CN111117205A - Silica aerogel heat insulation sealing material - Google Patents
Silica aerogel heat insulation sealing material Download PDFInfo
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- CN111117205A CN111117205A CN201910794884.5A CN201910794884A CN111117205A CN 111117205 A CN111117205 A CN 111117205A CN 201910794884 A CN201910794884 A CN 201910794884A CN 111117205 A CN111117205 A CN 111117205A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention relates to the technical field of heat insulation sealing materials, in particular to a silicon dioxide aerogel heat insulation sealing material. The silicon dioxide aerogel heat-insulation sealing material comprises the following raw materials in parts by weight: 5-8 parts of silicon dioxide aerogel, 95-105 parts of polyurethane, 1.5-3 parts of ionic liquid, 4-10 parts of chlorosilane, 3-5 parts of hollow microspheres, 1.5-2 parts of lubricant, 1-5 parts of flame retardant, 2-4 parts of dispersant, 1-2 parts of talcum powder, 9-11 parts of polyamide, 45-50 parts of polytetrafluoroethylene, 3-5 parts of guar gum and 10-13 parts of epoxy resin. According to the invention, through the research on the flame retardant, the low conductivity, the heat insulation and the heat preservation of the silicon dioxide aerogel heat insulation sealing material are ensured, and meanwhile, the sealing material has high flame retardance, good hydrophobicity, good dispersibility, good compatibility and good mechanical property.
Description
Technical Field
The invention relates to the technical field of heat insulation sealing materials, in particular to a silicon dioxide aerogel heat insulation sealing material.
Background
The heat insulating material has less structure exchange with environment,The material with the function of retarding heat flow transmission is mainly used for preventing heat loss of thermodynamic equipment and pipelines, and generally has the characteristics of light weight, looseness, porosity and small heat conductivity coefficient. The heat insulation material is widely used on the marine warship, is mainly used for fire-resistant separation, cabin insulation, heat insulation of high-temperature pipelines and the like, can effectively prevent heat from being conducted to the inside of an object, reduces the temperature in a cabin, and accordingly improves the comfort level of the living environment of officers and soldiers. The aerogel has a special three-dimensional network structure and extremely low density and heat conductivity coefficient, so that the aerogel can be applied to different conditions and occasions; the aerogel can be used as a raw material for gas filtration and can also be used as a catalytic carrier for catalysis. In addition, another main use of aerogels is as thermal insulation materials. The low thermal conductivity, high temperature resistance and other excellent thermal properties of the Si02The aerogel can be applied to the field of thermal insulation materials and serves as a raw material of a thermal insulation material. The sealing material is a material which is filled in joints, cracks, door and window frames, glass peripheries, pipe joints or joints with other structures of buildings, can block medium from penetrating through leakage channels and plays a role in water tightness and air tightness. The sealing material includes metal material (aluminum, lead, indium, stainless steel, etc.), non-metal material (rubber, plastic, ceramic, graphite, etc.), composite material (such as rubber-asbestos plate, aerogel felt-polyurethane), and most used is rubber elastomer material.
The conventional heat-insulating material not only causes environmental pollution, but also influences the health, and causes huge personal injury and property loss; the application of the flame-retardant heat-insulating material has certain limitation, the heat conductivity coefficient is high, toxic substances are easily emitted in the using process, and the flame-retardant heat-insulating material is easily ignited and causes a fire when the temperature is high; silica aerogel and polyurethane have somewhat poor water resistance.
Therefore, the present invention is directed to the development of a silica aerogel heat insulating sealing material having superior flame retardancy and water resistance.
Disclosure of Invention
In order to solve the technical problems, the first aspect of the invention provides a silica aerogel heat insulation sealing material, which comprises the following raw materials in parts by weight: 5-8 parts of silicon dioxide aerogel, 95-105 parts of polyurethane, 1.5-3 parts of ionic liquid, 4-10 parts of chlorosilane, 3-5 parts of hollow microspheres, 1.5-2 parts of lubricant, 1-5 parts of flame retardant, 2-4 parts of dispersant, 1-2 parts of talcum powder, 9-11 parts of polyamide, 45-50 parts of polytetrafluoroethylene, 3-5 parts of guar gum and 10-13 parts of epoxy resin.
As a preferred technical solution of the present invention, the ionic liquid is a tetrafluoroborate ionic liquid.
In a preferred embodiment of the present invention, the tetrafluoroborate ionic liquid is at least one selected from the group consisting of 1-butyl-3-methylimidazolium tetrafluoroborate, 1-ethyl-3-methylimidazolium tetrafluoroborate, 1-pentyl-3-methylimidazolium tetrafluoroborate, and 1-hexyl-3-methylimidazolium tetrafluoroborate.
As a preferred embodiment of the present invention, the chlorosilane-containing compound: the weight ratio of the tetrafluoroborate ionic liquid is (3-4): 1.
as a preferable technical scheme of the invention, the chlorosilane-containing compound is trimethylchlorosilane.
As a preferred technical solution of the present invention, the flame retardant is a phosphorus-nitrogen flame retardant or a tricyanurate flame retardant.
As a preferred embodiment of the present invention, the phosphate flame retardant: the weight ratio of the tricyanurate flame retardant is 1 (1.5-2.5).
In a preferred embodiment of the present invention, the phosphate flame retardant is tetrakis (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate.
As a preferred technical scheme of the invention, the tricyanurate flame retardant is tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate.
The second aspect of the invention provides a preparation method of a silica aerogel heat-insulation sealing material, which comprises the following steps:
(1) mixing silicon dioxide aerogel, polyurethane, ionic liquid, chlorosilane and hollow microspheres, and performing ultrasonic assistance to obtain a first mixture;
(2) wet ball milling polyamide, epoxy resin and polytetrafluoroethylene to 90-100 meshes to obtain a second mixture;
(3) adding the second mixture, the lubricant, the dispersant and the flame retardant into a high-speed mixer, mixing for 8-10min, adding the talcum powder, mixing for 20-25min at 60-70 ℃, and naturally cooling to normal temperature to obtain a third mixture;
(4) adding the first mixture, the third mixture and guar gum into a double-screw extruder, wherein the extrusion temperature is 140-165 ℃, and the screw rotation speed is 40-70 Hz; and cooling, shaping, drawing, cutting and blanking to obtain a finished product.
Has the advantages that: the invention provides a silica aerogel heat-insulation sealing material, which can ensure the low conductivity, heat insulation and heat preservation of the silica aerogel heat-insulation sealing material through the research on a flame retardant, and simultaneously can ensure that the sealing material has higher flame retardance, better hydrophobicity, dispersity, compatibility and mechanical property.
Detailed Description
The technical features of the technical solutions provided by the present invention are further clearly and completely described below with reference to the specific embodiments, and the scope of protection is not limited thereto.
The words "preferred", "more preferred", and the like, in the present invention refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range-describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein. For example, a stated range from "1 to 10" should be considered to include any and all subranges between the minimum value of 1 and the maximum value of 10. Exemplary subranges of the range 1 to 10 include, but are not limited to, 1 to 6.1, 3.5 to 7.8, 5.5 to 10, and the like.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
In order to solve the technical problems, the first aspect of the invention provides a silica aerogel heat insulation sealing material, which comprises the following raw materials in parts by weight: 5-8 parts of silicon dioxide aerogel, 95-105 parts of polyurethane, 1.5-3 parts of ionic liquid, 4-10 parts of chlorosilane, 3-5 parts of hollow microspheres, 1.5-2 parts of lubricant, 1-5 parts of flame retardant, 2-4 parts of dispersant, 1-2 parts of talcum powder, 9-11 parts of polyamide, 45-50 parts of polytetrafluoroethylene, 3-5 parts of guar gum and 10-13 parts of epoxy resin.
In one embodiment, the silica aerogel thermal insulation sealing material comprises the following raw materials in parts by weight: 7 parts of silicon dioxide aerogel, 100 parts of polyurethane, 2 parts of ionic liquid, 7 parts of chlorosilane, 4 parts of cenospheres, 1.8 parts of lubricating agent, 3 parts of flame retardant, 3 parts of dispersing agent, 1.5 parts of talcum powder, 10 parts of polyamide, 48 parts of polytetrafluoroethylene, 4 parts of guar gum and 12 parts of epoxy resin.
Silica aerogel
The silica aerogel is a novel light nano porous amorphous solid material, has the advantages of low refractive index, small Young modulus, low acoustic impedance, low thermal conductivity coefficient, strong adsorption performance and the like, and is a novel heat-insulating material with wide application prospect.
The source of the silica aerogel is not particularly limited in the present invention, and the silica aerogel can be prepared or obtained commercially, for example, commercially available silica aerogels include but are not limited to silica aerogels obtained from needleless technologies (Hebei) Inc.
Examples silica aerogel, manufacturer: chengdu Elizagen technologies, Inc., particle size: 5-20 nm.
Polyurethane
The polyurethane is fully called polyurethane, and can be prepared into polyurethane plastics, polyurethane fibers, polyurethane rubber and elastomers. The polyurethane elastomer is also called polyurethane rubber, abbreviated as TPU, and is (AB)nThe block linear polymer A is polyester or polyether with high molecular weight (1000-6000), B is diol containing 2-12 straight chain carbon atoms, and the chemical structure between AB segments is diisocyanate. The thermoplastic polyurethane rubber is crosslinked by intermolecular hydrogen bonds or slightly crosslinked between macromolecular chains, and the two crosslinking structures have reversibility along with the increase or decrease of temperature. The intermolecular force is weakened in a molten state or a solution state, and the intermolecular force is strongly connected together after cooling or solvent volatilization, so that the performance of the original solid is recovered. The polyurethane elastomer has the performance between that of plastic and rubber, and has the advantages of oil resistance, wear resistance, low temperature resistance, aging resistance, high hardness and elasticity.
In one embodiment, the polyurethane is a polyurethane elastomer.
The preparation method of the polyurethane elastomer comprises the following steps:
adding metered oligomer polyalcohol into a 500ml three-neck flask provided with a stirrer and a thermometer, heating to 120 ℃, dehydrating in vacuum at 5mm Hg for 1-1.5h, then cooling to 50-60 ℃, adding toluene diisocyanate, slowly heating to 80-100 ℃, and carrying out heat preservation reaction for 2-4 h; and degassing, pouring out to obtain a prepolymer, and sealing for later use. Taking a certain amount of prepolymer, adding a measured chain extender and a measured catalyst, quickly and uniformly stirring, pouring into a mold coated with a release agent at the temperature of 100-. The demolded test piece is cured at 100-120 ℃ for 24h and placed at room temperature for 1 week to perform the related performance test.
Ionic liquids
The ionic liquid refers to a liquid composed entirely of ions, such as KCI at high temperature, KOH is in a liquid state, and then the ionic liquid is the ionic liquid. Generally, the anion exchange resin is composed of organic cations such as imidazole, pyridine, quaternary ammonium, quaternary phosphorus and the like, inorganic anions such as tetrafluoroborate, hexafluorophosphate, trifluoromethylsulfonate and the like, and organic anions.
In one embodiment, the ionic liquid is a tetrafluoroborate ionic liquid.
In one embodiment, the ionic liquid is at least one of 1-butyl-3-methylimidazolium tetrafluoroborate, 1-ethyl-3-methylimidazolium tetrafluoroborate, 1-pentyl-3-methylimidazolium tetrafluoroborate, and 1-hexyl-3-methylimidazolium tetrafluoroborate.
In a preferred embodiment, the ionic liquid is 1-butyl-3-methylimidazolium tetrafluoroborate.
The 1-butyl-3-methylimidazole tetrafluoroborate is prepared by the following steps:
in a 100mL three-neck flask equipped with a reflux condenser, 0.09 to 0.11mol of 1-methylimidazole, 0.09 to 0.11mol of n-butyl bromide and 0.09 to 0.11mol of KBF were charged4Stirring and reacting for 3-4h at 80-100 ℃; after the reaction is finished, cooling to room temperature, adding 45-55mL of dichloromethane into the product, diluting and filtering, adding 1-1.2g of neutral alumina standard reagent into the filtrate, stirring at room temperature for 8-10mim, filtering, removing dichloromethane by a rotary evaporator, and drying in vacuum at 120-140 ℃ for 4-6h to obtain almost colorless oily ionic liquid.
Chlorosilane-containing compounds
The chlorosilane, namely the compound containing chlorine-containing silicon and hydrogen, has the excellent characteristics of low surface energy, high and low temperature resistance, electrical insulation, oxidation stability, weather resistance, flame retardancy, hydrophobicity, corrosion resistance, no toxicity, no odor, physiological inertia and the like.
The trimethylchlorosilane (trimethylchlorosilane) is colorless and transparent liquid, has pungent odor, is exposed in air, and is easy to react with moisture to generate hydrogen chloride.
In one embodiment, the chlorosilane is chlorotrimethylsilane.
Examples trimethylchlorosilane is supplied by mcoline, cat #: C821680-1L.
In one embodiment, the chlorosilane-containing: the weight ratio of the tetrafluoroborate ionic liquid is (3-4): 1.
hollow micro-bead
The hollow microsphere is a loose powder material with good fluidity and grey white appearance, has the characteristics of good sound insulation, good flame retardance, good electrical insulation, small density, low oil absorption rate, high strength, good dispersibility, good fluidity and the like, and is widely applied due to stable performance, good weather resistance and low price.
Hollow microbeads in the examples, manufacturer: chongqing Kai Yin chemical Co., Ltd, model: VS 5500.
The inventor finds that the dispersibility, compatibility, hydrophobicity and flame retardance of the silica aerogel sealing material can be improved by adding trimethylchlorosilane and tetrafluoroborate ionic liquid. The possible reasons for this are as follows: the polyurethane material is extremely easy to burn, melts and drips in the burning process, and has potential safety hazard; the tetrafluoroborate ionic liquid is adopted to modify the surface of the hollow microspheres, the fluorine element and the boron element in the tetrafluoroborate ionic liquid are coated on the surfaces of the hollow microspheres, so that the flame retardant property of the thermoplastic polyurethane can be obviously improved, the tetrafluoroborate ionic liquid synergizes with the hollow microspheres at the initial stage of combustion, a compact carbon layer is promoted to be formed on the surface of the polyurethane, the effects of heat insulation and oxygen isolation are achieved, flame propagation is prevented, and the tetrafluoroborate ionic liquid contains fluorine and boron and has a flame retardant effect; the tetrafluoroborate ionic liquid can also improve the dispersibility of a system, inhibit the formation of a filler network, enhance the interaction between the filler and resin and improve the tensile strength of the material; but the tetrafluoroborate ionic liquid has low water resistance, the tetrafluoroborate ionic liquid in the system can be subjected to surface modification by adding trimethylchlorosilane, the hydrophobicity of the tetrafluoroborate ionic liquid is improved, meanwhile, the trimethylchlorosilane has a modification effect on the silica aerogel, the surface of the modified silica aerogel is more regular, the collapse of gel can be prevented, the integrity of a gel network structure is kept, the silica aerogel is converted from a hydrophilic type to a hydrophobic type, the network structure is firmer, the particle distribution is more uniform, the dispersibility is improved, the trimethylchlorosilane also has a hydrophobic modification effect on the surface of the hollow microsphere, the trimethylchlorosilane can also make up the defect of slightly poor hydrolysis resistance of polyurethane, and the compatibility is improved; the trimethylchlorosilane also contains chlorine element, so that a certain flame retardant effect is achieved; when the weight ratio of the trimethylchlorosilane to the tetrafluoroborate ionic liquid is (3-4): 1, the sealing material has excellent flame retardance and hydrophobicity, incomplete coating of fluorine and boron on the surfaces of the hollow microspheres can be caused by reduction of the proportion of the tetrafluoroborate ionic liquid, the flame retardance is reduced, the hydrophobicity of the material can be reduced by increase of the proportion of the tetrafluoroborate ionic liquid, and the weight ratio of the trimethylchlorosilane to the tetrafluoroborate ionic liquid is (3-4): the trimethyl chlorosilane has the best coating on the hydrophilic group of the tetrafluoroborate ionic liquid in 1 hour, and the hydrophobicity is improved.
Lubricant agent
The lubricant is a lubricating medium for reducing the friction resistance of the friction pair and slowing down the abrasion of the friction pair.
In one embodiment, the lubricant is at least one of magnesium stearate, cadmium stearate, copper stearate, barium stearate, zinc stearate, calcium stearate, stearamide, monoglycerides of stearate, glycerol tristearate, ethylene bis stearamide, ethylene bis lauramide, ethylene bis oleamide, paraffin, low molecular weight ionomers, ethylene acrylic acid copolymers, and ethylene vinyl acetate copolymers.
In the examples the lubricant is magnesium stearate, manufacturer: shandong Youso chemical technology, Inc., Cat #: o45012316.
Flame retardant
The flame retardant is a functional auxiliary agent for endowing a flammable polymer with flame retardancy, and is mainly designed aiming at the flame retardancy of a high polymer material; the flame retardants are of various types, and are classified into additive type flame retardants and reactive type flame retardants according to the method of use. The additive flame retardant is added into the polymer by a mechanical mixing method to enable the polymer to have flame retardance, and at present, the additive flame retardant mainly comprises an organic flame retardant, an inorganic flame retardant, a halogen flame retardant (organic chloride and organic bromide) and a halogen-free flame retardant. Organic flame retardants are represented by bromine, phosphorus-nitrogen, red phosphorus and compounds, and inorganic flame retardants are mainly flame retardant systems such as antimony trioxide, magnesium hydroxide, aluminum hydroxide, silicon and the like.
In one embodiment, the flame retardant is a phosphate ester flame retardant, a tricyanurate flame retardant.
In one embodiment, the phosphate ester flame retardant: the weight ratio of the tricyanurate flame retardant is 1 (1.5-2.5).
In one embodiment, the phosphate flame retardant is tetrakis (1,2,2,6, 6-pentamethyl-4-piperidinyl) pyrophosphate.
In one embodiment, the tricyanurate flame retardant is tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate.
The tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate is obtained by carrying out ester exchange reaction on tetraethyl pyrophosphate and 1,2,2,6, 6-pentamethylpiperidinol under the action of a catalyst, and has a molecular formula as follows:
the tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate is prepared by the following method:
under the protection of nitrogen, 5g of tetraethyl pyrophosphate and 0.05g to 0.113g of tetraisopropyl titanate are put into a 250mL four-neck flask and dissolved by 25mL of xylene; then dissolving 11.81-17.72 g of 1,2,2,6, 6-pentamethylpiperidinol by using 95-140 ml of dimethylbenzene, slowly dropwise adding the solution into a reaction system, heating to 160-180 ℃ under the protection of nitrogen for reaction, continuously distilling off the generated ethanol in the reaction process, ending the reaction after 6-7h (GC monitoring reaction), washing with water, collecting an organic phase, removing water, and filtering to obtain a light yellow liquid which is tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate.
The tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate is prepared by taking trihydroxyethyl isocyanurate (mosaic), dimethyldichlorosilane (DMDCS) and 1-oxo-1-phospha-4-hydroxymethyl-2, 6, 7-trioxabicyclo [2.2.2] octane (PEPA) as raw materials, and has the following molecular formula:
the preparation method of the tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxyl) siloxy ] ethyl } isocyanurate comprises the following steps:
replacing air in a four-mouth bottle with nitrogen, adding 8.7-8.8g (0.0333mol) of saxophone, 150mL of dioxane and 12-13g (0.10mol) of DMDCS, heating to 70-80 ℃, and carrying out heat preservation reaction for 6-8 h; after the HCl gas is discharged, cooling to below 30 ℃; adding 19.5-20g (0.11mol) PEPA into the four-mouth bottle, heating to 90-100 ℃, and reacting for 8-9h under the condition of heat preservation; after HCl gas is discharged, 0.8-1.0g of melamine is added, the pH value of the system is adjusted to 5-6, the filtration is carried out, the filtrate is decompressed and distilled to remove dioxane and a small amount of low boiling point substances, 120-mL of chloroform is added, the mixture is stirred, dispersed and filtered, a filter cake is washed by proper amount of distilled water, and the filtration and the vacuum drying are carried out to obtain the tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate.
The inventors have found that the flame retardancy, hydrophobicity and durability of silica aerogel sealing materials can be improved by adding flame retardants tetrakis (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate and tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate. The possible reasons are as follows: secondary amino on a piperidine ring in the tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate can capture alkyl free radicals and alkoxy free radicals in a high polymer, so that the alkyl free radicals and the alkoxy free radicals lose activity to generate corresponding ester and peroxyester, the nitroxide free radicals can be regenerated while corresponding compounds are generated, the free radicals can be captured again, and the durability of the system is improved; nitrogen in the tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate dilutes combustible gas generated in the combustion process of the polymer during combustion, phosphorus in the tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate forms phosphoric acid when being heated, and the phosphoric acid promotes the formation of a compact carbon layer in the combustion process of the polymer, isolates an external heat source and oxygen and improves the flame retardant effect; the inventors have unexpectedly found that the addition of tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate further improves the flame retardant properties, and that when the weight ratio of tetrakis (1,2,2,6, 6-pentamethyl-4-piperidinyl) pyrophosphate to tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate is 1 (1.5-2.5), the silica aerogel heat insulating sealing material has excellent flame retardancy, hydrophobicity and mechanical properties because tris {2- [ dimethyl (1-oxo-1-phospha-2-, phosphorus in 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxyl) siloxy ] ethyl } ester can catalyze and promote the formation of carbon, and silicon in tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxyl) siloxy ] ethyl } isocyanurate can increase the thermal stability of the carbon layers, Si-O bonds form Si-C bonds in the combustion process, and the generated white combustion residues and carbide form a composite inorganic layer, so that volatile matters generated by combustion can be prevented from escaping, oxygen is isolated to achieve the purpose of flame retardance, and the synergistic flame retardant effect is achieved; the flame retardant of the tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate has PO groups which can be combined with H, OH active groups in a flame region to play a role in inhibiting flame, the secondary amine in the tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate has larger steric hindrance, the excessive using amount of the tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate can influence the reaction activity of the PO groups, the isocyanuric acid tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxyl) siloxy ] ethyl } ester contains primary amine, the reaction activity of the primary amine is larger than that of the secondary amine, the isocyanuric acid tris {2- [ dimethyl (1-oxo-1-phospha-2, too much 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } ester can affect the reaction of secondary amine with alkyl free radical and alkoxy free radical; the flame retardant containing the phosphate ester structure has good hydrophobic property, enhances the compatibility of the flame retardant and a polymer matrix, is not easy to generate the migration and precipitation phenomenon of the flame retardant, and ensures that the polymer has lasting flame retardant property; the two flame retardants both contain amino groups and can be used as a curing agent of epoxy resin to form a cross-linked network structure, and the weight ratio of the two substances is (3-4): 1, the cross-linked network structure is more stable, and the epoxy resin molecules are connected by the molecular bond with larger flexibility, thereby achieving the purpose of increasing the toughness.
Dispersing agent
The dispersing agent is a surfactant which has two opposite properties of lipophilicity and hydrophilcity in a molecule. The amphiphilic agent is capable of uniformly dispersing solid and liquid particles of inorganic and organic pigments which are difficult to dissolve in liquids, and also preventing settling and agglomeration of the particles to form stable suspensions.
In one embodiment, the dispersant is at least one of sodium tripolyphosphate, sodium hexametaphosphate, sodium pyrophosphate, triethylhexyl phosphoric acid, sodium dodecyl sulfate, methyl amyl alcohol, cellulose derivatives, polyethylene glycol.
In the examples, the dispersant is sodium lauryl sulfate, manufacturer: wuxi, Yatai, United chemical Co., Ltd, Cat No: K12.
talcum powder
The talcum powder is magnesium silicate mineral talcum talc, the main component of which is hydrous magnesium silicate, and the talcum powder is prepared by crushing, treating with hydrochloric acid, washing with water and drying, has excellent physical and chemical properties of lubricity, anti-sticking property, flow aid, fire resistance, acid resistance, insulativity, high melting point, chemical inactiveness, good covering power, softness, good luster, strong adsorption force and the like, and has the tendency of easily cracking into scales and special lubricity because the crystal structure of the talcum powder is layered.
In the examples, talc powder, manufacturer: shandong Youso chemical technology, Inc., Cat #: i93106215, fineness: 325 mesh.
Polyamide
The Polyamide is commonly known as Nylon (Nylon), and is called Polyamide in English, which is a general name of high polymers containing amide groups in a main chain repeating unit of a macromolecule. The polyamide has good comprehensive properties including mechanical property, heat resistance, abrasion resistance, chemical resistance and self-lubricity, has low friction coefficient and certain flame retardance, is easy to process, is suitable for being filled with glass fiber and other fillers for reinforcing modification, improves the performance and expands the application range.
The polyamide in the examples is nylon 66, manufacturer: good tin free international import and export limited company, model: 70G 33L.
Polytetrafluoroethylene
The polytetrafluoroethylene, commonly referred to as a "non-stick coating" or "easy-to-clean material", has very low surface energy and high temperature resistance.
Example polytetrafluoroethylene, manufacturer: shanghai yo-sey plastics limited, trade mark: f4 is transparent.
Guar gum
The guar gum is a water-soluble high molecular polymer and has a chemical name of guar gum hydroxypropyl trimethyl ammonium chloride. The natural guar gum is used as a raw material, the endosperm part left after the epidermis and the embryo are removed mainly contains galactose and mannose, the natural guar gum is dried, crushed, pressurized, hydrolyzed, precipitated by 20 percent ethanol solution, centrifugally separated, dried and reacted with water-loss condensed glyceryl ether trimethyl ammonium chloride to prepare the guar gum.
Guar in the examples, manufacturer: suzhou yuan tai run chemical limited, cat no: C14S.
Epoxy resin
The epoxy resin is a generic name of a polymer containing more than two epoxy groups in a molecule, and is a polycondensation product of epichlorohydrin and bisphenol A or polyol. The epoxy resin has excellent dielectric property, mechanical property, adhesive property and corrosion resistance, small curing shrinkage and linear expansion coefficient, good dimensional stability and good manufacturability.
The epoxy resin of the present invention is not particularly limited, and there may be mentioned: bisphenol a epoxy resins, novolac polyepoxy resins, glycidyl ether epoxy resins, and the like.
In the examples, the epoxy resin is bisphenol a epoxy resin, and the manufacturer: wuxi Long anhydration chemical Co., Ltd, brand: e-128.
In one embodiment, the preparation method of the silica aerogel heat insulation sealing material comprises the following steps:
(1) mixing silicon dioxide aerogel, polyurethane, ionic liquid, chlorosilane and hollow microspheres, and performing ultrasonic assistance to obtain a first mixture;
(2) wet ball milling polyamide, epoxy resin and polytetrafluoroethylene to 90-100 meshes to obtain a second mixture;
(3) adding the second mixture, the lubricant, the dispersant and the flame retardant into a high-speed mixer, mixing for 8-10min, adding the talcum powder, mixing for 20-25min at 60-70 ℃, and naturally cooling to normal temperature to obtain a third mixture;
(4) adding the first mixture, the third mixture and guar gum into a double-screw extruder, wherein the extrusion temperature is 140-165 ℃, and the screw rotation speed is 40-70 Hz; and cooling, shaping, drawing, cutting and blanking to obtain a finished product.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention. In addition, the starting materials used are all commercially available, unless otherwise specified.
Examples
Example 1
The silicon dioxide aerogel heat-insulation sealing material comprises the following raw materials in parts by weight: 5 parts of silicon dioxide aerogel, 95 parts of polyurethane, 1.5 parts of ionic liquid, 4 parts of chlorosilane, 3 parts of cenospheres, 1.5 parts of lubricant, 1 part of flame retardant, 2 parts of dispersant, 1 part of talcum powder, 9 parts of polyamide, 45 parts of polytetrafluoroethylene, 3 parts of guar gum and 10 parts of epoxy resin.
The polyurethane is a polyurethane elastomer;
the preparation method of the polyurethane elastomer comprises the following steps:
adding metered oligomer polyol into a 500ml three-neck flask provided with a stirrer and a thermometer, heating to 120 ℃, dehydrating under vacuum of 5mm Hg for 1.2h, then cooling to 60 ℃, adding toluene diisocyanate, slowly heating to 80 ℃, and reacting for 2h under heat preservation; and degassing, pouring out to obtain a prepolymer, and sealing for later use. And adding a certain amount of prepolymer into a measured chain extender and a measured catalyst, quickly and uniformly stirring, pouring into a mold coated with a release agent at the temperature of 120 ℃, and pressurizing for 1 hour in a flat vulcanizing machine at the temperature of 100 ℃ for further chain extension. And curing the demoulded test piece at 100 ℃ for 24h, and standing at room temperature for 1 week to perform related performance tests.
The ionic liquid is 1-butyl-3-methylimidazole tetrafluoroborate;
the 1-butyl-3-methylimidazole tetrafluoroborate is prepared by the following steps:
in a 100mL three-necked flask equipped with a reflux condenser, 0.lmol 1-methylimidazole, 0.lmol n-butyl bromide and 0.lmol KBF were charged4Stirring and reacting for 3 hours at the temperature of 80 ℃; after the reaction is finished, the reaction product is cooled to room temperature, 50mL of dichloromethane is added to the product for dilution and filtration, 1g of neutral alumina standard reagent is added to the filtrate, the mixture is stirred at room temperature for 10 mm for filtration, dichloromethane is removed by a rotary evaporator, and the mixture is dried in vacuum at 120 ℃ for 4 hours to obtain almost colorless oily ionic liquid.
The chlorosilane is trimethyl chlorosilane;
the chlorine-containing silane: the weight ratio of the tetrafluoroborate ionic liquid is 3.5: 1;
the lubricant is magnesium stearate;
the flame retardant is phosphate flame retardant or tricyanurate flame retardant;
the phosphate ester flame retardant comprises: the weight ratio of the tricyanurate flame retardant is 1: 2;
the phosphate flame retardant is tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate;
the tricyanurate flame retardant is tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate;
the tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate is prepared by the following method:
in a 250mL four-neck flask, 5g of tetraethyl pyrophosphate and 0.113g of tetraisopropyl titanate were placed under nitrogen protection and dissolved in 25mL of xylene; then, using 140ml of dimethylbenzene to dissolve 17.72g of 1,2,2,6, 6-pentamethylpiperidinol, slowly dropwise adding the solution into a reaction system, heating the solution to 180 ℃ under the protection of nitrogen for reaction, continuously evaporating generated ethanol in the reaction process, finishing the reaction after 6h (GC monitoring reaction), washing the reaction solution with water, collecting an organic phase, removing water, and filtering to obtain a light yellow liquid which is tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate.
The preparation method of the tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxyl) siloxy ] ethyl } isocyanurate comprises the following steps:
replacing air in a four-mouth bottle with nitrogen, adding 8.74g (0.0333mol) of mosaic, 150mL of dioxane and 12.91g (0.10mol) of DMDCS, heating to 70 ℃, and carrying out heat preservation reaction for 7 hours; after the HCl gas is discharged, cooling to below 30 ℃; adding 19.80g (0.11mol) PEPA into the four-mouth bottle, heating to 90 ℃, and reacting for 8 hours under the condition of heat preservation; after HCl gas is discharged, 0.80g of melamine is added, the pH value of the system is adjusted to 5-6, suction filtration is carried out, the filtrate is decompressed and distilled to remove dioxane and a small amount of low boiling point substances, 120mL of chloroform is added, stirring and dispersing are carried out, suction filtration is carried out, a filter cake is washed by proper amount of distilled water, suction filtration and vacuum drying are carried out, and the tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxyl) siloxy ] ethyl } isocyanurate is obtained.
The dispersing agent is sodium dodecyl sulfate;
the polyamide is nylon 66;
the epoxy resin is bisphenol A epoxy resin;
the preparation method of the silica aerogel heat-insulation sealing material comprises the following steps:
(1) mixing silicon dioxide aerogel, polyurethane, ionic liquid, chlorosilane and hollow microspheres, and performing ultrasonic assistance to obtain a first mixture;
(2) wet ball milling polyamide, epoxy resin and polytetrafluoroethylene to 90 meshes to obtain a second mixture;
(3) adding the second mixture, the lubricant, the dispersant and the flame retardant into a high-speed mixer, mixing for 10min, adding the talcum powder, mixing for 25min at 70 ℃, and naturally cooling to normal temperature to obtain a third mixture;
(4) adding the first mixture, the third mixture and guar gum into a double-screw extruder, wherein the extrusion temperature is 160 ℃, and the screw rotation speed is 55 Hz; and cooling, shaping, drawing, cutting and blanking to obtain a finished product.
Example 2
The silicon dioxide aerogel heat-insulation sealing material comprises the following raw materials in parts by weight: 8 parts of silicon dioxide aerogel, 105 parts of polyurethane, 3 parts of ionic liquid, 10 parts of chlorosilane, 5 parts of cenospheres, 2 parts of lubricant, 5 parts of flame retardant, 4 parts of dispersant, 2 parts of talcum powder, 11 parts of polyamide, 50 parts of polytetrafluoroethylene, 5 parts of guar gum and 13 parts of epoxy resin.
The other operations were the same as in example 1.
Example 3
The silicon dioxide aerogel heat-insulation sealing material comprises the following raw materials in parts by weight: 7 parts of silicon dioxide aerogel, 100 parts of polyurethane, 2 parts of ionic liquid, 7 parts of chlorosilane, 4 parts of cenospheres, 1.8 parts of lubricating agent, 3 parts of flame retardant, 3 parts of dispersing agent, 1.5 parts of talcum powder, 10 parts of polyamide, 48 parts of polytetrafluoroethylene, 4 parts of guar gum and 12 parts of epoxy resin.
The other operations were the same as in example 1.
Comparative example 1
The silicon dioxide aerogel heat-insulation sealing material comprises the following raw materials in parts by weight: 7 parts of silicon dioxide aerogel, 100 parts of polyurethane, 4 parts of hollow microspheres, 1.8 parts of lubricating agent, 3 parts of flame retardant, 3 parts of dispersing agent, 1.5 parts of talcum powder, 10 parts of polyamide, 48 parts of polytetrafluoroethylene, 4 parts of guar gum and 12 parts of epoxy resin.
The polyurethane is a polyurethane elastomer;
the preparation method of the polyurethane elastomer is the same as that of the polyurethane elastomer in example 1;
the lubricant is magnesium stearate;
the flame retardant is phosphate flame retardant or tricyanurate flame retardant;
the phosphate ester flame retardant comprises: the weight ratio of the tricyanurate flame retardant is 1: 2;
the phosphate flame retardant is tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate;
the tricyanurate flame retardant is tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate;
the tetrakis (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate was prepared by the same method as in example 1;
the tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate was prepared in the same manner as in example 1;
the dispersing agent is sodium dodecyl sulfate;
the polyamide is nylon 66;
the epoxy resin is bisphenol A epoxy resin;
the preparation method of the silica aerogel heat-insulation sealing material comprises the following steps:
(1) mixing silicon dioxide aerogel, polyurethane and hollow microspheres and carrying out ultrasonic assistance to obtain a first mixture;
(2) wet ball milling polyamide, epoxy resin and polytetrafluoroethylene to 90 meshes to obtain a second mixture;
(3) adding the second mixture, the lubricant, the dispersant and the flame retardant into a high-speed mixer, mixing for 10min, adding the talcum powder, mixing for 25min at 70 ℃, and naturally cooling to normal temperature to obtain a third mixture;
(4) adding the first mixture, the third mixture and guar gum into a double-screw extruder, wherein the extrusion temperature is 160 ℃, and the screw rotation speed is 55 Hz; and cooling, shaping, drawing, cutting and blanking to obtain a finished product.
Comparative example 2
The silicon dioxide aerogel heat-insulation sealing material comprises the following raw materials in parts by weight: 7 parts of silicon dioxide aerogel, 100 parts of polyurethane, 7 parts of chlorosilane, 4 parts of hollow microspheres, 1.8 parts of lubricating agent, 3 parts of flame retardant, 3 parts of dispersing agent, 1.5 parts of talcum powder, 10 parts of polyamide, 48 parts of polytetrafluoroethylene, 4 parts of guar gum and 12 parts of epoxy resin.
The polyurethane is a polyurethane elastomer;
the preparation method of the polyurethane elastomer is the same as that of the polyurethane elastomer in example 1;
the chlorosilane is trimethyl chlorosilane;
the lubricant is magnesium stearate;
the flame retardant is phosphate flame retardant or tricyanurate flame retardant;
the phosphate ester flame retardant comprises: the weight ratio of the tricyanurate flame retardant is 1: 2;
the phosphate flame retardant is tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate;
the tricyanurate flame retardant is tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate;
the tetrakis (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate was prepared by the same method as in example 1;
the tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate was prepared in the same manner as in example 1;
the dispersing agent is sodium dodecyl sulfate;
the polyamide is nylon 66;
the epoxy resin is bisphenol A epoxy resin;
the preparation method of the silica aerogel heat-insulation sealing material comprises the following steps:
(1) mixing silicon dioxide aerogel, polyurethane, chlorosilane and hollow microspheres and performing ultrasonic assistance to obtain a first mixture;
(2) wet ball milling polyamide, epoxy resin and polytetrafluoroethylene to 90 meshes to obtain a second mixture;
(3) adding the second mixture, the lubricant, the dispersant and the flame retardant into a high-speed mixer, mixing for 10min, adding the talcum powder, mixing for 25min at 70 ℃, and naturally cooling to normal temperature to obtain a third mixture;
(4) adding the first mixture, the third mixture and guar gum into a double-screw extruder, wherein the extrusion temperature is 160 ℃, and the screw rotation speed is 55 Hz; and cooling, shaping, drawing, cutting and blanking to obtain a finished product.
Comparative example 3
The silicon dioxide aerogel heat-insulation sealing material comprises the following raw materials in parts by weight: 7 parts of silicon dioxide aerogel, 100 parts of polyurethane, 2 parts of ionic liquid, 4 parts of hollow microspheres, 1.8 parts of lubricating agent, 3 parts of flame retardant, 3 parts of dispersing agent, 1.5 parts of talcum powder, 10 parts of polyamide, 48 parts of polytetrafluoroethylene, 4 parts of guar gum and 12 parts of epoxy resin.
The polyurethane is a polyurethane elastomer;
the preparation method of the polyurethane elastomer is the same as that of the polyurethane elastomer in example 1;
the ionic liquid is 1-butyl-3-methylimidazole tetrafluoroborate;
the 1-butyl-3-methylimidazolium tetrafluoroborate was prepared as described in example 1;
the lubricant is magnesium stearate;
the flame retardant is phosphate flame retardant or tricyanurate flame retardant;
the phosphate ester flame retardant comprises: the weight ratio of the tricyanurate flame retardant is 1: 2;
the phosphate flame retardant is tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate;
the tricyanurate flame retardant is tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate;
the tetrakis (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate was prepared by the same method as in example 1;
the tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate was prepared in the same manner as in example 1;
the dispersing agent is sodium dodecyl sulfate;
the polyamide is nylon 66;
the epoxy resin is bisphenol A epoxy resin;
the preparation method of the silica aerogel heat-insulation sealing material comprises the following steps:
(1) mixing silicon dioxide aerogel, polyurethane, ionic liquid and hollow microspheres and performing ultrasonic assistance to obtain a first mixture;
(2) wet ball milling polyamide, epoxy resin and polytetrafluoroethylene to 90 meshes to obtain a second mixture;
(3) adding the second mixture, the lubricant, the dispersant and the flame retardant into a high-speed mixer, mixing for 10min, adding the talcum powder, mixing for 25min at 70 ℃, and naturally cooling to normal temperature to obtain a third mixture;
(4) adding the first mixture, the third mixture and guar gum into a double-screw extruder, wherein the extrusion temperature is 160 ℃, and the screw rotation speed is 55 Hz; and cooling, shaping, drawing, cutting and blanking to obtain a finished product.
Comparative example 4
The silicon dioxide aerogel heat-insulation sealing material comprises the following raw materials in parts by weight: 7 parts of silicon dioxide aerogel, 100 parts of polyurethane, 2 parts of ionic liquid, 2 parts of chlorosilane, 4 parts of cenospheres, 1.8 parts of lubricating agent, 3 parts of flame retardant, 3 parts of dispersing agent, 1.5 parts of talcum powder, 10 parts of polyamide, 48 parts of polytetrafluoroethylene, 4 parts of guar gum and 12 parts of epoxy resin.
The polyurethane is a polyurethane elastomer;
the preparation method of the polyurethane elastomer is the same as that of the polyurethane elastomer in example 1;
the ionic liquid is 1-butyl-3-methylimidazole tetrafluoroborate;
the 1-butyl-3-methylimidazolium tetrafluoroborate was prepared as described in example 1;
the chlorosilane is trimethyl chlorosilane;
the chlorine-containing silane: the weight ratio of the tetrafluoroborate ionic liquid is 1: 1;
the lubricant is magnesium stearate;
the flame retardant is phosphate flame retardant or tricyanurate flame retardant;
the phosphate ester flame retardant comprises: the weight ratio of the tricyanurate flame retardant is 1: 2;
the phosphate flame retardant is tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate;
the tricyanurate flame retardant is tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate;
the tetrakis (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate was prepared by the same method as in example 1;
the tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate was prepared in the same manner as in example 1;
the dispersing agent is sodium dodecyl sulfate;
the polyamide is nylon 66;
the epoxy resin is bisphenol A epoxy resin;
the preparation method of the silica aerogel heat-insulating sealing material is the same as that of the embodiment 1.
Comparative example 5
The silicon dioxide aerogel heat-insulation sealing material comprises the following raw materials in parts by weight: 7 parts of silicon dioxide aerogel, 100 parts of polyurethane, 2 parts of ionic liquid, 16 parts of chlorosilane, 4 parts of cenospheres, 1.8 parts of lubricating agent, 3 parts of flame retardant, 3 parts of dispersing agent, 1.5 parts of talcum powder, 10 parts of polyamide, 48 parts of polytetrafluoroethylene, 4 parts of guar gum and 12 parts of epoxy resin.
The polyurethane is a polyurethane elastomer;
the preparation method of the polyurethane elastomer is the same as that of the polyurethane elastomer in example 1;
the ionic liquid is 1-butyl-3-methylimidazole tetrafluoroborate;
the 1-butyl-3-methylimidazolium tetrafluoroborate was prepared as described in example 1;
the chlorosilane is trimethyl chlorosilane;
the chlorine-containing silane: the weight ratio of the tetrafluoroborate ionic liquid is 8: 1;
the lubricant is magnesium stearate;
the flame retardant is phosphate flame retardant or tricyanurate flame retardant;
the phosphate ester flame retardant comprises: the weight ratio of the tricyanurate flame retardant is 1: 2;
the phosphate flame retardant is tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate;
the tricyanurate flame retardant is tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate;
the tetrakis (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate was prepared by the same method as in example 1;
the tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate was prepared in the same manner as in example 1;
the dispersing agent is sodium dodecyl sulfate;
the polyamide is nylon 66;
the epoxy resin is bisphenol A epoxy resin;
the preparation method of the silica aerogel heat-insulating sealing material is the same as that of the embodiment 1.
Comparative example 6
The silicon dioxide aerogel heat-insulation sealing material comprises the following raw materials in parts by weight: 7 parts of silicon dioxide aerogel, 100 parts of polyurethane, 2 parts of ionic liquid, 7 parts of chlorosilane, 4 parts of cenospheres, 1.8 parts of lubricating agent, 3 parts of dispersing agent, 1.5 parts of talcum powder, 10 parts of polyamide, 48 parts of polytetrafluoroethylene, 4 parts of guar gum and 12 parts of epoxy resin.
The polyurethane is a polyurethane elastomer;
the preparation method of the polyurethane elastomer is the same as that of the polyurethane elastomer in example 1;
the ionic liquid is 1-butyl-3-methylimidazole tetrafluoroborate;
the 1-butyl-3-methylimidazolium tetrafluoroborate was prepared as described in example 1;
the chlorosilane is trimethyl chlorosilane;
the chlorine-containing silane: the weight ratio of the tetrafluoroborate ionic liquid is 3.5: 1;
the lubricant is magnesium stearate;
the dispersing agent is sodium dodecyl sulfate;
the polyamide is nylon 66;
the epoxy resin is bisphenol A epoxy resin;
the preparation method of the silica aerogel heat-insulation sealing material comprises the following steps:
(1) mixing silicon dioxide aerogel, polyurethane, ionic liquid, chlorosilane and hollow microspheres, and performing ultrasonic assistance to obtain a first mixture;
(2) wet ball milling polyamide, epoxy resin and polytetrafluoroethylene to 90 meshes to obtain a second mixture;
(3) adding the second mixture, the lubricant and the dispersant into a high-speed mixer, mixing for 10min, adding the talcum powder, mixing for 25min at 70 ℃, and naturally cooling to normal temperature to obtain a third mixture;
(4) adding the first mixture, the third mixture and guar gum into a double-screw extruder, wherein the extrusion temperature is 160 ℃, and the screw rotation speed is 55 Hz; and cooling, shaping, drawing, cutting and blanking to obtain a finished product.
Comparative example 7
The silicon dioxide aerogel heat-insulation sealing material comprises the following raw materials in parts by weight: 7 parts of silicon dioxide aerogel, 100 parts of polyurethane, 2 parts of ionic liquid, 7 parts of chlorosilane, 4 parts of cenospheres, 1.8 parts of lubricating agent, 3 parts of flame retardant, 3 parts of dispersing agent, 1.5 parts of talcum powder, 10 parts of polyamide, 48 parts of polytetrafluoroethylene, 4 parts of guar gum and 12 parts of epoxy resin.
The polyurethane is a polyurethane elastomer;
the preparation method of the polyurethane elastomer is the same as that of the polyurethane elastomer in example 1;
the ionic liquid is 1-butyl-3-methylimidazole tetrafluoroborate;
the 1-butyl-3-methylimidazolium tetrafluoroborate was prepared as described in example 1;
the chlorosilane is trimethyl chlorosilane;
and (3) chlorosilane-containing: the weight ratio of the tetrafluoroborate ionic liquid is 3.5: 1;
the flame retardant is a phosphate flame retardant;
the phosphate flame retardant is tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate;
the tetrakis (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate was prepared by the same method as in example 1;
the dispersing agent is sodium dodecyl sulfate;
the polyamide is nylon 66;
the epoxy resin is bisphenol A epoxy resin;
the preparation method of the silica aerogel heat insulation sealing material is the same as that of the embodiment 1.
Comparative example 8
The silicon dioxide aerogel heat-insulation sealing material comprises the following raw materials in parts by weight: 7 parts of silicon dioxide aerogel, 100 parts of polyurethane, 2 parts of ionic liquid, 7 parts of chlorosilane, 4 parts of cenospheres, 1.8 parts of lubricating agent, 3 parts of flame retardant, 3 parts of dispersing agent, 1.5 parts of talcum powder, 10 parts of polyamide, 48 parts of polytetrafluoroethylene, 4 parts of guar gum and 12 parts of epoxy resin.
The polyurethane is a polyurethane elastomer;
the preparation method of the polyurethane elastomer is the same as that of the polyurethane elastomer in example 1;
the ionic liquid is 1-butyl-3-methylimidazole tetrafluoroborate;
the 1-butyl-3-methylimidazolium tetrafluoroborate was prepared as described in example 1;
the chlorosilane is trimethyl chlorosilane;
and (3) chlorosilane-containing: the weight ratio of the tetrafluoroborate ionic liquid is 3.5: 1;
the flame retardant is a tricyanurate flame retardant;
the tricyanurate flame retardant is tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate;
the tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate was prepared in the same manner as in example 1;
the dispersing agent is sodium dodecyl sulfate;
the polyamide is nylon 66;
the epoxy resin is bisphenol A epoxy resin;
the preparation method of the silica aerogel heat insulation sealing material is the same as that of the embodiment 1.
Example 9
The silicon dioxide aerogel heat-insulation sealing material comprises the following raw materials in parts by weight: 7 parts of silicon dioxide aerogel, 100 parts of polyurethane, 2 parts of ionic liquid, 7 parts of chlorosilane, 4 parts of cenospheres, 1.8 parts of lubricating agent, 3 parts of flame retardant, 3 parts of dispersing agent, 1.5 parts of talcum powder, 10 parts of polyamide, 48 parts of polytetrafluoroethylene, 4 parts of guar gum and 12 parts of epoxy resin.
The polyurethane is a polyurethane elastomer;
the preparation method of the polyurethane elastomer is the same as that of the polyurethane elastomer in example 1;
the ionic liquid is 1-butyl-3-methylimidazole tetrafluoroborate;
the 1-butyl-3-methylimidazolium tetrafluoroborate was prepared as described in example 1;
the chlorosilane is trimethyl chlorosilane;
and (3) chlorosilane-containing: the weight ratio of the tetrafluoroborate ionic liquid is 3.5: 1;
the lubricant is magnesium stearate;
the flame retardant is phosphate flame retardant or tricyanurate flame retardant;
the phosphate ester flame retardant comprises: the weight ratio of the tricyanurate flame retardant is 1: 0.5;
the phosphate flame retardant is tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate;
the tricyanurate flame retardant is tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate;
the tetrakis (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate was prepared by the same method as in example 1;
the tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate was prepared in the same manner as in example 1;
the dispersing agent is sodium dodecyl sulfate;
the polyamide is nylon 66;
the epoxy resin is bisphenol A epoxy resin;
the preparation method of the silica aerogel heat insulation sealing material is the same as that of the embodiment 1.
Comparative example 10
The silicon dioxide aerogel heat-insulation sealing material comprises the following raw materials in parts by weight: 7 parts of silicon dioxide aerogel, 100 parts of polyurethane, 2 parts of ionic liquid, 7 parts of chlorosilane, 4 parts of cenospheres, 1.8 parts of lubricating agent, 3 parts of flame retardant, 3 parts of dispersing agent, 1.5 parts of talcum powder, 10 parts of polyamide, 48 parts of polytetrafluoroethylene, 4 parts of guar gum and 12 parts of epoxy resin.
The polyurethane is a polyurethane elastomer;
the preparation method of the polyurethane elastomer is the same as that of the polyurethane elastomer in example 1;
the ionic liquid is 1-butyl-3-methylimidazole tetrafluoroborate;
the 1-butyl-3-methylimidazolium tetrafluoroborate was prepared as described in example 1;
the chlorosilane is trimethyl chlorosilane;
and (3) chlorosilane-containing: the weight ratio of the tetrafluoroborate ionic liquid is 3.5: 1;
the lubricant is magnesium stearate;
the flame retardant is phosphate flame retardant or tricyanurate flame retardant;
the phosphate ester flame retardant comprises: the weight ratio of the tricyanurate flame retardant is 1: 5;
the phosphate flame retardant is tetra (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate;
the tricyanurate flame retardant is tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate;
the tetrakis (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate was prepared by the same method as in example 1;
the tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate was prepared in the same manner as in example 1;
the dispersing agent is sodium dodecyl sulfate;
the polyamide is nylon 66;
the epoxy resin is bisphenol A epoxy resin;
the preparation method of the silica aerogel heat insulation sealing material is the same as that of the embodiment 1.
Comparative example 11
The silicon dioxide aerogel heat-insulation sealing material comprises the following raw materials in parts by weight: 7 parts of silicon dioxide aerogel, 100 parts of polyurethane, 4 parts of hollow microspheres, 1.8 parts of lubricating agent, 3 parts of dispersing agent, 1.5 parts of talcum powder, 10 parts of polyamide, 48 parts of polytetrafluoroethylene, 4 parts of guar gum and 12 parts of epoxy resin.
The polyurethane is a polyurethane elastomer;
the preparation method of the polyurethane elastomer is the same as that of the polyurethane elastomer in example 1;
the lubricant is magnesium stearate;
the dispersing agent is sodium dodecyl sulfate;
the polyamide is nylon 66;
the epoxy resin is bisphenol A epoxy resin;
the preparation method of the silica aerogel heat-insulation sealing material comprises the following steps:
(1) mixing silicon dioxide aerogel, polyurethane and hollow microspheres and carrying out ultrasonic assistance to obtain a first mixture;
(2) wet ball milling polyamide, epoxy resin and polytetrafluoroethylene to 90 meshes to obtain a second mixture;
(3) adding the second mixture, the lubricant and the dispersant into a high-speed mixer, mixing for 10min, adding the talcum powder, mixing for 25min at 70 ℃, and naturally cooling to normal temperature to obtain a third mixture;
(4) adding the first mixture, the third mixture and guar gum into a double-screw extruder, wherein the extrusion temperature is 160 ℃, and the screw rotation speed is 55 Hz; and cooling, shaping, drawing, cutting and blanking to obtain a finished product.
Performance evaluation:
1. measuring the limiting oxygen index of the silica aerogel heat insulation sealing material: national standard GB/T2046.2-2009;
2. measuring the contact angle of the silica aerogel heat insulation sealing material: national standard GB/T30693-2014;
3. measuring the tensile strength of the silica aerogel heat insulation sealing material: the national standard GB/T1040-92.
Table 1 performance test data
As can be seen from Table 1, the silica aerogel heat-insulating sealing material provided by the invention has good flame retardance, hydrophobicity and mechanical property.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (10)
1. The silicon dioxide aerogel heat-insulation sealing material is characterized by comprising the following raw materials in parts by weight: 5-8 parts of silicon dioxide aerogel, 95-105 parts of polyurethane, 1.5-3 parts of ionic liquid, 4-10 parts of chlorosilane, 3-5 parts of hollow microspheres, 1.5-2 parts of lubricant, 1-5 parts of flame retardant, 2-4 parts of dispersant, 1-2 parts of talcum powder, 9-11 parts of polyamide, 45-50 parts of polytetrafluoroethylene, 3-5 parts of guar gum and 10-13 parts of epoxy resin.
2. The silica aerogel thermal insulation seal material according to claim 1, wherein the ionic liquid is a tetrafluoroborate ionic liquid.
3. The silica aerogel thermal insulation seal material of claim 2, wherein the tetrafluoroborate ionic liquid is at least one of 1-butyl-3-methylimidazolium tetrafluoroborate, 1-ethyl-3-methylimidazolium tetrafluoroborate, 1-pentyl-3-methylimidazolium tetrafluoroborate, and 1-hexyl-3-methylimidazolium tetrafluoroborate.
4. The silica aerogel thermal insulation seal material according to claim 1, wherein the chlorosilane-containing: the weight ratio of the tetrafluoroborate ionic liquid is (3-4): 1.
5. the silica aerogel thermal insulation sealing material according to claim 1, wherein the chlorosilane is trimethylchlorosilane.
6. The silica aerogel heat insulation sealing material according to claim 1, wherein the flame retardant is phosphate ester flame retardant or tricyanurate flame retardant.
7. The silica aerogel heat insulation sealing material according to claim 6, wherein the phosphate ester flame retardant: the weight ratio of the tricyanurate flame retardant is 1 (1.5-2.5).
8. The silica aerogel thermal insulation sealing material according to claim 6 or 7, wherein the phosphate ester flame retardant is tetrakis (1,2,2,6, 6-pentamethyl-4-piperidyl) pyrophosphate.
9. The silica aerogel heat and seal material according to claim 6 or 7, wherein the tricyanurate flame retardant is tris {2- [ dimethyl (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2] octyl-4-methoxy) siloxy ] ethyl } isocyanurate.
10. A method for preparing a silica aerogel sealing material according to any of claims 1 to 9, comprising the steps of:
(1) mixing silicon dioxide aerogel, polyurethane, ionic liquid, chlorosilane and hollow microspheres, and performing ultrasonic assistance to obtain a first mixture;
(2) wet ball milling polyamide, epoxy resin and polytetrafluoroethylene to 90-100 meshes to obtain a second mixture;
(3) adding the second mixture, the lubricant, the dispersant and the flame retardant into a high-speed mixer, mixing for 8-10min, adding the talcum powder, mixing for 20-25min at 60-70 ℃, and naturally cooling to normal temperature to obtain a third mixture;
(4) adding the first mixture, the third mixture and guar gum into a double-screw extruder, wherein the extrusion temperature is 140-165 ℃, and the screw rotation speed is 40-70 Hz; and cooling, shaping, drawing, cutting and blanking to obtain a finished product.
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