Fire resistance class enhanced aerogel composition

Abstract

To provide reinforced aerogel compositions that are durable and easy to handle, have favorable performance in aqueous environments, have favorable insulation properties, and have favorable reaction to fire, combustion and flame-resistance properties, and to provide methods of preparing or manufacturing the same.SOLUTION: A composition has a silica-based aerogel framework, is reinforced with an open-cell macroporous framework, and includes one or more fireproof-class additives. The silica-based aerogel framework comprises at least one hydrophobic bound silicon and the composition or each of components thereof has desired properties.SELECTED DRAWING: Figure 1

Description

Technical Field

[0001] Cross - Reference to Related Applications This application claims the benefit of priority from U.S. Provisional Patent Application No. 62 / 678,850, filed on May 31, 2018, which is hereby incorporated by reference in its entirety, and all definitions of terms in this application shall be governed by this application.

[0002] The present invention generally relates to aerogel technology. More specifically, it relates to aerogel compositions containing fire - class additives.

Background Art

[0003] Low - density aerogel materials are widely considered to be the best available solid insulators. Aerogels function as insulators mainly by minimizing conduction (low structural density provides a tortuous path for energy transfer through the solid skeleton), convection (large pore volume and very small pore size result in minimal convection), and radiation (infrared - absorbing or scattering dopants are easily dispersed in the aerogel matrix). Aerogels can be used in a wide range of applications such as heating and cooling insulation, acoustic insulation, electronic dielectrics, aerospace, energy storage and production, filtration, etc. Furthermore, aerogel materials exhibit many other interesting acoustic, optical, mechanical, and chemical properties, making them very useful in various insulating and non - insulating applications.

[0004] However, what is needed are fire - class reinforced aerogel compositions having improved performance in various aspects including heat resistance, hydrophobicity, fire reaction, and others, either individually or in one or more combinations. However, considering the technology as a whole at the time the present invention was made, it was not obvious to those skilled in the art of the present invention how to overcome the drawbacks of the prior art.

[0005] To facilitate disclosure of the present invention, certain aspects of the prior art are discussed, but the applicant does not disclaim these technical aspects, and it is contemplated that the claimed invention may encompass one or more of the aspects of the prior art discussed herein.

[0006] In this specification, when a document, act, or item of knowledge is referred to or discussed, this reference or discussion does not admit that the document, act, or item of knowledge, or a combination thereof, was publicly available, known, part of common general knowledge, or otherwise constituted prior art under the applicable statutory provisions at the priority date, nor does it admit that it is known to be relevant to any attempt to solve any problem with which this specification is concerned.

SUMMARY OF THE INVENTION

PROBLEM TO BE SOLVED BY THE INVENTION

[0007] The long-standing but hitherto unmet needs for improved aerogel compositions are now satisfied by the novel, useful, and non-obvious present invention.

MEANS FOR SOLVING THE PROBLEM

[0008] In one embodiment, the present invention is a reinforced aerogel composition comprising a silica-based aerogel skeleton reinforced with an open-cell macroporous framework (「OCMF」) material and a fire-class additive, wherein the silica-based aerogel skeleton comprises at least one hydrophobic-bound silicon.

[0009] In one general aspect, the present disclosure provides a reinforced aerogel composition that is durable, easy to handle, has good performance in an aqueous environment, has good insulating properties, and further has good flame resistance and flame retardancy. In certain embodiments, the present disclosure provides a reinforced aerogel composition reinforced with OCMF, which composition has favorable performance in an aqueous environment, has favorable insulating properties, and also has favorable flame resistance and flame retardancy.

[0010] In another general aspect, the present disclosure provides a reinforced aerogel composition comprising a silica-based aerogel skeleton and OCMF. This composition has a) a thermal conductivity of 30 mW / m·K or less, b) an uptake amount of liquid water of 30 mass% (wt%) or less, and c) a heat of combustion of 717 cal / g or less. In certain embodiments, the reinforced aerogel composition of the present disclosure has a) a thermal conductivity of 25 mW / m·K or less; b) an uptake amount of liquid water of 20 wt% or less; and c) a heat of combustion of 717 cal / g or less. In certain embodiments, the reinforced aerogel composition of the present disclosure is 0.40 g / cm 3 Hereinafter, 0.30 g / cm 3 Hereinafter, 0.25 g / cm 3 Hereinafter, or 0.20 g / cm 3It has the following densities. In certain embodiments, the enhanced aerogel composition of the present disclosure has a thermal conductivity of 25 mW / m·K or less, 20 mW / m·K or less, 18 mW / m·K or less, a thermal conductivity of 15 mW / m·K to 30 mW / m·K, or a thermal conductivity of 15 mW / m·K to 20 mW / m·K. In certain embodiments, the enhanced aerogel composition of the present disclosure has a liquid water uptake of 30 wt% or less, 25 wt% or less, 20 wt% or less, 15 wt% or less, 10 wt% or less, or 5 wt% or less. In certain embodiments, the enhanced aerogel composition of the present disclosure has a heat of combustion of 717 cal / g or less, 700 cal / g or less, 675 cal / g or less, 650 cal / g or less, 625 cal / g or less, 600 cal / g or less, or 580 cal / g to 717 cal / g. In certain particular aspects, the combinations of the above values in thermal conductivity, water uptake, and heat of combustion are achieved by varying the composition of the gel precursor, the composition of the additive, the catalyst or other agent activating the precursor, the pH of the precursor solution, the respective dosing rates of the precursor, catalyst or additive, the time allowed for gelation to occur, the winding of the gel (in certain aspects), the aging time and pH, any post-gelation treatment, the extraction time and conditions (temperature, pressure), and any subsequent drying steps.

[0011] In another general aspect, the present disclosure provides an enhanced aerogel composition comprising a silica-based aerogel skeleton, a melamine-based OCMF, and a refractory class additive, having the following properties: a) a thermal conductivity of 15 mW / m·K to 30 mW / m·K, b) a liquid water uptake of 30 wt% or less, and c) a heat of combustion of 580 cal / g to 717 cal / g. In certain preferred embodiments, the OCMF material is an organic OCMF material. In certain other preferred embodiments, the OCMF material is a melamine-based OCMF material. In certain preferred embodiments, the enhanced aerogel composition of the present disclosure has about 1 wt% to about 30 wt%, about 1 wt% to about 25 wt%, about 1 wt% to about 20 wt%, about 1 wt% to about 15 wt%, about 1 wt% to about 10 wt%, or about 1 wt% to about 5 wt% of a hydrophobic organic inclusion.

[0012] In another general aspect, the present disclosure provides a method for manufacturing a reinforced aerogel composition, comprising: a) providing a precursor solution comprising a silica gel precursor material, a solvent, and optionally a catalyst; b) combining the precursor solution with a reinforcement comprising OCMF; c) transferring the silica gel precursor material in the precursor solution to a gel material or composition; and d) extracting at least a portion of the solvent from the gel material or composition to obtain an aerogel material or composition. In certain embodiments, the method of the present disclosure comprises incorporating a refractory class additive material into the reinforced aerogel composition by combining the refractory class additive material with the precursor solution at any stage before or during the transfer of the silica gel precursor material in the precursor solution to a gel composition. In preferred embodiments, the reinforcement comprises a melamine-based OCMF material. In certain embodiments, the method of the present disclosure comprises incorporating at least one hydrophobic bonded silicon into the aerogel material or composition by one or both of: i) including in the precursor solution at least one silica gel precursor material having at least one hydrophobic group; or ii) exposing the precursor solution, gel composition, or aerogel composition to a hydrophobizing agent. In certain embodiments, the method of the present disclosure comprises a step of incorporating at least one hydrophobic bonded silicon into the aerogel composition to provide a hydrophobic organic content in the aerogel composition of about 1 wt% to about 25 wt%, about 1 wt% to about 20 wt%, about 1 wt% to about 15 wt%, about 1 wt% to about 10 wt%, or about 1 wt% to about 5 wt%. In preferred embodiments, the method of the present disclosure produces a reinforced aerogel composition. In certain embodiments, the method of the present disclosure results in a reinforced aerogel composition comprising a silica-based aerogel skeleton, a melamine-based OCMF, and a refractory class additive, and having the following properties: a) a thermal conductivity of 15 mW / m·K to 30 mW / m·K; b) a liquid water uptake of 30 wt% or less; and c) a heat of combustion of 580 cal / g to 717 cal / g.

[0013] Furthermore, the following specific, non-limiting embodiments / examples are disclosed. The enumerated examples are shown to illustrate certain embodiments within the specific scope contemplated herein, including combinations of such embodiments or examples. The invention as claimed in the claims has a scope that extends beyond these non-limiting examples.

[0014] Embodiment 1 is a reinforced aerogel composition comprising a silica-based aerogel skeleton reinforced with an OCMF material and a refractory class additive, wherein the silica-based aerogel skeleton comprises at least one hydrophobic bonded silicon, and the reinforced aerogel composition has the following properties: i) a liquid water uptake of 20 wt% or less, ii) a thermal conductivity of 30 mW / m·K or less, and iii) a heat of combustion of 717 cal / g or less.

[0015] Embodiment 2 is a reinforced aerogel composition comprising a silica-based aerogel skeleton reinforced with an OCMF material having a density of 2 kg / m 3 ~25 kg / m 3 and a refractory class additive, wherein the silica-based aerogel skeleton comprises at least one hydrophobic bonded silicon, and the reinforced aerogel composition has the following properties: i) a liquid water uptake of 20 wt% or less; ii) a thermal conductivity of 30 mW / m·K or less; and iii) a heat of combustion of 717 cal / g or less.

[0016] Embodiment 3 is a reinforced aerogel composition comprising a silica-based aerogel skeleton reinforced with an OCMF material having a density of 2 kg / m 3 ~25 kg / m 3 and a refractory class additive, wherein the silica-based aerogel skeleton comprises at least one hydrophobic bonded silicon, and the reinforced aerogel composition has the following properties: i) a liquid water uptake of 1 wt% or more and 10 wt% or less; ii) a thermal conductivity of more than 8 mW / m·K and less than 25 mW / m·K; and iii) a heat of combustion of less than 717 cal / g and more than 400 cal / g.

[0017] Embodiment 4 is a reinforced OCMF composition strengthened with a silica-based aerogel composition and a fireproofing additive, wherein the silica-based aerogel skeleton contains at least one hydrophobic bonded silicon, and the reinforced aerogel composition has the following properties: i) a liquid water uptake of 20 wt% or less; ii) a thermal conductivity of 30 mW / m·K or less; and iii) a heat of combustion of less than 717 cal / g.

[0018] Embodiment 5 is a reinforced OCMF composition strengthened with a silica-based aerogel composition and a fireproofing additive, wherein the silica-based aerogel skeleton contains at least one hydrophobic bonded silicon, and the reinforced aerogel composition has the following properties: i) a liquid water uptake of 20 wt% or less; ii) a thermal conductivity of 30 mW / m·K or less; and iii) a heat of combustion of less than 717 cal / g.

[0019] Embodiment 6 is a reinforced OCMF composition strengthened with a silica-based aerogel composition and a fireproofing additive, wherein the silica-based aerogel skeleton contains at least one hydrophobic bonded silicon, and the reinforced aerogel composition has the following properties: i) a liquid water uptake of 1 wt% to 10 wt%; ii) a thermal conductivity greater than 8 mW / m·K and less than 25 mW / m·K; and iii) a heat of combustion of less than 717 cal / g and greater than 400 cal / g.

[0020] Embodiment 7 is a group of embodiments by any one of the reinforced aerogel compositions of Embodiments 1 to 3 or any one of the reinforced OCMF compositions of Embodiments 4 to 6, wherein the OCMF material contains an organic OCMF material or is an organic OCMF material.

[0021] Embodiment 8 is a group of embodiments by any one of the reinforced aerogel compositions of Embodiments 1 to 3 or any one of the reinforced OCMF compositions of Embodiments 4 to 6, wherein the OCMF material contains a melamine-based OCMF material or is a melamine-based OCMF material.

[0022] Embodiment 9 is a group of embodiments of any one of the reinforced aerogel compositions of Embodiments 1 to 3 or any one of the reinforced OCMF compositions of Embodiments 4 to 6, where the OCMF material includes a sheet-shaped OCMF material or is a sheet-shaped OCMF material.

[0023] Embodiment 10 is a group of embodiments of any one of the reinforced aerogel compositions of Embodiments 1 to 3 or any one of the reinforced OCMF compositions of Embodiments 4 to 6, where the OCMF material is an organic foam.

[0024] Embodiment 11 is a group of embodiments of any one of the reinforced aerogel compositions of Embodiments 1 to 3 or any one of the reinforced OCMF compositions of Embodiments 4 to 6, where the OCMF material is a melamine-based foam.

[0025] Embodiment 12 is a group of embodiments of any one of the reinforced aerogel compositions or reinforced OCMF compositions of Embodiments 1 to 11, where the OCMF material is neither a low-flammability material nor a non-flammable material.

[0026] Embodiment 13 is a group of embodiments of any one of the reinforced aerogel compositions or reinforced OCMF compositions of Embodiments 1 to 11, where the OCMF material is neither a low-flame-combustible material nor a non-flame-combustible material.

[0027] Embodiment 14 is a group of embodiments of any one of the reinforced aerogel compositions or reinforced OCMF compositions of Embodiments 1 to 11, where the OCMF material constitutes 2 wt% to 10 wt% of the composition.

[0028] Embodiment 15 is a group of embodiments of any one of the reinforced aerogel compositions or reinforced OCMF compositions of Embodiments 1 to 14, where the content of hydrophobic silicon bonds in the composition is 2 wt% to 10 wt%.

[0029] Embodiment 16 is a group of embodiments having a reinforced aerogel composition or a reinforced OCMF composition according to any one of Embodiments 1 to 14, wherein the content of hydrophobic silicon bonds in the composition is 2 wt% to 8 wt%.

[0030] Embodiment 17 is a group of embodiments by a reinforced aerogel composition or a reinforced OCMF composition according to any one of Embodiments 1 to 14, wherein the content of hydrophobic silicon bonds in the composition is 2 wt% to 6 wt%.

[0031] Embodiment 18 is a group of embodiments by a reinforced aerogel composition or a reinforced OCMF composition according to any one of Embodiments 1 to 17, wherein the composition has a heat of combustion of 700 cal / g or less.

[0032] Embodiment 19 is a group of embodiments by a reinforced aerogel composition or a reinforced OCMF composition according to any one of Embodiments 1 to 17, wherein the composition has a heat of combustion of 675 cal / g or less.

[0033] Embodiment 20 is a group of embodiments by a reinforced aerogel composition or a reinforced OCMF composition according to any one of Embodiments 1 to 17, wherein the composition has a heat of combustion of 650 cal / g or less.

[0034] Embodiment 21 is a group of embodiments by a reinforced aerogel composition or a reinforced OCMF composition according to any one of Embodiments 1 to 17, wherein the composition has a heat of combustion of 625 cal / g or less.

[0035] Embodiment 22 is a group of embodiments by a reinforced aerogel composition or a reinforced OCMF composition according to any one of Embodiments 1 to 21, wherein the composition has a thermal conductivity of 22 mW / m·K or less.

[0036] Embodiment 23 is a group of embodiments by a reinforced aerogel composition or a reinforced OCMF composition according to any one of Embodiments 1 to 21, wherein the reinforced aerogel composition has a thermal conductivity of 20 mW / m·K or less.

[0037] Embodiment 24 is a group of embodiments using any one of the reinforced aerogel compositions or reinforced OCMF compositions of Embodiments 1 to 21, wherein the reinforced aerogel composition has a thermal conductivity of 18 mW / m·K or less.

[0038] Embodiment 25 is a group of embodiments using any one of the reinforced aerogel compositions or reinforced OCMF compositions of Embodiments 1 to 21, wherein the reinforced aerogel composition has a density of 0.15 to 0.40 g / cm 3 .

[0039] Embodiment 26 is a group of embodiments using any one of the reinforced aerogel compositions or reinforced OCMF compositions of Embodiments 1 to 21, wherein the thermal decomposition starting point of the reinforced aerogel composition is 350°C or higher.

[0040] Embodiment 27 is a group of embodiments using any one of the reinforced aerogel compositions or reinforced OCMF compositions of Embodiments 1 to 21, wherein the thermal decomposition starting point of the reinforced aerogel composition is 360°C or higher.

[0041] Embodiment 28 is a group of embodiments using any one of the reinforced aerogel compositions or reinforced OCMF compositions of Embodiments 1 to 21, wherein the thermal decomposition starting point of the reinforced aerogel composition is 370°C or higher.

[0042] Embodiment 29 is a group of embodiments using any one of the reinforced aerogel compositions or reinforced OCMF compositions of Embodiments 1 to 21, wherein the thermal decomposition starting point of the reinforced aerogel composition is 380°C or higher.

[0043] Embodiment 30 is a group of embodiments using any one of the reinforced aerogel compositions or reinforced OCMF compositions of Embodiments 1 to 21, wherein the thermal decomposition starting point of the reinforced aerogel composition is 390°C or higher.

[0044] Embodiment 31 is an organic OCMF-reinforced aerogel composition containing a fire-resistant class additive and a hydrophobic organic content, wherein the endothermic decomposition start point of the fire-resistant class additive in the composition is within 50 °C of the thermal decomposition start point of the other parts of the composition other than the fire-resistant class additive, and it is an organic OCMF-reinforced aerogel composition.

[0045] Embodiment 32 is an organic OCMF-reinforced aerogel composition containing a fire-resistant class additive and a hydrophobic content of at least 5%, wherein the total heat of endothermic decomposition of the fire-resistant class additive in the composition is at least 30% of the exothermic heat of decomposition of the other parts of the composition other than the fire-resistant class additive, and it is an organic OCMF-reinforced aerogel composition.

[0046] Embodiment 33 is an organic OCMF-reinforced aerogel composition containing at least two fire-resistant class additives whose endothermic decomposition start points are at least 10 °C apart from each other.

[0047] Embodiment 34 is an organic OCMF-reinforced aerogel composition containing a fire-resistant class additive and a hydrophobic content, wherein the total heat of endothermic decomposition of the fire-resistant class additive in the composition is 80% or less of the exothermic heat of decomposition of the other parts of the composition other than the fire-resistant class additive, and it is an organic OCMF-reinforced aerogel composition.

[0048] Embodiment 35 is a group of embodiments according to any one of Embodiments 1 to 11 of the reinforced aerogel composition or the reinforced OCMF composition, wherein the hydrophobic content is at least 5%, and the total heat of endothermic decomposition of the fire-resistant class additive in the composition is at least 30% of the exothermic heat of decomposition of the other parts of the composition other than the fire-resistant class additive.

[0049] Embodiment 36 is a group of embodiments according to any one of Embodiments 1 to 11 of the reinforced aerogel composition or the reinforced OCMF composition, wherein the endothermic decomposition start point of the fire-resistant class additive in the composition is within 50 °C of the thermal decomposition start point of the other parts of the composition other than the fire-resistant class additive.

[0050] Embodiment 37 is a group of embodiments by any one of the reinforced aerogel compositions or reinforced OCMF compositions of Embodiments 1 to 11, which have at least two refractory class additives, and the endothermic decomposition start points of the two refractory class additives are at least 10 °C apart.

[0051] Embodiment 38 is a group of embodiments by any one of the reinforced aerogel compositions or reinforced OCMF compositions of Embodiments 1 to 11, in which the total heat of endothermic decomposition of the refractory class additive in the composition is 80% or less of the heat of exothermic decomposition of the other parts of the composition other than the refractory class additive.

[0052] Embodiment 39 is a group of embodiments by any one of the compositions of Embodiments 1 to 38, in which the increase in the furnace temperature in accordance with ISO 1182 of the composition is about 100 °C or less, about 90 °C or less, about 80 °C or less, about 70 °C or less, about 60 °C or less, about 50 °C or less, about 45 °C or less, about 40 °C or less, about 38 °C or less, about 36 °C or less, about 34 °C or less, about 32 °C or less, about 30 °C or less, about 28 °C or less, about 26 °C or less, about 24 °C or less, or within the range between any two of these values.

[0053] Embodiment 40 is a group of embodiments by any one of the compositions of Embodiments 1 to 39, in which the flame time of the composition in accordance with ISO 1182 is about 30 seconds or less, about 25 seconds or less, about 20 seconds or less, about 15 seconds or less, about 10 seconds or less, about 5 seconds or less, about 2 seconds or less, or within the range between any two of these values.

[0054] Embodiment 41 is a group of embodiments by any one of the compositions of Embodiments 1 to 40, in which the mass loss of the composition in accordance with ISO 1182 is about 50% or less, about 40% or less, about 30% or less, about 28% or less, about 26% or less, about 24% or less, about 22% or less, about 22% or less, about 20% or less, about 18% or less, about 16% or less, or within the range between any two of these values.

[0055] Embodiment 42 is a group of embodiments by any one of the compositions of the above embodiments, wherein the composition has low flammable combustibility.

[0056] Embodiment 43 is a group of embodiments by any one of the compositions of the above embodiments, wherein the composition has non-flammable combustibility.

[0057] Embodiment 44 is a group of embodiments by any one of the compositions of the above embodiments, wherein the composition has low combustibility.

[0058] Embodiment 45 is a group of embodiments by any one of the compositions of the above embodiments, wherein the composition has incombustibility.

[0059] Embodiment 46 is a group of embodiments by any one of the compositions of the above embodiments, wherein the endothermic decomposition starting point of the fire resistance class additive is higher than 280 °C, 300 °C, 350 °C, 400 °C, 450 °C or 500 °C.

[0060] Embodiment 47 is a group of embodiments by any one of the compositions of the above embodiments, wherein the exothermic decomposition starting point of the composition not containing the fire resistance class additive is higher than 280 °C, 300 °C, 350 °C, 400 °C, 450 °C or 500 °C.

[0061] Embodiment 48 is a group of embodiments by any one of the compositions of the above embodiments, wherein the OCMF material is a melamine-based foam.

[0062] Embodiment 49 is a group of embodiments by any one of the compositions of the above embodiments, wherein the OCMF material is a urethane-based polymer foam.

[0063] Embodiment 50 is a group of embodiments having any one of the compositions of the above claims, wherein the OCMF material is a reticulated foam.

[0064] Furthermore, the aerogel materials or frameworks of various embodiments of the present invention may be implemented using an aerogel particle-based slurry or suspension impregnated into the OCMF materials described in various embodiments. In yet another embodiment, various embodiments of the present invention involve impregnating various gel precursors into the OCMF materials in a suitable solvent and then using various methods including using supercritical fluids or by removing the solvent at high temperature and ambient or subcritical pressure to implement using an in-situ manufactured non-particulate aerogel material.

[0065] In another embodiment, the present invention includes reinforced aerogel compositions or OCMF-reinforced compositions having one or more or all of the above-described features and properties, including their various combinations and methods of manufacture.

[0066] These and other important objects, advantages, and features of the present invention will become apparent as the disclosure progresses.

[0067] The present invention includes structural features, combinations of elements, and features of the arrangement of parts exemplified in the disclosure shown below, and the scope of the present invention is set forth in the claims.

Brief Description of the Drawings

[0068]

Figure 1

[0069]

Figure 2

DETAILED DESCRIPTION OF THE INVENTION

[0070] In the following detailed description of the preferred embodiments, reference is made to the accompanying drawings, which form a part hereof, and in which are shown, by way of illustration, specific embodiments in which the invention may be practiced. It will be understood that other embodiments may be utilized and structural changes may be made without departing from the scope of the present invention.

[0071] As used in this specification and the appended claims, the singular forms "a", "an", and "the" include plural referents unless the content clearly dictates otherwise. As used in this specification and the appended claims, the term "or" is generally used in its sense including "and / or" unless the context clearly dictates otherwise.

[0072] As used herein, "about" means approximately or nearly and, in the context of the recited numerical or range, means ±15% of that numerical value. In one embodiment, the term "about" may include conventional rounding according to the significant figures of the numerical value. Further, the expression "about "x" to "y"" includes "about "x" to about "y"".

[0073] As used herein, the terms "composition" and "composite" are used interchangeably.

[0074] Aerogels are a group of porous materials having interconnected open cells that include a framework of interconnected structure, with a corresponding network of pores integrated within the framework and an interstitial phase within the network of pores that contains mainly gases such as air. Aerogels are typically characterized by low density, high porosity, large surface area, and small pore size. Aerogels can be distinguished from other porous materials by their physical and structural properties.

[0075] In the context of the present disclosure, the term "aerogel" or "aerogel material" refers to a gel that includes a framework of interconnected structure, has a corresponding network of interconnected pores integrated within the framework, contains a gas such as air as a dispersed interstitial medium, and has the following physical and structural properties (by nitrogen porosimetry testing) attributable to an aerogel: a) an average pore diameter of from about 2 nm to about 100 nm, (b) a porosity of at least 80% or more, and (c) a surface area of about 20 m 2 / g or more.

[0076] The aerogel materials of the present disclosure thus include, in addition to any aerogel or other open-cell compound that meets the defined elements described in the preceding paragraph, compounds that can be classified as xerogels, cryogels, ambigels, microporous materials, and the like.

[0077] Aerogel materials can also be further characterized by additional physical properties that include: (d) a pore volume of about 2.0 mL / g or more, particularly about 3.0 mL / g or more; (e) a density of about 0.50 g / cc or less, particularly about 0.25 g / cc or less; and (f) at least 50% of the total pore volume being composed of pores having a pore diameter of 2 to 50 nm. Meeting these additional properties is not necessary to characterize a compound as an aerogel material.

[0078] In the context of the present disclosure, the term "innovative processing and extraction techniques" refers to methods that result in low pore collapse and low shrinkage in the skeletal structure of a gel, and that replace the liquid interstitial phase in a wet gel material with a gas such as air. In drying techniques such as atmospheric evaporation, strong capillary pressures and other mass transfer limitations often occur at the liquid-vapor interface of the interstitial phase being evaporated or removed. The strong capillary forces generated by the evaporation or removal of the liquid can cause significant pore shrinkage and skeletal collapse within the gel material. By using innovative processing and extraction techniques during the extraction of the liquid interstitial phase, the negative impact of capillary forces on the pores and skeleton of the gel during liquid extraction (also referred to as solvent removal or drying) is reduced.

[0079] In certain embodiments, the innovative processing and extraction techniques use near-critical or supercritical liquids or near-critical or supercritical states to extract the liquid interstitial phase from the wet gel material. This can be achieved by removing the liquid interstitial phase from the gel in a state near the critical point or beyond the supercritical point of the liquid or liquid mixture. Co-solvents and solvent exchange can be used to optimize the near-critical or supercritical liquid extraction process.

[0080] In certain embodiments, the innovative processing and extraction techniques include modifying the gel skeleton to reduce the irreversible effects of capillary pressure and other mass transfer limitations at the liquid-vapor interface. This embodiment includes treating the gel skeleton with a hydrophobizing agent, or other functionalizing agent, which enables the gel skeleton to withstand or recover from any collapsing forces during liquid extraction performed below the critical point of the liquid interstitial phase. This embodiment can also include incorporating functional groups or skeletal elements that provide a skeletal elastic modulus high enough to withstand or recover from collapsing forces during liquid extraction performed below the critical point of the liquid interstitial phase.

[0081] In the context of the present disclosure, the term "skeleton" or "skeletal structure" refers to a network of interconnected oligomers, polymers, or particles that form the solid structure of a material. In the context of the present disclosure, the term "aerogel skeleton" or "aerogel skeletal structure" refers to a network of interconnected oligomers, polymers, or colloidal particles that form the solid structure of a gel or aerogel. The polymers or particles that make up the aerogel skeletal structure typically have a diameter of about 100 angstroms. However, the skeletal structures of the present disclosure may include networks of interconnected oligomers, polymers, or colloidal particles of any diameter size that form a solid structure within a material such as, for example, a gel or aerogel. Further, the term "silica-based aerogel" or "silica-based aerogel skeleton" refers to an aerogel skeleton in which silica constitutes at least 50% (by mass) of the oligomers, polymers, or colloidal particles that form the solid skeletal structure within the gel or aerogel.

[0082] Within the context of the present disclosure, the term "aerogel composition" refers to any composite material that includes an aerogel material as a component of the composition. Examples of aerogel compositions include fiber-reinforced aerogel composite materials; aerogel composite materials that include additive elements such as opacifying agents; aerogel composite materials strengthened by a continuous cellular macroporous skeleton; aerogel polymer composite materials; and composite materials in which aerogel microparticles, particles, granules, beads, or powders are incorporated into a solid or semi-solid material such as a binder, resin, cement, foam, polymer, or similar solid material, but are not limited thereto. Aerogel compositions are generally obtained after removing the solvent from the various gel materials disclosed in the present invention. The aerogel compositions thus obtained may be further subjected to additional processing or treatments. The various gel materials may also be subjected to additional processing or treatments that are separately known or useful in the art prior to being subjected to solvent removal (or liquid extraction or drying).

[0083] In the context of the present disclosure, the term "monolithic" refers to an aerogel material in which most (by mass) of the aerogel contained in the aerogel material or composition is in the form of a single interconnected aerogel nanostructure. Monolithic aerogel materials include aerogel materials that were initially formed to have a single interconnected gel or aerogel nanostructure but were subsequently divided, fragmented, or segmented into non-single aerogel nanostructures. Monolithic aerogel materials are distinguished from particulate aerogel materials. The term "particulate aerogel material" refers to an aerogel material in which most (by mass ratio) of the aerogel contained in the aerogel material is in the form of microparticles, particles, granules, beads, or powders, which can be combined or compressed together but lack an interconnected aerogel nanostructure between individual particles.

[0084] Within the context of the present disclosure, the term "wet gel" refers to a gel in which the mobile interstitial phase within the network of interconnected pores is composed primarily of a liquid such as a conventional solvent, a liquefied gas such as liquid carbon dioxide, or a combination thereof. Aerogels typically require the initial production of a wet gel followed by innovative processing and extraction to replace the mobile interstitial liquid in the gel with air. Examples of wet gels include, but are not limited to, alcogels, hydrogels, ketogels, carbogels, and any other wet gels known to those skilled in the art.

[0085] The aerogel composition of the present disclosure may constitute a reinforced aerogel composition. In the context of the present disclosure, the term "reinforced aerogel composition" refers to an aerogel composition containing a reinforcing phase within the aerogel material, where the reinforcing phase is not part of the aerogel skeleton itself. The reinforcing phase may be any material that provides improved flexibility, elasticity, conformity, or structural stability to the aerogel material. Examples of well-known reinforcing materials include continuous bubble macroporous skeleton reinforcing materials, closed-cell macroporous skeleton reinforcing materials, continuous bubble membranes, honeycomb reinforcing materials, polymer reinforcing materials, and fiber reinforcing materials such as discrete fibers, woven fabric materials, non-woven fabric materials, needle-punched non-wovens, batting, webs, mats, and felts, but are not limited thereto.

[0086] The reinforced aerogel composition of the present disclosure may include an aerogel composition reinforced with a continuous bubble macroporous skeleton material. In the context of the present disclosure, the term "continuous bubble macroporous skeleton" or "OCMF" refers to a skeleton of an interconnected structure having a substantially uniform composition, having a corresponding network of interconnected pores incorporated within the skeleton, and being characterized by an average pore diameter in the range of about 10 μm to about 700 μm. Such an average pore diameter can be measured by known techniques such as microscopy by optical analysis. Thus, the OCMF material of the present disclosure includes any continuous bubble material that satisfies the defined elements described in this paragraph, including other classifiable compounds such as foams, foam-like materials, and macroporous materials. The OCMF material is distinguished from materials having no uniform composition, such as materials that constitute a skeleton of an interconnected structure having a void volume within the skeleton, or an aggregate of fibers and binders having a void volume within a fiber matrix.

[0087] In the context of the present disclosure, the term "substantially uniform composition" refers to the uniformity of the composition of the material being referenced within an allowable range of 10%.

[0088] In the context of the present disclosure, the term "OCMF-reinforced aerogel composition" refers to a reinforced aerogel composition that includes a continuous bubble macroporous skeletal material as a reinforcing phase. Suitable OCMF materials for use in the present disclosure include, but are not limited to, OCMF materials made from organic polymer materials. Examples include OCMF materials made from polyolefins, polyurethanes, phenols, melamine, cellulose acetate, and polystyrene. In the context of the present disclosure, the term "organic OCMF" refers to an OCMF material having a skeleton mainly composed of an organic polymer material. In certain embodiments, OCMF materials made from melamine or melamine derivatives are also preferred. In the context of the present disclosure, the terms "melamine OCMF" or "melamine-based OCMF" refer to an organic OCMF material having a skeleton mainly composed of a polymer material obtained by reacting melamine with a condensing agent such as formaldehyde. Examples of OCMF materials made from melamine or melamine derivatives for use in the present disclosure are described in U.S. Pat. Nos. 8,546,457 and 4,666,948, and International Publication No. 2001 / 094436. The term "inorganic OCMF" refers to an OCMF material having a skeleton mainly composed of inorganic materials. Examples of inorganic OCMFs include, but are not limited to, cementitious materials, gypsum, and calcium silicate.

[0089] In the context of the present invention, the term "foam" refers to a material that includes a skeleton of a polymer structure with a substantially uniform composition, interconnected, and having a corresponding network or aggregate of pores integrated within the skeleton, formed by dispersing a proportion of gas in the form of bubbles in a liquid or resin foam material such that the gas bubbles are retained as pores when the foam material solidifies into a solid structure. Generally, foams can be manufactured using a variety of processes. See, for example, U.S. Pat. Nos. 6,147,134, 5,889,071, 6,187,831, and 5,229,429. Accordingly, the foam materials of the present disclosure include any material that meets the defined elements of this paragraph, including compounds that may be classified as OCMF materials, macroporous materials, etc. The foam as defined in the present invention can be of the type of thermoplastic resins, elastomers, and thermosetting resins (duromers).

[0090] The pores within a solid framework are sometimes referred to as "cells". Cells can be divided by cell walls or membranes and can form an aggregate of independent closed pores within a porous material. The term "closed cell" refers to a porous material in which at least 50% of the pore volume is (substantially) enclosed by a membrane or wall. The cells within a material may be interconnected via cell openings and form a network of interconnected open pores within the material. The term "open cell" refers to a porous material in which at least 50% of the pore volume is open cell. An open cell material can consist of a reticulated open cell material, a non-reticulated open cell material, or a combination thereof. A reticulated material is an open cell material produced via a reticulation process that removes or perforates the cell membranes within a porous material. Reticulated materials typically have a higher concentration of open cells than non-reticulated materials, but are more expensive and tend to be difficult to manufacture. Generally, no porous material has a completely single type of cell structure (open cell or closed cell). Porous materials can be manufactured using a variety of methods, including the foam manufacturing methods presented in U.S. Pat. Nos. 6,147,134, 5,889,071, 6,187,831, 5,229,429, and 4,454,248, as well as U.S. Patent Application No. 2007 / 0213417.

[0091] In the context of the present disclosure, the term "aerogel blanket" or "aerogel blanket composition" refers to an aerogel composition reinforced with a continuous sheet of a reinforcing material. The aerogel blanket composition can be distinguished from other reinforced aerogel compositions reinforced with discontinuous reinforcing materials, such as, for example, isolated aggregates or masses of reinforcing materials. The aerogel blanket composition is highly conformable while retaining the excellent thermal insulation properties of the aerogel and can be used like a blanket to cover surfaces of simple or complex shapes, and is thus particularly useful for applications that require flexibility.

[0092] In the context of the present disclosure, the terms "flexible" and "flexibility" refer to the ability of an aerogel material or composition to bend or flex without macroscopic damage. The aerogel compositions of the present disclosure can bend at least 5°, at least 25°, at least 45°, at least 65°, or at least 85° without macroscopic damage and / or have a bend radius of less than 4 feet, less than 2 feet, less than 1 foot, less than 6 inches, less than 3 inches, less than 2 inches, less than 1 inch, or less than 1 / 2 inch without macroscopic damage. Similarly, the term "highly flexible" or "high flexibility" refers to an aerogel material or composition that can bend up to at least 90° and / or has a bend radius of less than 1 / 2 inch without macroscopic damage. Further, the terms "classified flexible" and "classified as flexible" refer to an aerogel material or composition that can be classified as flexible according to ASTM C1101 (ASTM International, West Conshohohocken, Pennsylvania).

[0093] The aerogel compositions of the present disclosure can be of flexible, highly flexible, and / or classified flexible nature. The aerogel compositions of the present disclosure can also be drapable. In the context of the present disclosure, the terms "drapable" and "drapability" refer to the ability of an aerogel material or composition to be bent at a radius of curvature of about 4 inches or less to about 90° or more without macroscopic damage. An aerogel material or composition according to a particular embodiment of the present invention has flexibility such that the composition is non-rigid and can be applied and conformed to a three-dimensional surface or object, or is pre-formed into various shapes and configurations to facilitate installation or application.

[0094] In the context of the present disclosure, the term "additive" or "additive element" refers to a material that can be added to an aerogel composition before, during, or after the production of the aerogel. Additives can be added to change or improve the desirable properties of the aerogel or to counteract the undesirable properties of the aerogel. Additives are typically added to the aerogel material either before gelation into the precursor liquid, during gelation into the transition state material, or after gelation into the solid or semi-solid material. Examples of additives include, but are not limited to, microfibers, fillers, reinforcing agents, stabilizers, thickeners, elastic compounds, opacifying agents, coloring or pigment-forming compounds, radiation-absorbing compounds, radiation-reflecting compounds, fireproofing additives, corrosion inhibitors, thermal conductivity components, phase change materials, pH adjusters, redox adjusters, HCN mitigators, off-gas mitigators, conductive compounds, electrical insulating compounds, magnetic compounds, radar-blocking components, curing agents, anti-shrinkage agents, and other aerogel additives known in the art.

[0095] In the context of the present disclosure, the terms "thermal conductivity" and "TC" refer to a measure of the ability of a material or composition to transfer heat between two surfaces on either side of the material or composition, with a temperature difference between the two surfaces. Thermal conductivity is specifically measured as the heat energy transferred per unit time and per unit surface area divided by the temperature difference. This is typically recorded in SI units as mW / m·K (milliwatts per meter times Kelvin). The thermal conductivity of a material is determined by the "Test Method for Steady-State Thermal Transmission Properties by Means of the Heat Flow Meter Apparatus" (ASTM C518, ASTM International, West Conshohocken, Pennsylvania), the "a Test Method for Steady-State Heat Flux Measurements and Thermal Transmission Properties by Means of the Guarded-Hot-Plate Apparatus" (ASTM C177, ASTM International, West Conshohocken, Pennsylvania), the "a Test Method for Steady-State Heat Transfer Properties of Pipe Insulation" (ASTM C335, ASTM International, West Conshohocken, Pennsylvania), the "Thin Heater Thermal Conductivity Test" (ASTM C1114, ASTM International, West Conshohocken, Pennsylvania), the "Determination of thermal resistance by means of guarded hot plate and heat flow meter methods" (EN12667, the British Standards Institution (UK), or "Determination of steady-state thermal resistance and related properties - Guarded hot plate apparatus" (ISO 8203, International Organization for Standardization, Switzerland), etc., which can be determined by test methods known in the art (not limited thereto). Since different methods may yield different results, within the context of the present disclosure and unless explicitly stated otherwise, thermal conductivity measurements are obtained according to ASTM C518 (Standard Test Method for Steady-State Heat Transfer Properties by the Heat Flow Meter Apparatus) at the ambient atmospheric pressure, at a temperature of about 37.5 °C, and under a compressive load of about 2 psi. It should be understood that the measured values reported according to ASTM C518 typically correlate well with the measured values obtained according to EN 12667 with adjustments related to the compressive load. In certain embodiments, the aerogel material or composition of the present disclosure has a thermal conductivity of about 40 mW / m·K or less, about 30 mW / m·K or less, about 25 mW / m·K or less, about 20 mW / m·K or less, about 18 mW / m·K or less, about 16 mW / m·K or less, about 14 mW / m·K or less, about 12 mW / m·K or less, about 10 mW / m·K or less, about 5 mW / m·K or less, or within a range between any two of these values.

[0096] Thermal conductivity measurements can also be obtained at a temperature of about 10 °C at atmospheric pressure under compression. Thermal conductivity measurements at 10 °C are generally 0.5 to 0.7 mW / m·K lower than the corresponding thermal conductivity measurements at 37.5 °C. In certain embodiments, the aerogel material or composition of the present disclosure has a thermal conductivity at 10 °C of about 40 mW / m·K or less, about 30 mW / m·K or less, about 25 mW / m·K or less, about 20 mW / m·K or less, about 18 mW / m·K or less, about 16 mW / m·K or less, about 14 mW / m·K or less, about 12 mW / m·K or less, about 10 mW / m·K or less, about 5 mW / m·K or less, or within a range between any two of these values.

[0097] Within the context of the present disclosure, the term "density" refers to a measure of the mass per unit volume of an aerogel material or composition. The term "density" generally refers to the apparent density of the aerogel material and the bulk density of the aerogel composition. Density is typically kg / m 3or recorded as g / cc. The density of the aerogel material or composition can be determined by methods known in the art such as, for example, "Standard Test Method for Dimensions and Density of Preformed Block and Board-Type Thermal Insulation" (ASTM C303, ASTM International, West Conshohocken, Pennsylvania), "Standard Test Methods for Thickness and Density of Blanket or Batt Thermal Insulations" (ASTM C167, ASTM International, West Conshohocken, Pennsylvania), "Determination of the apparent density of preformed pipe insulation" (EN 13470, British Standards Institution, UK), or "Determination of the apparent density of preformed pipe insulation" (ISO 18098, International Organization for Standardization, Switzerland) (not limited to these). Since different methods may yield different results, in the context of the present disclosure, it should be understood that density measurements are obtained in accordance with the ASTM C167 standard ("Standard Test Method for Thickness and Density of Blanket or Batt Thermal Insulations") at 2 psi compression for thickness measurements, unless otherwise stated.In certain embodiments, the aerogel material or composition of the present disclosure has a density of about 0.60 g / cc or less, about 0.50 g / cc or less, about 0.40 g / cc or less, about 0.30 g / cc or less, about 0.25 g / cc or less, about 0.20 g / cc or less, about 0.18 g / cc or less, about 0.16 g / cc or less, about 0.14 g / cc or less, about 0.12 g / cc or less, about 0.10 g / cc or less, about 0.05 g / cc or less, about 0.01 g / cc or less, or within a range between any two of these values.

[0098] In the context of the present disclosure, the term "degree of hydrophobicity" refers to a measure of the ability of an aerogel material or composition to repel water.

[0099] The degree of hydrophobicity of an aerogel material or composition can be represented by the amount of liquid water uptake. In the context of the present disclosure, the term "amount of liquid water uptake" refers to a measure of the potential ability of an aerogel material or composition to absorb or otherwise retain liquid water. The amount of liquid water uptake can be expressed as the percentage (by mass or volume) of water absorbed or otherwise retained by the aerogel material or composition when exposed to liquid water under specific measurement conditions. The liquid water absorption of an aerogel material or composition can be determined by methods known in the art, such as, but not limited to, "Standard Test Method for Determining the Water Retention (Repellency) Characteristics of Fibrous Glass Insulation" (ASTM C1511, ASTM International, West Conshohocken, Pennsylvania), "Standard Test Method for Water Absorption by Immersion of Thermal Insulation Materials" (ASTM C1763, ASTM International, West Conshohocken, Pennsylvania), "Thermal insulating products for building applications: Determination of short term water absorption by partial immersion" (EN 1609, British Standards Institution, United Kingdom). Since different methods may yield different results, in the context of the present disclosure, it should be understood that the measured value of the liquid uptake is obtained in accordance with the ASTM C1511 standard ("Standard Test Method for Determining the Water Retention (Repellency) Characteristics of Fibrous Glass Insulation (Aircraft Type)") under ambient pressure and temperature, unless otherwise specified.In certain embodiments, the aerogel material or composition of the present disclosure can have a liquid water uptake of about 50 wt% or less, about 40 wt% or less, about 30 wt% or less, about 20 wt% or less, about 15 wt% or less, about 10 wt% or less, about 8 wt% or less, about 3 wt% or less, about 2 wt% or less, about 1 wt% or less, about 0.1 wt% or less, or in the range between any two of these values. An aerogel material or composition having an improved liquid water uptake compared to other aerogel materials or compositions has a lower ratio of liquid water uptake / retention compared to a reference aerogel material or composition.

[0100] The degree of hydrophobicity of an aerogel material or composition can be represented by the water vapor uptake. In the context of the present disclosure, the term "water vapor uptake" refers to a measure of the potential ability of an aerogel material or composition to absorb water vapor. The water vapor uptake can be expressed as the percentage (by mass) of water absorbed or otherwise retained by the aerogel material or composition when exposed to water vapor under specific measurement conditions. The water vapor uptake of an aerogel material or composition can be determined by methods known in the art, such as, but not limited to, "Standard Test Method for Determining the Water Vapor Sorption of Unfaced Mineral Fiber Insulation" (ASTM C1104, ASTM International, West Conshohocken, Pennsylvania), "Thermal insulating products for building applications: Determination of long term water absorption by diffusion" (EN 12088, British Standards Institution, United Kingdom). Since different methods may yield different results, in the context of the present disclosure, the measured value of the water vapor uptake is, unless otherwise stated, obtained in accordance with the ASTM C1104 standard (modified from 96 hours to 24 hours at 49 °C and 95% humidity under ambient pressure), and it should be understood that it is obtained in accordance with the ASTM C1104 standard (Standard Test Method for Determining the Water Vapor Sorption of Unfaced Mineral Fiber Insulation). In certain embodiments, the aerogel material or composition of the present disclosure can have a water vapor uptake of about 50 wt% or less, about 40 wt% or less, about 30 wt% or less, about 20 wt% or less, about 15 wt% or less, about 10 wt% or less, about 8 wt% or less, about 3 wt% or less, about 2 wt% or less, about 1 wt% or less, about 0.1 wt% or less, or within a range between any two of these values.An aerogel material or composition with improved water vapor uptake compared to another aerogel material or composition has a lower ratio of water vapor uptake / retention compared to a reference aerogel material or composition.

[0101] The hydrophobicity degree of an aerogel material or composition can be represented by measuring the equilibrium contact angle of water droplets at the interface with the surface of the material. The aerogel material or composition of the present disclosure can have a water contact angle of about 90° or more, about 120° or more, about 130° or more, about 140° or more, about 150° or more, about 160° or more, about 170° or more, about 175° or more, or within the range between any two of these values.

[0102] Within the context of the present disclosure, the terms "heat of combustion", "HOC" and "ΔH" C" refers to the measured amount of thermal energy released during the combustion or exothermic pyrolysis of a material or composition. The heat of combustion is typically recorded in calories per gram (cal / g) of the aerogel material or composition released, or as megajoules per kilogram (MJ / kg) of the thermal energy released per kilogram of the material or composition. The heat of combustion of a material or composition can be determined by methods known in the art, and such methods include, but are not limited to, "Reaction to fire tests for products - Determination of the gross heat of combustion (calific value)" (EN ISO 1716, International Organization for Standardization, Switzerland; adopted as EN). In the context of the present disclosure, the heat of combustion measurement is obtained in accordance with "Reaction to fire tests for products - Determination of the gross heat of combustion" (EN ISO 1716 standard) unless otherwise specified. In certain embodiments, the aerogel composition of the present disclosure can have a heat of combustion of about 750 cal / g or less, about 717 cal / g or less, about 700 cal / g or less, about 650 cal / g or less, about 600 cal / g or less, about 575 cal / g or less, about 550 cal / g or less, about 500 cal / g or less, about 450 cal / g or less, about 400 cal / g or less, about 350 cal / g or less, about 300 cal / g or less, about 250 cal / g or less, about 200 cal / g or less, about 150 cal / g or less, about 100 cal / g or less, about 50 cal / g or less, about 25 cal / g or less, about 10 cal / g or less, or within a range between any two of these values. An aerogel composition having an improved heat of combustion compared to another aerogel composition has a lower heat of combustion value compared to a reference aerogel composition. In certain embodiments of the present disclosure, the HOC of the aerogel composition is improved by incorporating a fire resistance class additive into the aerogel composition.

[0103] In the context of the present disclosure, all thermal analyses and related definitions refer to measurements performed by starting at 25°C and increasing to 1000°C at a rate of 20°C per minute in ambient air at normal pressure. Thus, any variations in these parameters (or re - execution under these conditions) must be considered when measuring and calculating the thermal decomposition onset point, peak heat release temperature, peak endothermic temperature, etc. In the context of the present disclosure, the terms "thermal decomposition onset point" and "T D " refer to the measurement of the lowest temperature of environmental heat at which a rapid exothermic reaction from the decomposition of an organic material appears within the material or composition. The thermal decomposition onset point of the organic material in a material or composition can be measured using thermogravimetric analysis (TGA). The TGA curve of a material represents the mass loss (% mass) of the material when exposed to an increase in ambient temperature and indicates thermal decomposition. The thermal decomposition onset point of a material can be correlated with the intersection of the following tangents of the TGA curve: a line tangent to the baseline of the TGA curve and a line tangent to the TGA curve at the point of maximum gradient between the baseline of the TGA curve and the rapid exothermic decomposition event associated with the decomposition of the organic material. In the context of the present disclosure, the measured value of the thermal decomposition onset point of an organic material is obtained using TGA analysis as provided in this paragraph unless otherwise stated.

[0104] The thermal decomposition start point of a material can also be measured using differential scanning calorimetry (DSC) analysis. The DSC curve of a material represents the thermal energy (mW / mg) released when the material is subjected to a gentle increase in ambient temperature. The onset of the thermal decomposition temperature of a material can be correlated with the point within the DSC curve where ΔmW / mg (change in thermal energy output) increases maximally, and thus indicates exothermic heat generation from the aerogel material. In the context of the present disclosure, the measured value of the thermal decomposition start point using DSC, TGA, or both is obtained using a temperature ramp rate of 20 °C / min, as further defined in the preceding paragraph, unless otherwise explicitly stated. DSC and TGA each provide similar values for this thermal decomposition start point, and often the tests are performed simultaneously so that results are obtained from both. In certain embodiments, the aerogel material or composition of the present disclosure has a thermal decomposition start point of about 300 °C or higher, about 320 °C or higher, about 340 °C or higher, about 360 °C or higher, about 380 °C or higher, about 400 °C or higher, about 420 °C or higher, about 440 °C or higher, about 460 °C or higher, about 480 °C or higher, about 500 °C or higher, about 550 °C or higher, about 600 °C or higher, or within a range between any two of these values. Within the context of this specification, for example, the fact that a first composition has a higher thermal decomposition start point than a second composition is considered an improvement of the first composition over the second composition. In this specification, it is contemplated that the thermal decomposition start point of a composition or material increases when one or more refractory class additives are added compared to a composition that does not contain refractory class additives.

[0105] In the context of the present disclosure, "the start point of endothermic decomposition" and "T" EDThe term "___" refers to the measured value of the lowest temperature of the ambient heat at which an endothermic reaction from decomposition or dehydration appears within a material or composition. The onset point of endothermic decomposition of a material or composition can be measured using thermogravimetric analysis (TGA). The TGA curve of a material shows the mass loss (mass %) of the material when it is exposed to an increase in ambient temperature. The onset point of thermal decomposition of a material may correlate with the intersection of the following tangents of the TGA curve: a line tangent to the baseline of the TGA curve, and a line tangent to the TGA curve at the point of maximum gradient during rapid endothermic decomposition or dehydration of the material. Within the context of the present disclosure, the measured value of the onset point of endothermic decomposition of a material or composition is obtained using TGA analysis as provided in this paragraph unless otherwise stated.

[0106] In the context of the present disclosure, "increase in furnace temperature" and "ΔT" R The term "___" refers to the maximum temperature (T MAX ) of a material or composition under pyrolysis conditions and the baseline temperature of that material or composition under pyrolysis conditions (usually the final temperature, or T FINRefers to the measured value of the difference from (). The increase in the furnace temperature is usually recorded in degrees Celsius or °C. The increase in the furnace temperature of a material or composition can be determined by methods known in the art, such as, but not limited to, "Reaction to fire tests for building and transport products: Non-combustibility test" (EN ISO 1182, International Organization for Standardization, Switzerland; EN adopted). In the context of the present disclosure, the measured value of the increase in the furnace temperature is obtained under conditions equivalent to the EN ISO 1182 standard (Reaction to fire tests for building and transport products: Non-combustibility test), unless otherwise stated. In certain embodiments, the aerogel composition of the present disclosure can have an increase in the furnace temperature of about 100 °C or less, about 90 °C or less, about 80 °C or less, about 70 °C or less, about 60 °C or less, about 50 °C or less, about 45 °C or less, about 40 °C or less, about 38 °C or less, about 36 °C or less, about 34 °C or less, about 32 °C or less, about 30 °C or less, about 28 °C or less, about 26 °C or less, about 24 °C or less, or within the range between any two of these values. In the context of the stability of the composition at high temperatures, for example, if a first composition has a lower increase in the furnace temperature than a second composition, this is considered an improvement of the first composition over the second composition. It is contemplated herein that the increase in the furnace temperature of the composition is reduced when one or more fire resistance class additives are added as compared to a composition that does not contain any fire resistance class additives.

[0107] In the context of the present disclosure, "flame time" and "T" FLAMEThe term "___" refers to the measurement of a sustained flame of a material or composition under pyrolysis conditions, where "sustained flame" is the persistence of a flame at any part on the visible portion of the test piece that lasts for 5 seconds or more. The flame time is usually recorded in seconds or minutes. The flame time of a material or composition can be determined by methods known in the art such as, but not limited to, "Reaction to Fire Tests for Building and Transport Products: Non-combustibility Test" (EN ISO 1182, International Organization for Standardization, Switzerland; EN adopted). In the context of the present disclosure, the measurement of the flame time is obtained under conditions equivalent to the EN ISO 1182 standard (Reaction to Fire Tests for Building and Transport Products: Non-combustibility Test) unless otherwise stated. In certain embodiments, the aerogel composition of the present disclosure has a flame time of about 30 seconds or less, about 25 seconds or less, about 20 seconds or less, about 15 seconds or less, about 10 seconds or less, about 5 seconds or less, about 2 seconds or less, or within the range between any two of these values. Within the context of this specification, for example, the fact that a first composition has a shorter flame time than a second composition is considered an improvement of the first composition over the second composition. In the context of this specification, it is contemplated that the flame time of a composition is reduced when one or more fire class additives are added as compared to a composition that does not contain any fire class additives.

[0108] In the context of the present disclosure, the terms "mass loss" and "ΔM" refer to a measure of the amount of material, composition, or component that is lost or burned out under pyrolysis conditions. Mass loss is typically recorded as mass % or wt%. The mass loss of a material, composition, or composite can be determined by methods known in the art, such as the EN ISO 1182 standard (Reaction to fire tests for building products and transportable products: Non-combustibility test). In the context of the present disclosure, measurements of mass loss are obtained under conditions equivalent to the EN ISO 1182 standard (Reaction to fire tests for building products and transportable products: Non-combustibility test) unless otherwise specified. In certain embodiments, the aerogel compositions of the present disclosure can have a mass loss of about 50% or less, about 40% or less, about 30% or less, about 28% or less, about 26% or less, about 24% or less, about 22% or less, about 20% or less, about 18% or less, about 16% or less, or within a range between any two of these values. In the context of this specification, for example, if a first composition has a lower mass loss than a second composition, this is considered an improvement of the first composition over the second composition. In the context of this specification, it is contemplated that the mass loss of a composition will be reduced when one or more fire class additives are added as compared to a composition that does not contain any fire class additives.

[0109] In the context of the present disclosure, the term "peak heat release temperature" refers to a measure of the temperature of the ambient heat at which the exothermic heat release from decomposition is at a maximum. The peak heat release temperature of a material or composition can be measured using thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), or a combination thereof. DSC and TGA each provide similar values for the peak heat release temperature, and often the tests are performed simultaneously so that results are obtained from both. In a typical DSC analysis, the heat flow is plotted against the increasing temperature, and the peak heat release temperature is the temperature at which the highest peak appears in such a curve. In the context of the present disclosure, measurements of the peak heat release temperature of a material or composition are obtained using TGA analysis as provided in this paragraph unless otherwise specified.

[0110] In the context of endothermic substances, the term "peak endothermic temperature" refers to the measured value of the environmental heat temperature at which the endothermic heat absorption due to decomposition is at a minimum. The peak endothermic temperature of a material or composition can be measured using thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), or a combination thereof. In a typical DSC analysis, the heat flow is plotted against the rising temperature, and the peak endothermic temperature is the temperature at which the lowest peak appears in such a curve. In the context of the present disclosure, the measurement of the peak endothermic temperature of a material or composition is obtained using TGA analysis as provided in this paragraph, unless otherwise specified.

[0111] Within the context of the present disclosure, the terms "low-flammability" and "low-flammable" refer to a material or composition that satisfies the following combination of properties: i) an increase in furnace temperature of 50°C or less, ii) a flame time of 20 seconds or less, and iii) a mass loss of 50 wt% or less. In the context of the present disclosure, the terms "non-flammability" and "non-flammable" refer to a material or composition that satisfies the following combination of properties: i) an increase in furnace temperature of 40°C or less, ii) a flame time of 2 seconds or less, and iii) a mass loss of 30 wt% or less. As described herein, it is contemplated that the flammability of a composition (e.g., a combination of an increase in furnace temperature, flame time, and mass loss) is reduced by containing one or more fire class additives.

[0112] Within the context of the present disclosure, the terms "low-combustibility" and "low-combustible" refer to a low-combustible material or composition having a total heat of combustion (HOC) of 3 MJ / kg or less. In the context of the present disclosure, the terms "non-combustibility" and "non-combustible" refer to a non-combustible material or composition having a heat of combustion (HOC) of 2 MJ / kg or less. It is contemplated that the HOC of a composition is reduced by containing one or more fire class additives as described herein.

[0113] An aerogel is described as a framework of an interconnected structure most commonly composed of oligomers, polymers, or colloidal particles that are interconnected. The aerogel framework can be made from a variety of precursor materials, including inorganic precursor materials (such as precursors used to produce silica-based aerogels), organic precursor materials (such as precursors used to produce carbon-based aerogels), inorganic / organic hybrid precursor materials, and combinations thereof. In the context of the present disclosure, the term "amalgam aerogel" refers to an aerogel produced from a combination of two or more different gel precursors, and the corresponding precursors are referred to as "amalgam precursors".

[0114] Inorganic aerogels are generally formed from metal oxide or metal alkoxide materials. The metal oxide or metal alkoxide material can be based on the oxide or alkoxide of any metal that can form an oxide. Such metals include, but are not limited to, silicon, aluminum, titanium, zirconium, hafnium, yttrium, vanadium, cerium, and the like. Inorganic silica aerogels have conventionally been produced by hydrolysis and condensation of silica-based alkoxides (such as tetraethoxysilane), or by gelation of silicic acid or water glass. Other related inorganic precursor materials for silica-based aerogel synthesis include, but are not limited to, metal silicates such as sodium silicate or potassium silicate, alkoxysilanes, partially hydrolyzed alkoxysilanes, tetraethoxysilane (TEOS), partially hydrolyzed TEOS, condensation polymers of TEOS, tetramethoxysilane (TMOS), partially hydrolyzed TMOS, condensation polymers of TMOS, tetra-n-propoxysilane, partially hydrolyzed and / or condensation polymers of tetra-n-propoxysilane, polyethylsilicate, partially hydrolyzed polyethylsilicate, monomeric alkylalkoxysilane, bis-trialkoxyalkyl or arylsilane, polyhedral silsesquioxane, or combinations thereof.

[0115] In certain embodiments of the present disclosure, for example, pre-hydrolyzed TEOS such as Silbond H-5 (SBH5, Silbond Corp) hydrolyzed at a water / silica ratio of about 1.9 to 2 can be used commercially and may be further hydrolyzed before being incorporated into the gelation process. Partially hydrolyzed TEOS or TMOS such as polysilicate (Silbond 40) or polymethylsilicate can also be used commercially or may be further hydrolyzed before being incorporated into the gelation process.

[0116] Examples of inorganic aerogels can also include gel precursors containing at least one hydrophobic group such as alkyl metal alkoxides, cycloalkyl metal alkoxides, aryl metal alkoxides, etc., which can impart or improve specific properties in the gel such as stability and hydrophobicity. Specifically, inorganic silica aerogels can include hydrophobic precursors such as alkylsilanes or arylsilanes. Hydrophobic gel precursors can be used as the primary precursor material for forming the skeleton of the gel material. However, hydrophobic gel precursors are more commonly used as co-precursors in combination with simple metal alkoxides in the formation of amalgam aerogels. Examples of hydrophobic inorganic precursor materials for silica-based aerogel synthesis include trimethylmethoxysilane (TMS), dimethyldimethoxysilane (DMS), methyltrimethoxysilane (MTMS), trimethylethoxysilane, dimethyldiethoxysilane (DMDS), methyltriethoxysilane (MTES), ethyltriethoxysilane (ETES), diethyldiethoxysilane, ethyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane (PhTES), hexamethyldisilazane, hexaethyldisilazane, etc., but are not limited thereto. Any derivatives of the above precursors may be used, specifically, specific polymer groups or other chemical groups may be added or cross-linked to one or more of the above precursors.

[0117] The aerogel may be treated to impart or improve hydrophobicity. The hydrophobic treatment can be applied to the sol-gel solution, the wet gel before liquid extraction, or the aerogel after liquid extraction. The hydrophobic treatment is particularly common in the production of metal oxide aerogels such as silica aerogels. Examples of the hydrophobization treatment of the gel will be discussed in more detail below, specifically in the context of treating a silica wet gel. However, the specific examples and illustrations provided herein are not intended to limit the scope of the disclosure to any particular type of hydrophobic treatment procedure or aerogel substrate. The disclosure encompasses related hydrophobic treatment methods for aerogels in either the form of a wet gel or a dry aerogel, in addition to any gels or aerogels known to those skilled in the art.

[0118] The hydrophobic treatment is carried out by reacting a hydroxy moiety on the gel, such as a silanol group (Si-OH) present on the skeleton of the silica gel, with a functional group of the hydrophobizing agent. The resulting reaction converts the silanol group (Si-OH) and the hydrophobizing agent into a hydrophobic group present on the skeleton of the silica gel. The hydrophobizing agent compound can react with the hydroxyl group on the gel according to the following reaction: R N MX 4-N (Hydrophobizing agent) + MOH (Silanol) → MOMR N (Hydrophobic group) + HX. The hydrophobic treatment can be carried out on both the outer macro surface of the silica gel and the inner pore surface within the porous network of the gel.

[0119] The gel can be immersed in a mixture of a hydrophobizing agent and any hydrophobic treatment solvent in which the hydrophobizing agent is soluble and miscible with the gel solvent in the wet gel. A wide range of hydrophobic treatment solvents can be used, including solvents such as methanol, ethanol, isopropanol, xylene, toluene, benzene, dimethylformamide, hexane, etc. Also, a liquid or gaseous hydrophobizing agent may be brought into direct contact with the gel to impart hydrophobicity.

[0120] The hydrophobic treatment process can include mixing or stirring to assist the penetration of the hydrophobizing agent into the wet gel. The hydrophobic treatment process may also include varying other conditions such as temperature and pH to further enhance and optimize the treatment reaction. After the reaction is completed, the wet gel is washed to remove unreacted compounds and reaction by-products.

[0121] The hydrophobizing agent for the hydrophobic treatment of aerogel is represented by the general formula R N MX 4-N (wherein M is a metal, R is a hydrophobic group such as CH3, CH2CH3, C6H6, or a similar hydrophobic alkyl, cycloalkyl or aryl moiety, etc., and X is a halogen, usually Cl). Specific examples of the hydrophobizing agent include, but are not limited to, trimethylchlorosilane (TMCS), triethylchlorosilane (TECS), triphenylchlorosilane (TPCS), dimethylchlorosilane (DMCS), dimethyldichlorosilane (DMDCS), etc. Further, the hydrophobizing agent may be represented by the formula Y(R3M)2 (wherein M is a metal, Y is a cross-linking group such as NH or O, etc., and R is a hydrophobic group such as CH3, CH2CH3, C6H6, or a similar hydrophobic alkyl, cycloalkyl or aryl moiety, etc.). Specific examples of such hydrophobizing agents include, but are not limited to, hexamethyldisilazane [HMDZ], hexamethyldisiloxane [HMDSO], etc. The hydrophobizing agent may further include a compound represented by the formula R N MV 4-N (wherein V is a reactive group or leaving group other than a halogen). Specific examples of such hydrophobizing agents include, but are not limited to, hydrophobizing agents such as vinyltriethoxysilane and vinyltrimethoxysilane.

[0122] The hydrophobic treatment of the present invention may also be carried out during the removal, exchange or drying of the liquid in the gel. In certain embodiments, the hydrophobic treatment may be carried out in a supercritical fluid environment (such as, but not limited to, supercritical carbon dioxide, etc.) and may be carried out in combination with a drying or extraction step.

[0123] In the context of the present disclosure, the term "hydrophobic-bound silicon" refers to silicon atoms within the backbone of a gel or aerogel that contain at least one hydrophobic group covalently bonded to a silicon atom. Examples of hydrophobic-bound silicon include, but are not limited to, silicon atoms within silica groups within a gel backbone formed from a gel precursor (e.g., MTES or DMDS) containing at least one hydrophobic group. Also, examples of hydrophobic-bound silicon include, but are not limited to, silicon atoms within or on the surface of a gel backbone that have been treated with a hydrophobizing agent (e.g., HMDZ) to impart or improve hydrophobicity by incorporating additional hydrophobic groups into the composition. Hydrophobic groups of the present disclosure include, but are not limited to, methyl, ethyl, propyl, isopropyl, butyl, isobutyl, tert-butyl, octyl, phenyl, or other substituted or unsubstituted hydrophobic organic groups known to those skilled in the art. In the context of the present disclosure, the terms "hydrophobic group", "hydrophobic organic material", and "hydrophobic organic content" specifically exclude readily hydrolyzable organosilicon-bonded alkoxy groups on the backbone of the gel material that are the product of the reaction between an organic solvent and a silanol group. Such excluded groups can be distinguished from this hydrophobic organic content by NMR analysis. The amount of hydrophobic-bound silicon contained in the aerogel can be analyzed using NMR spectroscopy such as CP / MAS 29 Si solid NMR. NMR analysis of the aerogel enables the characterization and relative quantification of M-type hydrophobic-bound silicon (e.g., monofunctional silica such as TMS derivatives); D-type hydrophobic-bound silicon (e.g., bifunctional silica such as DMDS derivatives); T-type hydrophobic-bound silicon (e.g., trifunctional silica such as MTES derivatives); and Q-type silicon (e.g., tetrafunctional silica such as TEOS derivatives). Also, NMR analysis can classify a particular type of hydrophobic-bound silicon into subtypes (e.g., classifying T-type hydrophobic-bound silicon into T 1 species, T 2It can be used to analyze the bonding chemistry of hydrophobic bonded silicon contained in the aerogel by enabling classification into three types, namely, type M, type D, and type T. Specific details regarding the NMR analysis of the silica material can be found in the paper by Geppi et al., "Applications of Solid-State NMR to the Study of Organic / Inorganic Multicomponent Materials," specifically on pages 7 - 9 (Appl. Spec. Rev. (2008), 44 - 1: 1 - 89), and the specifically cited pages are incorporated by reference.

[0124] CP / MAS 29 The characterization of hydrophobic bonded silicon in the NMR analysis of Si can be based on the following chemical shift peaks: M 1 (30 to 10 ppm); D 1 (10 to -10 ppm), D 2 (-10 to -20 ppm); T 1 (-30 to -40 ppm), T 2 (-40 to -50 ppm), T 3 (-50 to -70 ppm); Q 2 (-70 to -85 ppm), Q 3 (-85 to -95 ppm), Q 4 (-95 to -110 ppm). These chemical shift peaks are approximate and illustrative and are not intended to be limiting or definitive. The exact chemical shift peaks due to the various silicon species within the material may depend on the specific chemical composition of the material and can generally be deciphered by routine experiments and analysis by those skilled in the art.

[0125] In the context of the present disclosure, the terms "hydrophobic organic content" or "hydrophobe content" or "hydrophobic content" refer to the amount of hydrophobic organic material bound to the backbone in an aerogel material or composition. The hydrophobic organic content of an aerogel material or composition can be expressed as a mass percentage of the amount of hydrophobic organic material on the aerogel backbone relative to the total amount of materials in the aerogel material or composition. The hydrophobic organic content can be calculated by one skilled in the art based on the nature and relative concentrations of the materials used to manufacture the aerogel material or composition. The hydrophobic organic content can also be measured using thermogravimetric analysis (TGA) of the material of interest, preferably under an oxygen atmosphere (although TGA under alternative gas environments can also be useful). Specifically, the percentage of hydrophobic organic material in the aerogel can be correlated with the percentage of mass loss in the hydrophobic aerogel material or composition when exposed to the combustion heat temperature during TGA analysis, with adjustments made for the loss of moisture, residual solvents, and readily hydrolyzable alkoxy groups during TGA analysis. To measure and determine the hydrophobic content in the aerogel compositions of the present invention, other alternative techniques may be used, such as differential scanning calorimetry, elemental analysis (especially carbon), chromatography techniques, nuclear magnetic resonance spectra, and other analytical techniques known to those skilled in the art. In certain cases, a combination of known techniques may be useful or necessary when determining the hydrophobic content of the aerogel compositions of the present invention.

[0126] The aerogel materials or compositions of the present disclosure can have a hydrophobic organic content of 50 wt% or less, 40 wt% or less, 30 wt% or less, 25 wt% or less, 20 wt% or less, 15 wt% or less, 10 wt% or less, 8 wt% or less, 6 wt% or less, 5 wt% or less, 4 wt% or less, 3 wt% or less, 2 wt% or less, 1 wt% or less, or within a range between any two of these values.

[0127] The term "fuel content" refers to the total amount of combustible materials in an aerogel material or composition, which can be correlated with the total percentage of mass loss in the aerogel material or composition when exposed to the combustible heat temperature during TGA or TG-DSC analysis, with adjustments made for moisture loss. Examples of the fuel content of an aerogel material or composition can include hydrophobic organic content, and other combustible residual alcohol solvents, fillers, reinforcing materials, and readily hydrolyzable alkoxy groups.

[0128] Organic aerogels are generally formed from carbon-based polymer precursors. Such polymer materials can include, but are not limited to, resorcinol formaldehyde (RF), polyimide, polyacrylate, polymethyl methacrylate, acrylate oligomer, polyoxyalkylene, polyurethane, polyphenol, polybutadiene, trialkoxysilyl-terminated polydimethylsiloxane, polystyrene, polyacrylonitrile, polyfurfural, melamine-formaldehyde, cresol formaldehyde, phenol-furfural, polyether, polyol, polyisocyanate, polyhydroxybenzene, polyvinyl alcohol dialdehyde, polycyanurate, polyacrylamide, various epoxy resins, agar, agarose, chitosan, and combinations thereof. As an example, organic RF aerogels are typically produced from the sol-gel polymerization of resorcinol or melamine and formaldehyde under alkaline conditions.

[0129] Organic / inorganic hybrid aerogels are mainly composed of (organically modified silica ("ormosil") aerogels. These ormosil materials contain organic components covalently bonded to the silica network. Ormosils are typically formed by the hydrolysis and condensation of organically modified silanes R-Si(OX)3 with conventional alkoxide precursors Y(OX)4. In these formulas, X can represent, for example, CH3, C2H5, C3H7, C4H9, Y can represent, for example, Si, Ti, Zr or Al, and R can be any organic fragment such as methyl, ethyl, propyl, butyl, isopropyl, methacrylate, acrylate, vinyl, epoxide, etc. Also, the organic components in the ormosil aerogel may be dispersed throughout the silica network or chemically bonded.

[0130] In the context of the present disclosure, the term "ormosil" encompasses the aforementioned materials and other organically modified materials, and is sometimes also referred to as "ormocers". Ormosils are often used as coatings in which the ormosil film is cast onto a substrate, for example, by a sol-gel process. Examples of other organic-inorganic hybrid aerogels of the present disclosure include, but are not limited to, silica-polyether, silica-PMMA, silica-chitosan, carbides, nitrides, and other combinations of the aforementioned organic and inorganic aerogel-forming compounds. The published U.S. Patent (Patent Application No. 20050192367 (paragraphs

[0022] -

[0038] and

[0044] -

[0058] )) includes teachings of such hybrid organic-inorganic materials, which are incorporated herein by reference for the individually cited sections and paragraphs.

[0131] In certain embodiments, the aerogel of the present disclosure is preferably an inorganic silica aerogel mainly formed from a prepolymerized silica precursor as an oligomer or a hydrolyzed silicate ester formed from a silicon alkoxide in an alcohol solvent. In certain embodiments, such a prepolymerized silica precursor or hydrolyzed silicate ester may be formed in situ from other precursors or silicate esters such as alkoxysilanes or water glass. However, the present disclosure can generally be implemented using any other aerogel composition known in the art and is not limited to one precursor material or an amalgam mixture of precursor materials.

[0132] The production of aerogels generally includes the following steps: i) forming a sol-gel solution, ii) forming a gel from the sol-gel solution, and iii) extracting the solvent from the gel material by innovative treatment and extraction to obtain a dried aerogel material. This process will be discussed in more detail below, specifically in the context of forming inorganic aerogels such as silica aerogels. However, the specific examples and illustrations provided herein are not intended to limit the present disclosure to any particular type of aerogel and / or manufacturing method. The present disclosure may include any aerogel formed by any related manufacturing method known to those skilled in the art, unless otherwise specified.

[0133] The first step in forming an inorganic aerogel generally involves forming a sol-gel solution by hydrolysis and condensation of a silica precursor, such as, but not limited to, metal alkoxide precursors, in an alcohol-based solvent. The main variables in the formation of the inorganic aerogel include the type of alkoxide precursor contained in the sol-gel solution, the nature of the solvent, the processing temperature and pH of the sol-gel solution (which can be varied by addition of an acid or base), and the precursor / solvent / water ratio in the sol-gel solution. Control of these variables in forming the sol-gel solution can enable control of the growth and aggregation of the gel skeleton during the subsequent transition of the gel material from the "sol" state to the "gel" state. The properties of the resulting aerogel are affected by the pH of the precursor solution and the molar ratio of the reactants, but any pH and any molar ratio that enable gel formation can be used in the present disclosure.

[0134] A sol-gel solution is formed by combining at least one gelling precursor with a solvent. Suitable solvents for use in forming a sol-gel solution include lower alcohols having 1 to 6 carbon atoms, particularly 2 to 4 carbon atoms, although other solvents can be used as known to those skilled in the art. Examples of useful solvents include, but are not limited to, methanol, ethanol, isopropanol, ethyl acetate, ethyl acetoacetate, acetone, dichloromethane, tetrahydrofuran, etc. Also, multiple solvents may be combined to achieve a desired degree of dispersion or to optimize the properties of the gel material. The selection of the optimal solvent for the sol-gel formation step and the gel formation step thus depends on the specific precursors, fillers and additives incorporated into the sol-gel solution, and the targeted processing conditions for gelation and liquid extraction, and the desired properties of the final aerogel material.

[0135] Water may be present in the precursor-solvent solution. Water acts to hydrolyze the metal alkoxide precursor to a metal hydroxide precursor. The hydrolysis reaction can be Si(OC2H5)4 + 4H2O → Si(OH)4 + 4(C2H5OH) (using TEOS in ethanol solvent as an example). The resulting hydrolyzed metal hydroxide precursor remains suspended in the solvent solution in a "sol" state as individual molecules or as small polymeric (or oligomerized) colloidal clusters of molecules. For example, the polymerization / condensation of the Si(OH)4 precursor can occur as follows: 2Si(OH)4 = (OH)3Si-O-Si(OH)3 + H2O. This polymerization can continue until colloidal clusters of polymerized (or oligomerized) SiO2 (silica) molecules are formed.

[0136] Acids and bases can be incorporated into the sol-gel solution to control the pH of the solution and catalyze the hydrolysis and condensation reactions of the precursor materials. Any acid can be used to catalyze the precursor reaction and obtain a solution of lower pH, and exemplary acids include HCl, H2SO4, H3PO4, oxalic acid, and acetic acid. Similarly, any base can be used to catalyze the precursor reaction and obtain a solution of higher pH, and an exemplary base includes NH4OH.

[0137] The sol-gel solution can further contain co-gelling precursors in addition to filler materials and other additives. The filler and other additives may be administered into the sol-gel solution at any point before or during gel formation. The filler material and other additives may be incorporated into the gel material after gelation by various techniques known to those skilled in the art. In certain embodiments, the sol-gel solution containing the gelling precursor, solvent, catalyst, water, filler, and other additives is a homogeneous solution capable of effective gel formation under appropriate conditions.

[0138] Once a sol-gel solution is formed and optimized, the gel-forming components in the sol-gel can be transferred to a gel material. The process of transferring the gel-forming components to the gel material includes an initial gel-forming process in which the gel solidifies to the gelation point of the gel material. The gelation point of the gel material can be regarded as the point at which the gelling solution shows resistance to flow and / or the point at which a substantially continuous polymer backbone is formed throughout its volume. Various gel-forming techniques are known to those skilled in the art. Examples include maintaining the mixture in a static state for a sufficient period of time, adjusting the pH of the solution, adjusting the temperature of the solution, directly applying certain types of energy (ultraviolet light, visible light, infrared light, microwaves, ultrasonic waves, particle beams, electromagnetic radiation) to the mixture, or combinations thereof, but are not limited thereto.

[0139] The process of transferring the gel-forming components (gel precursors) to the gel material may include an aging (also called curing) process before liquid extraction or removing the solvent from the gel (also called drying the gel). Aging the gel material after reaching the gelation point can further strengthen the gel skeleton by increasing the number of cross-links within the network. The aging period of the gel can be adjusted to control various properties within the resulting aerogel material. This aging procedure can be useful for preventing potential volume loss and shrinkage during liquid extraction. Aging can include maintaining the gel (before extraction) in a static state for a long time, maintaining the gel at a high temperature, adding cross-linking promoting compounds, or any combination thereof. The preferred temperature for aging is typically about 10°C to about 100°C, but other suitable temperatures are also contemplated herein. The aging of the gel material typically continues until liquid extraction of the wet gel material.

[0140] The period for transferring the gel-forming material (gel precursor) to the gel material includes both the initial gel-forming period (from the start of gelation to the gelation point) and any subsequent curing and aging period of the gel material prior to liquid extraction from the gel or removal of the solvent (also referred to as drying of the gel) (from the gelation point to the start of liquid extraction / solvent removal). The total time for transferring the gel-forming material to the gel material is typically between about 1 minute and several days, typically about 30 hours or less, about 24 hours or less, about 15 hours or less, about 10 hours or less, about 6 hours or less, about 4 hours or less, about 2 hours or less, preferably about 1 hour or less, about 30 minutes or less, about 15 minutes or less, or about 10 minutes or less.

[0141] In another embodiment, the resulting gel material may be washed with a suitable secondary solvent in place of the primary reaction solvent present in the wet gel. Such secondary solvents can be linear monohydric alcohols having one or more aliphatic carbon atoms, dihydric alcohols having two or more carbon atoms, branched alcohols, cyclic alcohols, cycloaliphatic alcohols, aromatic alcohols, polyhydric alcohols, ethers, ketones, cyclic ethers, or derivatives thereof. In another embodiment, the resulting gel material may be washed with an additional amount of the same solvent present in the gel material, thereby removing, in particular, unwanted by-products or other precipitates in the gel material.

[0142] Once the gel material is formed and processed, the liquid of the gel can then be at least partially extracted from the wet gel using an extraction method including innovative processing and extraction techniques to form an aerogel material. The extraction of the liquid plays an important role, in particular, in engineeringly controlling the properties of the aerogel such as porosity and density, as well as related properties such as thermal conductivity. Generally, when the liquid is extracted from the gel in a manner that results in low shrinkage of the porous network and framework of the wet gel, an aerogel is obtained. This extraction of the liquid is sometimes referred to as solvent removal or drying.

[0143] An example of an alternative method of forming a silica aerogel uses a metal oxide salt such as sodium silicate, also known as water glass. The water glass solution is first produced by mixing sodium silicate with water and an acid to form a silicic acid precursor solution. The salt by-products can be removed from the silicic acid precursor by ion exchange, surfactant separation, membrane filtration, or other chemical or physical separation techniques. The resulting sol can then be gelled, for example by the addition of a base catalyst, to produce a hydrogel. The hydrogel can be washed to remove residual salts or reactants. Removal of water from the pores of the gel can be accomplished via exchange with a polar organic solvent such as ethanol, methanol, acetone, etc. Next, the liquid in the gel is at least partially extracted using innovative processing and extraction techniques. In one embodiment,

[0144] Aerogels are generally formed by removing the liquid mobile phase from the gel material at a temperature and pressure near or above the critical point of the liquid mobile phase. When the critical point is reached (near critical) or exceeded (supercritical) (i.e., the pressure and temperature of the system are at or above the critical pressure and critical temperature, respectively), a new supercritical phase different from the liquid or gas phase appears in the fluid. The solvent can then be removed without introducing the liquid-vapor interface, capillary pressure, or any associated mass transfer limitations typically associated with the liquid-vapor boundary. Furthermore, the supercritical phase is generally more miscible with organic solvents and thus has a better ability for extraction. Cosolvents and solvent exchange are also commonly used to optimize the supercritical fluid drying process.

[0145] If evaporation or extraction occurs well below the critical point, the capillary forces generated by the evaporation of the liquid may cause shrinkage and pore collapse within the gel material. Maintaining the mobile phase at a pressure and temperature near or above the critical point during the solvent extraction process reduces the negative impact of such capillary forces. In certain embodiments of the present disclosure, using near-critical conditions just below the critical point of the solvent system enables the production of aerogel materials or compositions with a sufficiently low shrinkage rate, and thus a commercially viable final product can be manufactured.

[0146] Several additional aerogel extraction techniques are known in the art, including various approaches in the use of supercritical fluids in the drying of aerogels. For example, Kistler (J. Phys. Chem. (1932) 36: 52-64) describes a simple supercritical extraction process in which the gel solvent is maintained above its critical pressure and temperature, thereby reducing evaporative capillary forces and maintaining the structural integrity of the gel network. U.S. Patent No. 4,610,863 describes an extraction process in which the gel solvent is exchanged with liquid carbon dioxide and then extracted under conditions where the carbon dioxide is in a supercritical state. U.S. Patent No. 6670402 teaches that by injecting supercritical (not liquid) carbon dioxide into an extractor that has been preheated and pre-pressurized substantially above the supercritical state, liquid is extracted from the gel by rapid solvent exchange, thereby producing an aerogel. U.S. Patent No. 5962539 describes a method for obtaining an aerogel from a polymer material in the form of a sol-gel in an organic solvent, the method comprising exchanging the organic solvent with a fluid having a critical temperature below the decomposition temperature of the polymer and extracting the fluid / sol-gel using a supercritical fluid such as supercritical carbon dioxide, supercritical ethanol or supercritical hexane to obtain an aerogel. U.S. Patent No. 6315971 discloses a process for producing a gel composition comprising drying a wet gel comprising a gel solid and a desiccant under drying conditions sufficient to reduce shrinkage of the gel during drying and removing the desiccant. U.S. Patent No. 5420168 describes a process by which a resorcinol / formaldehyde aerogel can be produced using a simple air-drying procedure. U.S. Patent No. 5565142 describes a drying technique in which the gel surface is modified to be stronger and more hydrophobic so that the gel skeleton and pores can resist collapse during ambient drying or subcritical extraction. Other examples of extracting liquid from an aerogel material are described in Nos. 5275796 and 5395805.

[0147] In one embodiment of extracting liquid from a wet gel, a supercritical fluid such as carbon dioxide is used. For example, first, the primary solvent present in the pore network of the gel is substantially exchanged with liquid carbon dioxide, and then the wet gel is heated (typically in an autoclave) above the critical temperature of carbon dioxide (about 31.06 °C), and the pressure of the system is increased to a pressure higher than the critical pressure of carbon dioxide (about 1070 psig). The pressure around the gel material can be slightly varied to facilitate the removal of liquid from the gel. Carbon dioxide can be recycled through the extraction system to facilitate the continuous removal of the primary solvent from the wet gel. Finally, the temperature and pressure are slowly returned to ambient conditions to produce a dried aerogel material. Carbon dioxide can be pretreated to a supercritical state before being injected into the extraction chamber.

[0148] In another exemplary method of forming an aerogel, it involves reducing harmful capillary pressure at the solvent / pore interface through chemical modification of the matrix material in the wet gel state via conversion of surface hydroxyl groups to hydrophobic trimethylsilyl ethers, thereby enabling liquid extraction from the gel material at temperatures and pressures below the critical point of the solvent.

[0149] In another embodiment, after freezing the liquid (solvent) in the gel material at a low temperature, the solvent can be removed from the gel material by a sublimation process. Such removal or drying of the solvent from the gel material is understood to be within the scope of the present disclosure. Such removal largely retains the gel structure and thus produces an aerogel with unique properties.

[0150] The large-scale production of aerogel materials or compositions can be complicated by the difficulties associated with the continuous formation of gel materials on a large scale and the difficulties associated with liquid extraction from large amounts of gel materials using innovative processing and extraction techniques. In certain embodiments, the aerogel materials or compositions of the present disclosure are compatible with large-scale production. In certain embodiments, the gel materials of the present disclosure can be manufactured on a large scale via a continuous casting and gelation process. In certain embodiments, the aerogel materials or compositions of the present disclosure are manufactured on a large scale that requires the use of large-scale extraction containers. Examples of the large-scale extraction containers of the present disclosure include those having a volume of about 0.1 m 3 or more, about 0.25 m 3 or more, about 0.5 m 3 or more, or about 0.75 m 3 or more.

[0151] The aerogel compositions of the present disclosure can have a thickness of about 15 mm or less, about 10 mm or less, about 5 mm or less, about 3 mm or less, about 2 mm or less, or about 1 mm or less.

[0152] The aerogel composition can be reinforced with various reinforcing materials in order to achieve a more flexible, elastic, and conformable composite product. The reinforcing material can be added to the gel at any point during the gelation process to produce a wet reinforced gel composition. The wet gel composition can then be dried to produce a reinforced aerogel composition.

[0153] The aerogel composition can be OCMF-reinforced with various continuous bubble macroporous skeletal reinforcing materials in order to achieve a more flexible, elastic, and conformable composite product. The OCMF reinforcing material can be added to the gel at any point during the gelation process prior to gelation to produce a wet reinforced gel composition. The wet gel composition can then be dried to produce an OCMF-reinforced aerogel composition. The OCMF reinforcing material can be formed from an organic polymer material such as melamine or a melamine derivative and exists in the form of a continuous sheet or panel.

[0154] The melamine OCMF material can be produced from an aqueous solution of a melamine-formaldehyde condensate. The aqueous solution of the melamine-formaldehyde condensation product is produced by combining a melamine-formaldehyde precursor with a solvent, an emulsifier / dispersant, a curing agent such as an acid, etc., and a foaming agent such as a C5-C7 hydrocarbon, etc. Next, by curing the melamine-formaldehyde solution or resin at a high temperature above the boiling point of the foaming agent, an OCMF containing a plurality of interconnected three-dimensionally branched melamine structures is obtained, and a corresponding interconnected pore network is incorporated within its skeleton. The melamine-formaldehyde precursor generally has a molar ratio of formaldehyde to melamine in the range of 5:1 to 1.3:1, typically in the range of 3.5:1 to 1.5:1. The precursor may be in the form of a powder, a spray, a resin or a solution. The solvent contained in the melamine-formaldehyde precursor solution can include an alcohol such as methanol, ethanol or butanol, etc.

[0155] The emulsifier / dispersant contained in the melamine-formaldehyde condensation liquid can include an anionic surfactant, a cationic emulsifier, or a nonionic surfactant. Useful anionic surfactants include, but are not limited to, diphenylene oxide sulfonate, alkane and alkylbenzene sulfonate, alkylnaphthalene sulfonate, olefin sulfonate, alkyl ether sulfonate, fatty alcohol sulfate, ether sulfate, α-sulfo fatty acid ester, acylaminoalkane sulfonate, acyl isethionate, alkyl ether carboxylate, N-acyl sarcosinate, alkyl and alkyl ether phosphate, etc. Useful cationic emulsifiers include, but are not limited to, alkyltriammonium salts, alkylbenzyldimethylammonium salts, or alkylpyridinium salts. Useful nonionic surfactants include, but are not limited to, alkylphenol polyglycol ethers, fatty alcohol polyglycol ethers, fatty acid polyglycol ethers, fatty acid alkanolamides, ethylene oxide-propylene oxide block copolymers, amine oxides, glycerol fatty acid esters, sorbitan esters, and alkyl polyglycosides. The emulsifier / dispersant can be added in an amount of 0.2 to 5% by mass based on the melamine-formaldehyde precursor.

[0156] The curing agent contained in the melamine-formaldehyde precursor solution can include an acidic compound. The amount of these curing agents is generally in the range of 0.01% to 20% by mass, typically in the range of 0.05% to 5% by mass, based on the melamine-formaldehyde precursor, and all of these are based on the melamine-formaldehyde precursor. Useful acidic compounds are selected from the group consisting of organic acids and inorganic acids such as hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, formic acid, acetic acid, oxalic acid, toluenesulfonic acid, amidosulfonic acid, acid anhydrides, and mixtures thereof, but are not limited thereto.

[0157] The blowing agent contained in the melamine-formaldehyde precursor solution can include a physical blowing agent or a chemical blowing agent. Useful physical blowing agents include hydrocarbons such as pentane and hexane; halogenated hydrocarbons, more specifically chlorinated and / or fluorinated hydrocarbons such as methylene chloride, chloroform, trichloroethane, chlorofluorocarbon, and hydrochlorofluorocarbon (HCFC); alcohols such as methanol, ethanol, n-propanol or isopropanol; ethers, ketones and esters such as methyl formate, ethyl formate, methyl acetate or ethyl acetate; and gases such as air, nitrogen or carbon dioxide, but are not limited thereto. In certain embodiments, it is preferred to add a physical blowing agent having a boiling point of 0 °C to 80 °C. Useful chemical blowing agents include isocyanates mixed with water (releasing carbon dioxide as an active blowing agent); carbonates and / or bicarbonates mixed with acids (releasing carbon dioxide as an active blowing agent); and azo compounds such as azodicarbonamide, but are not limited thereto. The blowing agent is present in the melamine-formaldehyde precursor solution in an amount of 0.5% to 60% by weight, particularly 1% to 40% by weight, and in certain embodiments 1.5% to 30% by weight, based on the melamine-formaldehyde precursor.

[0158] The melamine-formaldehyde precursor solution can be formed into a melamine OCMF material by heating the solution to a temperature generally above the boiling point of the blowing agent used, thereby forming an OCMF containing a plurality of interconnected three-dimensionally branched melamine structures having a corresponding network of interconnected continuous gas pores integrated within the skeleton. The introduction of thermal energy can be carried out by high-frequency radiation via electromagnetic radiation, for example, in the frequency range of 0.2 to 100 GHz, more specifically 0.5 to 10 GHz, at 5 to 400 kW, for example 5 to 200 kW, and in certain embodiments 9 to 120 kW per kilogram of the mixture used. A magnetron is a useful source of dielectric radiation, and one magnetron may be used, or two or more magnetrons may be used simultaneously.

[0159] The OCMF material can be dried to remove residual liquids (water, solvents, blowing agents). Post-treatment can also be utilized to hydrophobize the OCMF material. This post-treatment can use a hydrophobic coating agent having high thermal stability and / or low flammability, such as silicone, silicate, or fluorine compound.

[0160] The density of the melamine OCMF is generally in the range of 0.005 to 0.3 g / cc, for example, in the range of 0.01 to 0.2 g / cc, in certain embodiments, in the range of 0.03 to 0.15 g / cc, and most specifically in the range of 0.05 to 0.15 g / cc. The average pore diameter of the melamine OCMF is generally in the range of 10 μm to about 1000 μm, especially in the range of 50 to 700 μm.

[0161] In one embodiment, the OCMF reinforcement is incorporated into the aerogel composition as a continuous sheet. This process includes first manufacturing a continuous sheet of OCMF-reinforced gel by casting or impregnating a gel precursor solution onto a continuous sheet of OCMF reinforcement material, enabling the material to form in the reinforced gel composition sheet. Then, liquid may be at least partially extracted from the OCMF-reinforced gel composition sheet to produce a sheet-like OCMF-reinforced aerogel composition.

[0162] The aerogel composition can include an opacifying agent to reduce the radiative component of heat transfer. At any point prior to gel formation, the opacifying compound or its precursor may be dispersed in a mixture containing the gel precursor. Examples of opacifying compounds include, but are not limited to, boron carbide (B4C), diatomaceous earth, manganese ferrite, MnO, NiO, SnO, Ag2O, Bi2O3, carbon black, titanium oxide, iron titanate, aluminum oxide, zirconium silicate, zirconium oxide, iron(II) oxide, iron(III) oxide, manganese dioxide, iron titanate (ilmenite), chromium oxide, carbides (such as SiC, TiC, WC), or mixtures thereof. Examples of opacifying compound precursors include, but are not limited to, TiOSO4 or TiOCl2.

[0163] The aerogel composition can include one or more fire-class additives. In the context of the present disclosure, the term "fire-class additive" refers to a material that has an endothermic effect in the context of the reaction to fire and can be incorporated into the aerogel composition. Further, in certain embodiments, the fire-class additive has an endothermic decomposition onset point (E d ) that is less than 100 °C higher than the thermal decomposition onset point (T D ) of the aerogel composition in which the fire-class additive is present, and in more particular embodiments, has an E d that is less than or equal to 50 °C lower than the T D of the aerogel composition in which the fire-class additive is present. In other words, the E D of the fire-class additive has a range of (T d - 50 °C) to (T d + 100 °C):

[0164]

Number

[0165] Prior to, simultaneously with, or subsequent to integration or mixing with a sol (e.g., a silica sol prepared in various ways from an alkyl silicate or water glass, as understood in the prior art), a refractory class additive can be mixed or otherwise dispersed in a medium containing ethanol and optionally up to 10 volume % water. The mixture may be mixed and / or stirred as necessary to achieve substantially uniform dispersion of the additive in the medium. Without being bound by theory, utilization of the hydrated forms of the clays and other refractory class additives described above provides an additional endothermic effect. For example, halloysite clay (commercially available from Applied Minerals, Inc. under the trademark DRAGONITE or otherwise available from Imerys simply as halloysite), kaolinite clay are aluminosilicate clays that have an endothermic effect by releasing water of hydration (gas dilution) at high temperature in their hydrated form. As another example, hydrated forms of carbonates can release carbon dioxide upon heating or at high temperature.

[0166] In the context of the present disclosure, the term "dehydration heat" means the amount of heat (and, where applicable, dihydroxylation) required to vaporize water from a hydrated form of a material when not exposed to elevated temperature. Dehydration heat is typically expressed on a unit mass basis.

[0167] In certain embodiments, the refractory class additives of the present disclosure have an onset of thermal decomposition at about 350 °C or greater, about 400 °C or greater, about 450 °C or greater, about 500 °C or greater, about 550 °C or greater, about 600 °C or greater, about 650 °C or greater, about 700 °C or greater, about 750 °C or greater, about 800 °C or greater, or in the range between any two of these values. In certain embodiments, the refractory class additives of the present disclosure have an onset of thermal decomposition at about 440 °C or about 570 °C. In certain embodiments, the refractory class additives of the present disclosure have a T of an aerogel composition (without the refractory class additive) in which the refractory class additive is incorporated dIt has a thermal decomposition starting point higher or lower than by 50 °C or less, 40 °C or less, 30 °C or less, 20 °C or less, 10 °C or less, 5 °C or less, or within the range between any two of these values.

[0168] Examples of the refractory class additives of the present disclosure include clay materials such as phyllosilicate clays (such as illite, etc.), kaolinite (aluminum silicate; Al2Si2O5(OH)4), halloysite (aluminum silicate; Al2Si2O5(OH)4), endellite (aluminum silicate; Al2Si2O5(OH)4), mica (silica mineral), diaspore, gibbsite (aluminum hydroxide), montmorillonite, beidellite, pyrophyllite (aluminum silicate; Al2Si4O 10(OH)2), nontronite, bravaisite, smectite, leverrierite, rectorite, seridite, attapulgite, chloropal, volkonskoite, allophane, racewinite, dillnite, severite, miloschite, collyrite, cimolite and newtonite, magnesium hydroxide (or magnesium dihydroxide, "MDH"), alumina trihydrate ("ATH"), carbonates such as dolomite and lithium carbonate (but not limited to these), etc. can be mentioned, but not limited to these. Among the clay materials, in certain embodiments of the present disclosure, clay materials having at least a partially layered structure are used. In certain embodiments of the present disclosure, the clay material as a refractory class additive in the aerogel composition has at least some water, for example, in a hydrated form. The additive may be in a hydrated crystalline form or may be in a hydrated state during the manufacture / processing of the composition of the present invention. In certain embodiments, the refractory class additive also includes a low melting point additive that absorbs heat without changing the chemical composition. Examples of this class are low melting point glasses such as, for example, inert glass beads. Other additives that can be useful in the compositions of the present disclosure include wollastonite (calcium silicate) and titanium dioxide (TiO2), but not limited to these. In certain embodiments, other additives include, for example, infrared opacifying agents such as titanium dioxide or silicon carbide (but not limited to these), ceramifiers such as low melting point glass frit (but not limited to these), calcium silicate, or charformers such as, for example, phosphates and sulfates (but not limited to these), but not limited to these. In certain embodiments, the additive may require special processing considerations such as, for example, techniques to ensure that the additive is uniformly distributed and does not aggregate so greatly as to cause variations in product performance.The processing technology can additionally include static and dynamic mixers, stabilizers, adjustment of process conditions, and others known in the art. The amount of additives in the final aerogel composition may depend on various other property requirements and may vary in the range of 5% to about 70% by mass. In certain embodiments, the amount of additives in the final aerogel composition is from 10% to about 60% by mass, and in certain preferred embodiments, it is from about 20% to about 40% by mass. In certain embodiments, there may be more than one type of additive. Also, one or more refractory class additives may be present in the final aerogel composition. In certain preferred embodiments including aluminosilicate refractory class additives, the additive is present at about 60 - 70 wt% in the final aerogel composition.

[0169] In certain embodiments of the present disclosure, a method for manufacturing an OCMF - enhanced aerogel composition having refractory class performance is provided. The refractory class compositions of these embodiments also have sufficient hydrophobicity for use as insulation materials in industrial environments, as required by the water uptake and low thermal conductivity, which helps to meet the always - required energy - saving needs. To obtain such a combination of desirable properties, simply adding additives or simply adding refractory class additives is not successful. One can try various modifications and combinations, or various additives, to reach an optimized solution, but such efforts are not always successful and there are risks for manufacturability with reproducible quality control regarding these desired properties. An important aspect of these embodiments is to evaluate the thermal behavior (evaluated by thermogravimetry or differential scanning calorimetry) of the composition that would provide all desirable properties except for the fire performance, and to consider refractory class additives that closely match the starting point of thermal decomposition of the underlying composition, or the temperature at which the most heat is released or the most heat is absorbed due to the onset of thermal decomposition of the refractory class additive.

[0170] In certain embodiments, the desired fire properties of the final composition may include not only intrinsic properties such as heat of combustion (ISO 1716), but also system fire properties such as the reaction to fire performance in accordance with ISO 1182. In the case of ISO 1182, the mass loss, the increase in furnace temperature, and the flame time when exposed to a furnace at a temperature of about 750 °C are evaluated.

[0171] The OCMF-reinforced aerogel composition may have various components that add fuel to the system. Further, it may have various other components that do not contribute as fuel but can interfere with combustion when exposed to a flame. Thus, the combustion behavior of such a system cannot be predicted simply based on the components. In situations where multiple properties are desired, in certain embodiments, the composition should be reached disregarding its fire properties, and the thermal performance of the composition thus reached should be evaluated to find suitable fire-resistant class additives that provide fire properties without compromising the other properties that the starting composition was intended to provide.

[0172] In certain embodiments, the onset temperature of thermal decomposition is an important property of the composition. In certain other specific embodiments, the temperature at which the heat release peaks can be an important property for the purpose of developing an aerogel OCMF composition with enhanced fire performance. If there are multiple fuel components present in the composition identified by multiple peaks in the DSC curve, such a composition will function well by matching the peak heat release temperature of the OCMF-reinforced aerogel composition with a fire-resistant class additive having an endothermic peak heat release temperature in the range of 140 °C, 120 °C, 100 °C, or 80 °C. In many embodiments, the endothermic peak heat release temperature is within 50 °C.

[0173] The aerogel materials and compositions of the present disclosure have been shown to be highly effective as thermal insulators. However, the application of the methods and materials of the present disclosure is not intended to be limited to uses related to thermal insulators. The methods and materials of the present disclosure can be applied to any system or use that would benefit from the unique combination of properties or procedures provided by the materials and methods of the present disclosure.

Examples

[0174] The following examples provide various non-limiting embodiments and characteristics of the present disclosure. In the following examples, the wt% of the additives is provided based on 100% of the mass of the silica and hydrophobic components of the aerogel composition. Thermal analysis, TGA, and DSC were performed using a Netzsch STA4449 F1 Jupitor simultaneous thermal analyzer, starting at 25°C and ramping at a rate of 20°C per minute up to 1000°C in air at ambient pressure. References to the hydrophobic substance content of the sol refer to the mass of the solid material in the final aerogel composition derived from the hydrophobic alkylsilane in the sol as a percentage of the mass of the final aerogel composition.

[0175] Example 1 A polysilicate ethyl sol was produced by hydrolyzing TEOS (tetraethoxysilane) in ethanol and water using a sulfuric acid catalyst and then stirred at ambient temperature for about 16 hours. A polymethylsilsesquioxane sol was produced by hydrolyzing MTES (methyltriethoxysilane) and DMDES (dimethyl diethoxysilane) (approx. 4:1 molar ratio) in ethanol and water using a phosphoric acid catalyst and then stirred at ambient temperature for about 16 hours or more. The polysilicate ethyl and polymethylsilsesquioxane (MTES + DMDES) sols were combined (approx. 2:1 mass ratio) to form a precursor sol. This precursor sol was such that the target total hydrophobic substance content in the final aerogel composition prepared from the sol was 30 - 40 wt%. The combined precursor sol was stirred at ambient temperature for 2 hours or more.

[0176] Example 2 A sample of melamine OCMF material (BASOTECT UF from BASF) with a thickness of 10 mm and a density of about 6 kg / m 3 was prepared. A substantially homogeneous mixture of 70 g of magnesium dihydroxide (fire retardant additive; MDH) in about 450 mL of ethanol (containing up to 10% by volume of water) was combined with about 540 mL of the silica sol from Example 1 and stirred for more than 5 minutes. Next, about 10 mL of 28 wt% NH4OH solution was added, and then the sol mixture was stirred for at least 1 minute. When the sol mixture was impregnated into the melamine OCMF material and gelled, gelation occurred within 2 minutes. The resulting gel composition was allowed to stand for about 10 minutes to cure. Next, the gel composition was aged at 68 °C for 16 hours in an ethanol aging fluid containing 10 volume% (vol%) H2O and 1.1 wt / vol% NH4OH (1.1 g of NH4OH per 100 mL of fluid) at a fluid-to-gel composition ratio of about 1.5:1. The aging temperature and the composition of the aging fluid may be further changed to vary the overall aging time.

[0177] Coupons (samples) of the gel composition were then subjected to solvent extraction with supercritical CO2 and then dried at 120 °C for 4 hours. The target silica density was 0.07 g / cc, and the resulting material density of the aerogel composition was 0.159 g / cc. The hydrophobic substance content of the aerogel composition was about 4.34 wt%.

[0178] Example 3 A gel composition was produced in the same procedure as in Example 2, except that a mixture of 72 g of MDH in about 529 mL of ethanol (containing up to 10% by volume of water) was combined with about 460 mL of the silica sol of Example 1. The target silica density was 0.06 g / cc, and the resulting material density of the aerogel composition was 0.185 g / cc. The hydrophobic substance content of the aerogel composition was about 3.97 wt%.

[0179] Example 4 A gel composition was prepared using the same procedure as in Example 2, except that a substantially homogeneous mixture of 96 g of MDH in about 376 mL of ethanol (containing up to 10% water by volume) was combined with about 614 mL of the silica sol from Example 1. The target silica density was 0.08 g / cc, and the resulting material density of the aerogel composition was 0.178 g / cc. The hydrophobe content of the aerogel composition was about 3.97 wt%.

[0180] Example 5 A gel composition was prepared using the same procedure as in Example 2, except that a substantially homogeneous mixture of 84 g of MDH in about 539 mL of ethanol (containing up to 10% water by volume) was combined with about 460 mL of the silica sol from Example 1. The target silica density was 0.06 g / cc, and the resulting material density of the aerogel composition was 0.142 g / cc. The hydrophobe content of the aerogel composition was about 3.6 wt%.

[0181] Example 6 A gel composition was prepared using the same procedure as in Example 2, except that about 529 mL of a substantially homogeneous mixture of ethanol (containing up to 10% water by volume; no fire-resistant additives) was combined with about 460 mL of the silica sol of Example 1. The target silica density was 0.06 g / cc, and the resulting material density of the aerogel composition was 0.074 g / cc. The hydrophobe content of the aerogel composition was about 8.3 wt%.

[0182] Example 7 A gel composition was prepared using the same procedure as in Example 2, except that a substantially uniform mixture of 72 g of inert glass beads (a fire-resistant class additive) in approximately 529 mL of ethanol (containing up to 10% water by volume) was combined with approximately 460 mL of the silica sol from Example 1. The target silica density was 0.06 g / cc, and the resulting material density of the aerogel composition was 0.141 g / cc. The hydrophobe content of the aerogel composition was approximately 3.93 wt%.

[0183] Example 8 A substantially homogeneous mixture of 60 g of wollastonite (commercially available as NYAD) in about 529 mL of ethanol solvent was combined with about 460 mL of the silica sol from Example 1, and a gel composition was produced using the same procedure as in Example 2, except for this combination. The target silica density was 0.06 g / cc, and the resulting material density of the aerogel composition was 0.161 g / cc. The hydrophobic substance content of the aerogel composition was about 3.95 wt%.

[0184] Example 9 A substantially homogeneous mixture of 72 g of titanium dioxide (refractory class additive; TiO2) in about 529 mL of ethanol (containing up to 10% by volume of water) was combined with about 460 mL of the silica sol from Example 1, and a gel composition was produced in the same procedure as in Example 2, except for this combination. The target silica density was 0.06 g / cc, and the resulting material density of the aerogel composition was 0.159 g / cc. The hydrophobic substance content of the aerogel composition was about 3.95 wt%.

[0185] Example 10 About 23 kg / m 3 A sample of a 10 mm thick polyurethane OCMF material having a density of was prepared. A substantially homogeneous mixture of 60 g of MDH (refractory class additive) in about 529 mL of ethanol (containing up to 10% by volume of water) was combined with about 460 mL of the silica sol from Example 1 and stirred for more than 5 minutes. Next, about 10 mL of a 28% by volume NH4OH solution was added, and then the sol mixture was stirred for at least 1 minute. Then, the sol mixture was impregnated into the polyurethane OCMF material and gelled. Gelation occurred within 2 minutes. The resulting gel composition was allowed to stand for about 10 minutes to cure. Next, the gel composition was aged at 68 °C for 16 hours in an ethanol aging fluid containing 10% by volume of H2O and 1.1 wt / vol% NH4OH (1.1 g of NH4OH per 100 mL of fluid) at a fluid to gel composition ratio of about 1.5:1.

[0186] Next, the gel composition coupon (sample) was solvent-extracted with supercritical CO2 and dried at 120 °C for 4 hours. The target silica density was 0.06 g / cc, and the obtained material density of the aerogel composition was 0.165 g / cc. The content of hydrophobic substances in the aerogel composition was about 3.95 wt%.

[0187] Example 11 A polysilicate ethyl sol was produced by hydrolyzing TEOS in EtOH and H2O using a sulfuric acid catalyst and then stirred at ambient temperature for 16 hours or more. A polymethylsilsesquioxane sol was produced by hydrolyzing MTES and DMDES (about 8:1 molar ratio) in EtOH and H2O using an acetic acid catalyst and then stirred at ambient temperature for 16 hours or more. The polysilicate ethyl (TEOS) and polymethylsilsesquioxane (MTES + DMDES) sols were combined (mass ratio about 10:1) to form a silica sol. This silica sol had a target sol hydrophobic substance content in the final aerogel composition of about 12 wt%. The combined silica sol was stirred at ambient temperature for 2 hours or more.

[0188] Example 12 A sample of a melamine OCMF material with a thickness of 10 mm and a density of about 6 kg / m 3 was prepared. A substantially homogeneous mixture of 60 g of MDH (refractory class additive) in about 718 mL of ethanol (containing up to 10 volume% water) was combined with about 266 mL of the silica sol from Example 11 and stirred for 5 minutes or more. Next, about 10 mL of a 28 wt% NH4OH solution was added, and then the sol mixture was stirred for at least 1 minute. Next, the sol mixture was impregnated into the melamine OCMF material and gelled. Gelation occurred within 2 minutes. The obtained gel composition was allowed to stand for about 10 minutes to cure. Next, the gel composition was treated in ethanol containing a 0.12 M trimethylsilyl derivative of hexamethyldisilazane ("TMS"), 8 volume% H2O, and 0.8 g of NH4OH3 per 100 mL of ethanol at a fluid-to-gel composition ratio of about 1.5:1 at 68 °C for 16 hours.

[0189] The coupon of the gel composition was then subjected to solvent extraction with supercritical CO2 and dried at 120 °C for 4 hours. The target silica density was 0.05 g / cc, and the obtained material density of the aerogel composition was 0.176 g / cc.

[0190] Example 13 A gel composition was produced using the same procedure as in Example 12, except that a substantially homogeneous mixture of about 718 mL of ethanol solvent (without a refractory class additive) was combined with about 256 mL of the silica sol of Example 8. The target silica density was 0.05 g / cc, and the obtained material density of the aerogel composition was 0.081 g / cc.

[0191] Example 14 A gel composite material was produced using the same procedure as in Example 11, except that tetraethyl orthosilicate (TEOS) and polymethylsilsesquioxane (MTES+DMDES) sols were combined at a mass ratio of about 7:1 to form a silica sol with a target total hydrophobic substance content of 16 wt% in the final aerogel composition.

[0192] Example 15 A gel composition was produced using the same procedure as in Example 12, except that a substantially homogeneous mixture of 72 g of MDH (refractory class additive) in about 668 mL of ethanol solvent was combined with about 317 mL of the silica sol of Example 14. The target silica density was 0.06 g / cc, and the obtained material density of the aerogel composition was 0.195 g / cc. Using the thermogravimetric curve, it was found that the thermal decomposition starting point was 399.5 °C, and using the DSC curve, it was found that the peak heat release temperature was 439.6 °C. Also, the extrapolated thermal decomposition starting temperature of the composition containing the refractory class additive was measured to be 395.8 °C using the thermogravimetric curve and the peak heat release temperature was 560.9 °C using the DSC curve.

[0193] For comparison, when the composition within this example without the fire resistance class additive was measured using a thermogravimetric curve, it was found that the extrapolated onset point of thermal decomposition was 369.4 °C, and when measured using a DSC curve, the peak heat release temperature was found to be 607.9 °C.

[0194] Example 16 A gel composition was produced in the same procedure as Example 12, except that a mixture of about 668 mL of ethanol solvent (without the fire resistance class additive) was combined with about 317 mL of the silica sol of Example 14. The target silica density was 0.06 g / cc, and the resulting material density of the aerogel composition was 0.092 g / cc.

[0195] Example 17 A polysilsicate sol was produced by hydrolyzing TEOS in ethanol and water using a sulfuric acid catalyst and stirred at room temperature for about 16 hours. This hydrophobe-free sol was used without adding polymethylsilsesquioxane sol or other hydrophobic substances.

[0196] Example 18 A gel composite material was produced in the same procedure as Example 12, except that a mixture of about 662 mL of ethanol solvent (without the fire resistance class additive) was combined with about 328 mL of the silica sol of Example 17 and gelled. The gel was treated at 68 °C for 16 hours with a solution containing 0.3 M TMS in ethanol (8% by volume H2O and 0.8 g of NH4OH per 100 mL of ethanol, at a fluid to gel composite material ratio of about 1.5:1). The target silica density was 0.06 g / cc, and the resulting material density of the aerogel composite material was 0.086 g / cc.

[0197] Example 19 A gel composite material was produced in the same procedure as Example 12, except that a mixture of about 662 mL of ethanol solvent (without refractory class additives) was combined with about 328 mL of the silica sol of Example 17 and gelled. The gel was treated at 68 °C for 16 hours with a solution containing 0.6 M MTES (8 vol% H2O and 0.8 g of NH4OH per 100 mL of ethanol, at a fluid-to-gel composite material ratio of about 1.5:1). The target silica density was 0.06 g / cc, and the resulting material density of the aerogel composite material was 0.103 g / cc.

[0198] Example 20 A gel composite material was produced in the same procedure as Example 2, except that a substantially homogeneous mixture of 112 g of halloysite clay (refractory class additive; DRAGONITE) in about 453 mL of ethanol (containing up to 8 vol% water) was combined with about 537 mL of the silica sol of Example 1. The target silica density was 0.07 g / cc, and the resulting material density of the aerogel composite material was 0.196 g / cc. The hydrophobic substance content of the aerogel composition was about 3.37 wt%.

[0199] Example 21 A gel composite material was produced in the same procedure as Example 2, except that a substantially homogeneous mixture of 72 g of halloysite clay (refractory class additive; DRAGONITE) in about 529 mL of ethanol (containing up to 10 vol% water) was combined with about 460 mL of the silica sol from Example 1. The target silica density was 0.06 g / cc, and the resulting material density of the aerogel composite material was 0.128 g / cc. The hydrophobic substance content of the aerogel composition was about 3.91 wt%. The thermal decomposition onset point was measured as 492.9 °C using a thermogravimetric curve, and the peak heat release temperature was measured as 565.9 °C using a DSC curve. Also, the extrapolated thermal decomposition onset point of the composition containing the refractory class additive was measured as 370.9 °C using a thermogravimetric curve, and the peak heat release temperature was measured as 565.9 °C using a DSC curve.

[0200] For comparison, the composition within this example without the fire rating additive had an extrapolated onset point of thermal decomposition of 369.4 °C when measured using a thermogravimetric curve and a peak heat release temperature of 607.9 °C when measured using a DSC curve.

[0201] Example 22 A gel composite material was produced using the same procedure as in Example 2, except that a substantially homogeneous mixture of two fire rating additives, namely 36 g of halloysite clay (DRAGONITE) and 36 g of alumina trihydrate (ATH), in approximately 529 mL of ethanol (containing up to 10 vol% water) was combined with approximately 460 mL of the silica sol from Example 1. The target silica density was 0.06 g / cc, and the resulting material density of the aerogel composite was 0.149 g / cc. The hydrophobic substance content of the aerogel composition was approximately 3.94 wt%.

[0202] Example 23 A gel composite material was produced in the same procedure as in Example 2, except that a substantially homogeneous mixture of 72 g of alumina trihydrate (ATH) in approximately 529 mL of ethanol (containing up to 10 vol% water) was combined with approximately 460 mL of the silica sol from Example 1. The target silica density was 0.06 g / cc, and the resulting material density of the aerogel composite was 0.152 g / cc. The hydrophobic substance content of the aerogel composition was approximately 3.94 wt%. Using a thermogravimetric curve, the onset point of thermal decomposition was measured as 289.8 °C, and using a DSC curve, the peak heat release temperature was measured as 334.1 °C.

[0203] For comparison, the composition within this example without the fire rating additive had an extrapolated onset point of thermal decomposition of 369.4 °C when measured using a thermogravimetric curve and a peak heat release temperature of 607.9 °C when measured using a DSC curve.

[0204] Example 24 A gel composite material was produced using the same procedure as in Example 12, except that about 426 mL of the silica sol from Example 11 was combined with a substantially homogeneous mixture of 100 g of halloysite clay (DRAGONITE) in about 558 mL of ethanol (containing up to 10% by volume of water). These were combined in such a way as to target a hydrophobic substance content of 28 wt%. The target silica density was 0.083 g / cc, and the resulting material density of the aerogel composite material was 0.184 g / cc.

[0205] Example 25 A gel composition was produced in the same procedure as in Example 2, except that a substantially homogeneous mixture of 56 g of halloysite clay (DRAGONITE from Applied Minerals, Inc.) and 56 g of ATH in about 453 mL of ethanol (containing up to 8% by volume of water) was combined with about 537 mL of the silica sol from Example 1. The target silica density was 0.07 g / cc, and the resulting material density of the aerogel composite material was 0.196 g / cc. The hydrophobic substance content of the aerogel composition was about 3.36 wt%.

[0206] Table 1 is shown below to illustrate the compositions of the above examples. The term "wt% addition amount" refers to the amount of additive added to the composition based on the amount of silica present. For example, a "wt% addition amount" of 120% indicates that 120 g of additive was added per 100 g of silica in the composition.

[0207]

Table 1

[0208]

Table 2

[0209] The above-mentioned advantages, and the advantages revealed from the above description, are efficiently achieved. Since changes can be made in the above configuration without departing from the scope of the present invention, it is intended that all matters included in the above description or shown in the attached drawings be construed as illustrative and not in a limiting sense.

[0210] Also, the following claims are intended to cover all of the general and specific features of the present invention described herein, and also all descriptions of the scope of the present invention that may be said to fall therebetween in language. Some embodiments of the invention related to the present invention are shown below. [Aspect 1] A reinforced aerogel composition comprising a silica-based aerogel skeleton reinforced with an OCMF material and a refractory class additive, wherein the silica-based aerogel skeleton contains at least one hydrophobic bonded silicon, and the reinforced aerogel composition has the following properties: i) A liquid water uptake of 20% by mass or less; ii) A thermal conductivity of 30 mW / m·K or less in accordance with ASTM C518 standard at a temperature of about 37.5 °C, ambient environment, atmospheric pressure and a compressive load of about 2 psi; and iii) A heat of combustion of less than 717 cal / g in accordance with EN ISO 1716 standard; The reinforced aerogel composition having the above properties. [Aspect 2] 2 kg / m 3 ~25 kg / m 3 A reinforced aerogel composition comprising a silica-based aerogel skeleton reinforced with an OCMF material having a density of and a refractory class additive, wherein the silica-based aerogel skeleton contains at least one hydrophobic bonded silicon, and the reinforced aerogel composition has the following properties: i) A liquid water uptake of 20% by mass or less; ii) A thermal conductivity of 30 mW / m·K or less in accordance with ASTM C518 standard at a temperature of about 37.5 °C, ambient environment, atmospheric pressure and a compressive load of about 2 psi; and iii) A heat of combustion of less than 717 cal / g in accordance with EN ISO 1716 standard; The reinforced aerogel composition having the above properties. [Aspect 3] 2 kg / m 3 ~25 kg / m 3 A reinforced aerogel composition comprising a silica-based aerogel skeleton reinforced with an OCMF material having a density of and a refractory class additive, wherein the silica-based aerogel skeleton contains at least one hydrophobic bonded silicon, and the reinforced aerogel composition has the following properties: i) A liquid water uptake of 1% to 10% by mass; ii) A thermal conductivity greater than 8 mW / m·K and less than 25 mW / m·K in accordance with ASTM C518 standard at a temperature of about 37.5 °C, ambient environment, atmospheric pressure and a compressive load of about 2 psi; and iii) A heat of combustion of less than 717 cal / g and more than 400 cal / g, in accordance with the EN ISO 1716 standard; An enhanced aerogel composition having the following. [Aspect 4] A silica-based aerogel composition and an enhanced OCMF composition reinforced with a fire-resistant class additive, wherein the silica-based aerogel skeleton contains at least one hydrophobic bonded silicon, and the enhanced aerogel composition has the following properties: i) A liquid water uptake of 20% by mass or less; ii) A thermal conductivity of 30 mW / m·K or less, in accordance with the ASTM C518 standard, at a temperature of about 37.5 °C, ambient environment, atmospheric pressure, and a compressive load of about 2 psi; and iii) A heat of combustion of less than 717 cal / g, in accordance with the EN ISO 1716 standard; An enhanced OCMF composition having the following. [Aspect 5] A silica-based aerogel composition and an enhanced OCMF composition reinforced with a fire-resistant class additive, wherein the silica-based aerogel skeleton contains at least one hydrophobic bonded silicon, and the enhanced aerogel composition has the following properties: i) A liquid water uptake of 20% by mass or less; ii) A thermal conductivity of 30 mW / m·K or less, in accordance with the ASTM C518 standard, at a temperature of about 37.5 °C, ambient environment, atmospheric pressure, and a compression of about 2 psi; and iii) A heat of combustion of less than 717 cal / g, in accordance with the EN ISO 1716 standard; An enhanced OCMF composition having the following. [Aspect 6] A silica-based aerogel composition and an enhanced OCMF composition reinforced with a fire-resistant class additive, wherein the silica-based aerogel skeleton contains at least one hydrophobic bonded silicon, and the enhanced aerogel composition has the following properties: i) A liquid water uptake between 1% and 10% by mass; ii) A thermal conductivity greater than 8 mW / m·K and less than 25 mW / m·K, in accordance with the ASTM C518 standard, at a temperature of about 37.5 °C, ambient environment, atmospheric pressure, and a compression of about 2 psi; and iii) Heat of combustion less than 717 cal / g and more than 400 cal / g, conforming to EN ISO 1716 standard; An enhanced OCMF composition having [Aspect 7] The enhanced aerogel composition according to any one of Aspects 1 to 3 or the enhanced OCMF composition according to any one of Aspects 4 to 6, wherein the OCMF material comprises an organic OCMF material or is an organic OCMF material. [Aspect 8] The enhanced aerogel composition according to any one of Aspects 1 to 3 or the enhanced OCMF composition according to any one of Aspects 4 to 7, wherein the OCMF material comprises a melamine-based OCMF material or is a melamine-based OCMF material. [Aspect 9] The enhanced aerogel composition according to any one of Aspects 1 to 3 or the enhanced OCMF composition according to any one of Aspects 4 to 6, wherein the OCMF material comprises a sheet-like OCMF material or is a sheet-like OCMF material. [Aspect 10] The enhanced aerogel composition according to any one of Aspects 1 to 3 or the enhanced OCMF composition according to any one of Aspects 4 to 9, wherein the OCMF material is an organic foam. [Aspect 11] The enhanced aerogel composition according to any one of Aspects 1 to 3 or the enhanced OCMF composition according to any one of Aspects 4 to 6, wherein the OCMF material is a melamine-based foam. [Aspect 12] The enhanced aerogel composition or enhanced OCMF composition according to any one of Aspects 1 to 11, wherein the OCMF material is neither a low flammability material nor a non-flammable material. [Aspect 13] The enhanced aerogel composition or enhanced OCMF composition according to any one of Aspects 1 to 11, wherein the OCMF material is neither a low flaming combustible material nor a non-flaming combustible material. [Aspect 14] The enhanced aerogel composition or enhanced OCMF composition according to any one of Aspects 1 to 11, wherein the OCMF material constitutes 2% to 10% by mass of the composition. [Aspect 15] The reinforced aerogel composition or reinforced OCMF composition according to any one of Aspects 1 to 14, wherein the content of the hydrophobic silicon bond in the composition is 2% by mass to 10% by mass. [Aspect 16] The reinforced aerogel composition or reinforced OCMF composition according to any one of Aspects 1 to 14, wherein the content of the hydrophobic silicon bond in the composition is 2% by mass to 8% by mass. [Aspect 17] The reinforced aerogel composition or reinforced OCMF composition according to any one of Aspects 1 to 14, wherein the content of the hydrophobic silicon bond in the composition is 2% by mass to 6% by mass. [Aspect 18] The reinforced aerogel composition or reinforced OCMF composition according to any one of Aspects 1 to 17, wherein the composition has a heat of combustion of 700 cal / g or less in accordance with the EN ISO 1716 standard. [Aspect 19] The reinforced aerogel composition or reinforced OCMF composition according to any one of Aspects 1 to 17, wherein the composition has a heat of combustion of 675 cal / g or less in accordance with the EN ISO 1716 standard. [Aspect 20] The reinforced aerogel composition or reinforced OCMF composition according to any one of Aspects 1 to 17, wherein the composition has a heat of combustion of 650 cal / g or less in accordance with the EN ISO 1716 standard. [Aspect 21] The reinforced aerogel composition or reinforced OCMF composition according to any one of Aspects 1 to 17, wherein the composition has a heat of combustion of 625 cal / g or less in accordance with the EN ISO 1716 standard. [Aspect 22] The reinforced aerogel composition or reinforced OCMF composition according to any one of Aspects 1 to 21, wherein the composition has a thermal conductivity of 22 mW / m·K or less in accordance with the ASTM C518 standard at a temperature of about 37.5°C, ambient environment, atmospheric pressure, and a compressive load of about 2 psi. [Aspect 23] The reinforced aerogel composition according to any one of Aspects 1 to 21, having a thermal conductivity of 20 mW / m·K or less in accordance with ASTM C518 standard at a temperature of about 37.5 °C, ambient environment, atmospheric pressure, and a compressive load of about 2 psi. [Aspect 24] The reinforced aerogel composition according to any one of Aspects 1 to 21, having a thermal conductivity of 18 mW / m·K or less in accordance with ASTM C518 standard at a temperature of about 37.5 °C, under ambient environment and atmospheric pressure, and a compressive load of about 2 psi. [Aspect 25] The reinforced aerogel composition according to any one of Aspects 1 to 21, having a density of 0.15 to 0.40 g / cm 3 3. [Aspect 26] The reinforced aerogel composition according to any one of Aspects 1 to 21, wherein the starting point of thermal decomposition of the organic content of the reinforced aerogel composition is 350 °C or higher. [Aspect 27] The reinforced aerogel composition according to any one of Aspects 1 to 21, wherein the starting point of thermal decomposition of the reinforced aerogel composition is 360 °C or higher. [Aspect 28] The reinforced aerogel composition according to any one of Aspects 1 to 21, wherein the starting point of thermal decomposition of the reinforced aerogel composition is 370 °C or higher. [Aspect 29] The reinforced aerogel composition according to any one of Aspects 1 to 21, wherein the starting point of thermal decomposition of the reinforced aerogel composition is 380 °C or higher. [Aspect 30] The reinforced aerogel composition according to any one of Aspects 1 to 21, wherein the starting point of thermal decomposition of the reinforced aerogel composition is 390 °C or higher. [Aspect 31] An organic OCMF-reinforced aerogel composition containing a refractory class additive and a hydrophobic organic content, wherein the starting point of endothermic decomposition of the refractory class additive in the composition is within 50 °C of the starting point of thermal decomposition of the other parts of the composition other than the refractory class additive. [Aspect 32] An organic OCMF-reinforced aerogel composition containing a refractory class additive and at least 5% hydrophobic content, wherein the total heat of endothermic decomposition of the refractory class additive in the composition is at least 30% of the exothermic heat of decomposition of the other parts of the composition other than the refractory class additive. [Aspect 33] An organic OCMF-reinforced aerogel composition containing at least two refractory class additives, and the starting points of endothermic decomposition of each of them are at least 10 °C apart. [Aspect 34] An organic OCMF-reinforced aerogel composition containing a refractory class additive and a hydrophobic content, wherein the total heat of endothermic decomposition of the refractory class additive in the composition is 80% or less of the exothermic heat of decomposition of the other parts of the composition other than the refractory class additive. [Aspect 35] The hydrophobic content is at least 5%, and the total heat of endothermic decomposition of the refractory class additive in the composition is at least 30% of the exothermic heat of decomposition of the other parts of the composition other than the refractory class additive. The reinforced aerogel composition or the reinforced OCMF composition according to any one of Aspects 1 to 11. [Aspect 36] The starting point of endothermic decomposition of the refractory class additive in the composition is within 50 °C of the starting point of thermal decomposition of the other parts of the composition other than the refractory class additive. The reinforced aerogel composition or the reinforced OCMF composition according to any one of Aspects 1 to 11. [Aspect 37] Containing at least two refractory class additives, and the starting points of endothermic decomposition of each of the two refractory class additives are at least 10 °C apart. The reinforced aerogel composition or the reinforced OCMF composition according to any one of Aspects 1 to 11. [Aspect 38] The total heat quantity of the endothermic decomposition of the refractory class additive in the composition is 80% or less of the exothermic decomposition heat quantity of the other parts of the composition other than the refractory class additive. The reinforced aerogel composition or the reinforced OCMF composition according to any one of Aspects 1 to 11. [Aspect 39] The increase in the furnace temperature of the composition conforming to ISO 1182 is about 100°C or less, about 90°C or less, about 80°C or less, about 70°C or less, about 60°C or less, about 50°C or less, about 45°C or less, about 40°C or less, about 38°C or less, about 36°C or less, about 34°C or less, about 32°C or less, about 30°C or less, about 28°C or less, about 26°C or less, about 24°C or less, or within the range between any two of these values. The composition according to any one of Aspects 1 to 38. [Aspect 40] The flame time of the composition conforming to ISO 1182 is about 30 seconds or less, about 25 seconds or less, about 20 seconds or less, about 15 seconds or less, about 10 seconds or less, about 5 seconds or less, about 2 seconds or less, or within the range between any two of these values. The composition according to any one of Aspects 1 to 39. [Aspect 41] The mass loss of the composition conforming to ISO 1182 is about 50% or less, about 40% or less, about 30% or less, about 28% or less, about 26% or less, about 24% or less, about 22% or less, about 20% or less, about 18% or less, about 16% or less, or within the range between any two of these values. The composition according to any one of Aspects 1 to 40. [Aspect 42] The composition has low flaming combustibility. The composition according to any one of Aspects 1 to 41. [Aspect 43] The composition has non-flaming combustibility. The composition according to any one of Aspects 1 to 42. [Aspect 44] The composition has low flammability. The composition according to any one of Aspects 1 to 43. [Aspect 45] The composition is non-combustible. The composition according to any one of Aspects 1 to 44. [Aspect 46] The composition according to any one of Aspects 1 to 45, wherein the starting point of the endothermic decomposition of the refractory class additive is higher than 280 °C, 300 °C, 350 °C, 400 °C, 450 °C or 500 °C. [Aspect 47] The composition according to any one of Aspects 1 to 46, wherein the starting point of the exothermic decomposition of the organic content of the composition not containing the refractory class additive is higher than 280 °C, 300 °C, 350 °C, 400 °C, 450 °C or 500 °C. [Aspect 48] The composition according to any one of Aspects 1 to 47, wherein the OCMF material is a melamine-based foam. [Aspect 49] The composition according to any one of Aspects 1 to 48, wherein the OCMF material is a urethane-based polymer foam. [Aspect 50] The composition according to any one of Aspects 1 to 49, wherein the OCMF material is a reticulated foam.

Claims

1. A reinforced aerogel composition, wherein the reinforced aerogel composition comprises: a reinforced silica-based aerogel material; and one or more endothermic refractory class additives combined with the reinforced silica-based aerogel material, and the reinforced silica-based aerogel material comprises: an open-cell macroporous framework (OCMF) material; and a silica-based aerogel material combined with the open-cell macroporous framework (OCMF) material, and the one or more endothermic refractory class additives are present in the reinforced aerogel composition in an amount of 5% to 70% by mass, the OCMF material constitutes 2% to 10% by mass of the reinforced aerogel composition, the reinforced silica-based aerogel material has a thermal decomposition onset temperature, where the thermal decomposition onset temperature is the measured value of the minimum temperature of the ambient heat at which a rapid exothermic reaction from the decomposition of the organic material in the reinforced silica-based aerogel material appears when measured using thermogravimetric analysis (TGA) or differential scanning calorimetry (DSC) analysis, which is carried out by starting from 25°C and rising to 1000°C at a rate of 20°C per minute in air at normal pressure for 1 minute, the one or more endothermic refractory class additives have an endothermic decomposition onset temperature within 50°C of the thermal decomposition onset temperature of the reinforced silica-based aerogel material, and the endothermic decomposition onset temperature is the measured value of the minimum temperature of the ambient heat at which an endothermic reaction from dehydration or dihydroxylation appears in the one or more endothermic refractory class additives when measured using thermogravimetric analysis (TGA) carried out by starting from 25°C and rising to 1000°C at a rate of 20°C per minute in air at normal pressure for 1 minute, a composition.

2. The reinforced aerogel composition according to claim 1, wherein the OCMF material comprises a melamine-based OCMF material.

3. The reinforced aerogel composition according to claim 1, wherein the OCMF material comprises a sheet-like OCMF material.

4. The reinforced aerogel composition according to claim 1, wherein the OCMF material comprises a foam selected from the group consisting of a thermoplastic resin, an elastomer, and a thermosetting resin.

5. The reinforced aerogel composition according to claim 1, wherein the silica-based aerogel material is an organically modified silica-based aerogel material.

6. The reinforced aerogel composition according to claim 5, wherein the OCMF material comprises a combustible material having a heat of combustion exceeding 2 MJ / kg when determined according to the EN ISO 1716 standard.

7. The reinforced aerogel composition according to claim 1, wherein the reinforced aerogel composition has a thermal decomposition start temperature of 280°C to 390°C.

8. The reinforced aerogel composition according to claim 1, wherein the one or more endothermic refractory class additives include halloysite clay.

9. The reinforced aerogel composition i) has an uptake amount of liquid water of 20 wt% or less; ii) has a thermal conductivity of 30 mW / m·K or less at a temperature of about 37.5°C and a compressive load of about 2 psi under ambient conditions and atmospheric pressure in accordance with ASTM C518. The reinforced aerogel composition according to claim 1.

10. A reinforced aerogel composition, wherein the reinforced aerogel composition comprises a reinforced silica-based aerogel material and at least one or more endothermic refractory class additives combined with the reinforced silica-based aerogel material, wherein the reinforced silica-based aerogel material comprises an open-cell macroporous framework (OCMF) material and a silica-based aerogel material combined with the open-cell macroporous framework (OCMF) material, wherein the one or more endothermic refractory class additives are present in the reinforced aerogel composition in an amount of 5% to 70% by mass, the OCMF material constitutes 2% to 10% by mass of the reinforced aerogel composition, the reinforced silica-based aerogel material has an exothermic decomposition heat, the one or more endothermic refractory class additives have an endothermic decomposition heat measured using thermogravimetric analysis (TGA) performed by increasing from 25°C to 1000°C at a rate of 20°C per minute in atmospheric air at normal pressure, and the endothermic decomposition heat is at least 30% of the exothermic decomposition heat of the reinforced silica-based aerogel material when measured using thermogravimetric analysis (TGA) or differential scanning calorimetry (DSC) analysis performed by increasing from 25°C to 1000°C at a rate of 20°C per minute in atmospheric air at normal pressure. Reinforced aerogel composition.

11. The reinforced aerogel composition according to claim 10, wherein the OCMF material includes a melamine-based OCMF material.

12. The reinforced aerogel composition according to claim 10, wherein the OCMF material includes a sheet-like OCMF material.

13. The reinforced aerogel composition according to claim 10, wherein the OCMF material includes a foam selected from the group consisting of a thermoplastic resin, an elastomer, and a thermosetting resin.

14. ​ The reinforced aerogel composition according to claim 10, wherein the silica-based aerogel material is an organically modified silica-based aerogel material.

15. The reinforced aerogel composition according to claim 14, wherein the OCMF material contains a combustible material having a heat of combustion exceeding 2 MJ / kg when determined according to the EN ISO 1716 standard.

16. The reinforced aerogel composition has a thermal decomposition start temperature of 350°C to 390°C, where the thermal decomposition start temperature is measured using thermogravimetric analysis (TGA) or differential scanning calorimetry (DSC) analysis that is carried out by starting from 25°C and rising to 1000°C at a rate of 20°C per minute in atmospheric air, and is the measured value of the lowest temperature of the environmental heat at which a rapid exothermic reaction from the decomposition of the organic material in the reinforced aerogel composition appears. The reinforced aerogel composition according to claim 10.

17. The reinforced aerogel composition according to claim 10, wherein the one or more endothermic refractory class additives contain halloysite clay.

18. The reinforced aerogel composition according to claim 10, wherein the heat of decomposition of the reinforced silica-based aerogel material is 625 cal / g to 700 cal / g in accordance with the EN ISO 1716 standard.

19. The reinforced aerogel composition according to claim 10, wherein the reinforced aerogel composition contains at least two endothermic refractory class additives, and the endothermic decomposition start points of the at least two endothermic refractory class additives are at least 10°C apart.

20. The at least one or more endothermic refractory class additives are selected from the group consisting of phylosilicate clay, kaolinite, halloysite, endellite, mica, diaspore, gibbsite, montmorillonite, beidellite, pyrophyllite, nontronite, bravaisite, smectite, rectorite, sericite, attapulgite, chlorite, volkonskoite, allophane, racewinite, dilnite, sepiolite, miloschite, corilite, simolite, and neutrite, magnesium hydroxide, magnesium dihydroxide, alumina trihydrate, carbonate, inert glass beads, wollastonite, and titanium dioxide. The reinforced aerogel composition according to claim 10.

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