stirring in a stirring kettle, adding 1mol/L hydrochloric acid to adjust the pH value to 3.0, continuously stirring for 10min, adding 20% ammonia water to adjust the pH value to 7.9, and continuously stirring uniformly to prepare aerogel sol.
And c, uniformly spraying the prepared aerogel sol on the section of the foaming sheet, standing for 8 hours at the temperature of 60 ℃ to convert the aerogel sol into gel, and thus obtaining the wet gel foaming sheet composite material.
And d, placing the prepared wet gel foamed sheet composite material in an oven at the temperature of 80 ℃ and drying for 50min at normal pressure to obtain the aerogel composite foamed sheet.
The foamed sheet has an apparent density of 0.072g/cm2The average pore diameter of the cross section is 100 mu m, the thickness of the aerogel composite foaming sheet is 1.2mm, and the thermal conductivity is 0.022 W.m-1·K-1。
Example 4
A preparation method of an aerogel composite foaming sheet comprises the following steps:
a preparation of foamed sheet
Weighing 50 parts of polypropylene resin, 6 parts of foaming agent AC and ZrO according to parts by weight20.5 part of Sb2O32 parts of (a) to (b),3 parts of hydrophilic fumed silica; the preparation method comprises the following steps of uniformly mixing the materials in an internal mixer with the temperature of 153 ℃ to prepare a sheet, irradiating and crosslinking the prepared sheet, foaming at the high temperature of 260 ℃, cooling to obtain a closed-cell foamed sheet, and slitting the foamed sheet into a thin foamed sheet with the specified thickness of 1.5mm by using slitting equipment in parallel with the surface.
b, preparing aerogel sol:
weighing 10 parts of aerogel silicon source, 20 parts of deionized water and 35 parts of ethanol in parts by weight, uniformly stirring in a stirring kettle, adding 1mol/L hydrochloric acid to adjust the pH value to 3.5, continuously stirring for 60min, adding 20% ammonia water to adjust the pH value to 8.0, and continuously stirring uniformly to prepare aerogel sol.
And c, uniformly spraying the prepared aerogel sol on the section of the foaming sheet, standing for 5 hours at the temperature of 70 ℃ to convert the aerogel sol into gel, and thus obtaining the wet gel foaming sheet composite material.
And d, placing the prepared wet gel foamed sheet composite material in an oven at 80 ℃ and drying for 60min at normal pressure to obtain the aerogel composite foamed sheet.
The foamed sheet had an apparent density of 0.065g/cm2The average pore diameter of the cross section is 107 μm, the thickness of the aerogel composite foamed sheet is 1.5mm, and the thermal conductivity is 0.028 W.m-1·K-1。
Example 5
A preparation method of an aerogel composite foaming sheet comprises the following steps:
a: preparing a foamed sheet:
weighing 90 parts of polypropylene resin, 1 part of foaming agent OBSH and TiO in parts by weight20.5 part, Al (OH)32 parts of hydrophilic fumed silica 5 parts; the preparation method comprises the following steps of uniformly mixing the materials in an internal mixer with the temperature of 153 ℃ to prepare a sheet, irradiating and crosslinking the prepared sheet, foaming at the high temperature of 220 ℃, cooling to obtain a closed-cell foamed sheet, and cutting the foamed sheet into a thin foamed sheet with the specified thickness of 0.3mm by using a cutting device in parallel with the surface.
b: preparing aerogel sol:
weighing 6 parts of aerogel silicon source, 35 parts of deionized water and 35 parts of ethanol in parts by weight, uniformly stirring in a stirring kettle, adding 1mol/L hydrochloric acid to adjust the pH value to 4.0, continuously stirring for 10min, adding 20% ammonia water to adjust the pH value to 7.1, and continuously stirring uniformly to prepare aerogel sol.
c: and uniformly spraying the prepared aerogel sol on a section of the foaming sheet, standing for 10 hours at the temperature of 50 ℃ to convert the aerogel sol into gel, and thus obtaining the wet gel foaming sheet composite material.
d: and (3) drying the prepared wet gel foamed sheet composite material in an oven at 100 ℃ for 10min under normal pressure to obtain the aerogel composite foamed sheet.
The foamed sheet had an apparent density of 0.249g/cm2The average pore diameter of the section is 55 mu m, the thickness of the aerogel composite foaming sheet is 0.3mm, and the thermal conductivity is 0.035 W.m-1·K-1。
The above description is only a preferred embodiment of the present invention, but the scope of the present invention is not limited to this embodiment, and any person skilled in the art can be covered by the present invention without inventive changes or substitutions within the technical scope of the present invention.
The test method of the invention comprises the following steps:
apparent Density determination
The apparent density of the foamed sheet layer was measured by the method described in GB/T6343-2009. 5 samples of 10000X 10000mm in parallel in the transverse direction were taken, and the average thickness and mass thereof were measured to obtain an apparent density.
Average pore diameter
The enlarged image of the pore diameter of the foamed sheet layer was read by a digital microscope, the area of all cells appearing in a certain area of the cut surface was measured, the circle-equivalent diameter was converted, and the average pore diameter was determined by averaging the number of cells.
Thickness measurement
The thicknesses of the substrate layer and the foamed sheet layer according to the present invention were measured by the method described in GB/T6672-2001. The test piece was cut out across the entire width in the transverse direction at about lm from the longitudinal end of the sample, the test piece was 100mm wide and 1000mm long, and thickness measurement was performed on 20 portions of the sample using a thickness measuring instrument, and the average thickness was the arithmetic average of all the measured values.
Average cell chord length
And reading the magnified image of the section of the foamed sheet by a digital microscope, determining the number of the cells or the cell walls within the range of 30mm long of the ruler, and then dividing the straight length by the number of the cells to obtain the average cell chord length t. If the coupon length is less than 30mm, the number of cells is determined in the maximum length. When the cell structure is anisotropic, the average cell diameter is determined in 3 main directions, respectively, and expressed as an average of 3 results.
Volume occupied by open cells with cut surfaces
Cutting a sample with original thickness on the cut foamed sheet, testing the average cell chord length t, and measuring the volume occupied by the open cells on the section of the foamed sheet
Figure BDA0003162810370000121
Wherein l is the length of the sample, w is the width of the sample, h is the thickness of the sample, and t is the average cell chord length of the sample.
In the invention, the aerogel and other materials are compounded and used to exert the heat insulation advantage of the aerogel to the maximum extent, which is the development trend of aerogel application.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. The utility model provides a compound foaming sheet of aerogel which characterized in that, it includes foaming sheet layer and aerogel layer, aerogel layer is attached to on the section face on foaming sheet layer, foaming sheet is the obturator foaming sheet, it cuts the face naturally and forms a large amount of sunken cellular network structures after being dissected, thereby can greatly increased the surface area of section face, adopt natural structure like this to make the combination nature of foaming sheet and aerogel inseparabler, cellular network structure is used as the skeleton of toughening of aerogel layer simultaneously, so that can protect the aerogel layer that forms in cellular network structure difficult destroyed in production and use.
2. The aerogel composite foamed sheet of claim 1, wherein the foamed sheet has an average pore size of 30 μm to 300 μm.
3. An aerogel composite foam sheet as in claim 2, wherein the number of open cells per square centimeter of the cross-sectional area of the foam sheet is 103To 106And (4) respectively.
4. An aerogel composite foamed sheet according to claim 3, wherein the number of cells having a diameter of less than 10 μm and a diameter of more than 300 μm in a cross-sectional plane of the foamed sheet is less than 50% of the total number of cells, and the number of cells having a diameter of 30 μm to 300 μm in a cross-sectional plane of the foamed sheet is more than 50% of the total number of cells.
5. An aerogel composite foam sheet as in claim 3, wherein the open cells per square centimeter cross-sectional area of the foam sheet occupy a volume of 10-4cm3～10-3cm3。
6. The aerogel composite foamed sheet according to claim 5, wherein the aerogel sol is uniformly adhered to the cut surface of the foamed sheet, and the adhered mass is 5g/m2～100g/m2。
7. The preparation method of the aerogel composite foamed sheet is characterized by comprising the following steps of S3:
uniformly spraying the prepared aerogel sol on a section of a foaming sheet, standing for 5-10 h at the temperature of 50-70 ℃ to convert the aerogel sol into gel to obtain a wet gel foaming sheet composite material, and drying the prepared wet gel foaming sheet composite material in a drying device at the temperature of 80-100 ℃ for 10-60 min to obtain the aerogel composite foaming sheet.
8. The method of claim 7, further comprising the steps of:
s1: preparing a foamed sheet, specifically, weighing 50-90 parts by weight of resin, 1-10 parts by weight of foaming agent, 0.1-0.5 part by weight of opacifier, 1-3 parts by weight of flame retardant and 1-5 parts by weight of white carbon black, uniformly mixing in an internal mixer at 120-160 ℃ to prepare the sheet, irradiating the prepared sheet to generate crosslinking, foaming at a high temperature of 200-280 ℃, cooling to obtain the foamed sheet, cutting the foamed sheet into thin foamed sheets with a specified thickness by using cutting equipment,
s2: the preparation method comprises the steps of weighing 5-10 parts by weight of an aerogel silicon source, 10-35 parts by weight of deionized water and 10-35 parts by weight of ethanol, uniformly stirring in a stirring kettle, adding an acidic catalyst to adjust the pH value to 3-4, continuously stirring for 10-60 min, adding an alkaline catalyst to adjust the pH value to 7-8, and continuously stirring uniformly to prepare the aerogel sol.
9. The method of claim 8, wherein in step S1,
the resin is selected from one or more of the following: one or more of polystyrene, polyurethane, polyvinyl chloride, polyethylene, polypropylene, ethylene-vinyl acetate copolymer, ethylene propylene diene monomer, nitrile butadiene rubber, natural rubber, polyvinyl formal, cellulose acetate, polymethyl methacrylate, polychlorinated or sulfonated polyethylene, polycarbonate, polyimide,
the foaming agent is one or more of azodimethyl phthalein amine, N '-dinitrosopentamethylenetetramine, 4' -oxo-bis-benzenesulfonyl hydrazide, sodium bicarbonate and urea,
the light-shading agent is SiC or Al2O3、TiO2、ZrO2One or more of the components (A) and (B),
the flame retardant is Sb2O3、Al(OH)3、Mg(OH)2One or more of red phosphorus, expandable graphite and ammonium polyphosphate,
the white carbon black is one or more of hydrophobic white carbon black and hydrophilic white carbon black,
the silicon source is one or more of ethyl orthosilicate, methyl triethoxysilane, methyl trimethoxysilane, polysiloxane, silsesquioxane and trimethylchlorosilane,
the acid catalyst is 0.5-1 mol/L hydrochloric acid, and the alkaline catalyst is 10-20% ammonia water by mass concentration.
10. Use of the aerogel composite foamed sheet according to any of claims 1 to 6, in thermal insulation in the building field or in the field of electronic devices.
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CN110524962A (en) * 2019-06-25 2019-12-03 深圳中凝科技有限公司 A kind of automobile aeroge thermoplastic material and its preparation method and application
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