CN111471251A - Aerogel-containing heat insulation material and preparation method thereof - Google Patents
Aerogel-containing heat insulation material and preparation method thereof Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C08J2309/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
- C08J2309/02—Copolymers with acrylonitrile
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- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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- C08J2409/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
- C08J2409/02—Copolymers with acrylonitrile
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- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2427/06—Homopolymers or copolymers of vinyl chloride
Abstract
The invention discloses an aerogel-containing heat insulation material which comprises an organic foaming material base material, and graphene aerogel particles and phase change microcapsules which are dispersed in the base material. The preparation method comprises the following steps: pre-swelling polyvinyl chloride, plasticizing polyvinyl chloride, melting and blending nitrile rubber and polyvinyl chloride, open mixing at low temperature, foaming by die pressing and slicing. The aerogel-containing heat insulation material provided by the invention is low in production cost, excellent in cold resistance, low in density, good in bending resistance and softness, free of aerogel dust overflow, washable and beneficial to a human body. The aerogel-containing heat insulation material is mainly used as a cold-proof heat insulation material in a natural environment at a low temperature, is particularly suitable for being applied to the fields of textile clothing, home textiles, outdoor products and the like, and widens the application range of the aerogel.
Description
Technical Field
The invention relates to a heat insulation material, in particular to an aerogel-containing heat insulation material and a preparation method thereof, belonging to the technical field of heat insulation materials.
Background
In cold winter, people usually select various clothes made of cold-proof and warm-keeping materials, such as warm-keeping clothes using down or chemical fiber cotton as filler, and warm-keeping clothes made of animal fur or fur-like materials, which can basically meet the daily warm-keeping requirements of people. The clothes using the down feather as the filler are relatively light and have good heat retention, but the heat retention in a humid environment is greatly reduced, and meanwhile, the problems of being too bulky to wear, easy to run down, difficult to clean, easy to mildew and the like exist, so that the wearing experience and the service life are influenced. However, the thermal clothes adopting animal fur or imitated fur have good thermal insulation, but have the problems of heavy weight, inconvenient movement, difficult nursing and the like. New cold-proof and warm-keeping materials are always the focus of research of people.
Aerogel is a nano-porous solid material with low density and high porosity, and is the best solid material with heat insulation performance at present. Graphene is a new material which is emerging in recent years, the graphene aerogel combines various excellent performances of graphene and aerogel, has the general characteristics of common aerogel and also has excellent far infrared performance, the normal emissivity of the far infrared with the wavelength of 6-14 mu m reaches over 88 percent, and the graphene aerogel can assist in promoting human microcirculation; meanwhile, the graphene has the advantages of antibiosis, peculiar smell absorption, static resistance and the like. The graphene aerogel is applied to the field of textile and clothing, and the benefit to the body can be greatly improved.
Phase change materials are materials that can absorb or release a large amount of energy (i.e., enthalpy of phase change) when a substance undergoes a phase change, and have the ability to change its physical state within a certain temperature range. When the physical state of the phase-change material is changed, the temperature of the material is almost kept unchanged before the phase change is completed, a wide temperature platform is formed, and although the temperature is unchanged, the latent heat absorbed or released is quite large. Dispersing the phase-change material into spherical small particles, and then encapsulating a layer of shell material with stable performance on the surface to finally form the phase-change microcapsule. The phase-change material is microencapsulated, thereby well solving the problems and difficulties in the application of the phase-change material.
The foaming heat-insulating material is a porous material with lower density, and is a product with fine pores. The material has low thermal conductivity, can well play a role in heat preservation and insulation, and has wide application in the field of heat insulation and cold protection.
How to combine the advantages of the three materials to prepare a novel heat insulation material is a problem to be solved by the technical personnel in the field.
Disclosure of Invention
The technical problems to be solved by the invention are as follows:
(1) the aerogel manufactured in the form of particles, blocks and films has high brittleness, cannot resist external force impact when existing alone, and is limited in application;
(2) the existing organic flexible aerogel has high difficulty in batch production and high cost, and is not suitable for the use in the civil market at present;
(3) the existing aerogel powder composite inorganic fiber felt product has high weight, poor bending property and easy overflow of aerogel dust, and has great limitation on use scenes such as light weight, softness, frequent bending and washing;
(4) when the aerogel is applied to a cold-proof material on the surface of a human body, the condition that the human body feels too hot can occur.
In order to solve the technical problems, the invention combines the advantages of aerogel materials, phase-change materials and foaming materials to provide a novel heat-insulating material. According to the invention, graphene aerogel particles and a phase-change microcapsule material are used as main modified fillers, an organic foaming material is used as a base material, and the graphene aerogel particles and the phase-change microcapsule material are blended to prepare the composite material containing graphene aerogel. The technical scheme is as follows:
in a first aspect of the present invention, there is provided an aerogel-containing insulation material, comprising a base material of an organic foam material, and graphene aerogel particles and phase-change microcapsules dispersed in the base material.
In some embodiments, the average particle size of the graphene aerogel particles and the phase change microcapsules is less than 15 microns.
In some embodiments, the average particle size of the graphene aerogel particles and the phase-change microcapsules is in a range of 100 to 500 nanometers.
In some embodiments, the organic foam material is a blend foam material of nitrile rubber and polyvinyl chloride.
In some embodiments, the nitrile rubber is present in an amount of 50 to 80 parts by weight and the polyvinyl chloride is present in an amount of 20 to 50 parts by weight.
In some embodiments, the nitrile rubber is present at 50 parts by weight and the polyvinyl chloride is present at 50 parts by weight.
In some embodiments, the degree of polymerization of the polyvinyl chloride prior to foaming is 700 to 1500.
In some embodiments, the degree of polymerization of the polyvinyl chloride prior to foaming is 1000.
In a second aspect of the present invention, there is provided a method for preparing an aerogel-containing insulation material, comprising the steps of:
firstly, pre-swelling polyvinyl chloride;
step two, plasticizing polyvinyl chloride;
thirdly, melting and blending the polyvinyl chloride and the nitrile rubber to obtain a master batch;
step four, adding a foaming agent, a deodorant, a vulcanizing agent, an accelerant, graphene aerogel particles and a phase-change microcapsule into the masterbatch for fully mixing to obtain a foaming precursor;
and step five, foaming and vulcanizing the foaming precursor.
In some embodiments, a method of making an aerogel-containing insulation material comprises the steps of:
step one, heating polyvinyl chloride to above 60 ℃, adding a plasticizer and a heat stabilizer, and fully and uniformly mixing to complete pre-swelling;
secondly, performing thin-pass plasticization on the pre-swelled polyvinyl chloride on an internal mixer until the polyvinyl chloride is uniform and transparent, and completing the plasticization; the banburying temperature is 130-145 ℃, and the stirring speed is 40-60 r/min;
mixing the plasticized nitrile rubber and the plasticized polyvinyl chloride, and adding zinc oxide, stearic acid, an anti-aging agent, white carbon black and calcium carbonate for banburying to obtain a master batch; banburying temperature is 140-170 ℃, stirring speed is 60-80r/min, and time is 7-15 min;
step four, adding a foaming agent, a deodorant, a vulcanizing agent, an accelerant, graphene aerogel particles and a phase-change microcapsule material into the masterbatch for fully mixing; the temperature is 50-60 ℃, the roller speed is 20r/min, the sheet is taken out after passing through the roller for 3-5 times, and the sheet is placed for 24 hours; cutting the sample according to the size of the mould to obtain a foaming precursor;
putting the foaming precursor into a mold, and then placing the mold on a flat vulcanizing machine for mold pressing foaming and vulcanizing; the temperature is 150-165 ℃, the pressure is 7-12 MPa, and the time is 8-15 min, so as to obtain a foamed product;
and step six, cutting the foamed product into sheet materials with uniform thickness by a slicing machine, namely the aerogel-containing heat insulation material.
The invention has the beneficial effects that: the aerogel-containing heat insulation material provided by the invention is low in production cost, excellent in cold resistance, low in density, good in bending resistance and softness, free of aerogel dust overflow, washable and beneficial to a human body. The aerogel-containing heat insulation material is mainly used as a cold-proof heat insulation material in a natural environment at a low temperature, is particularly suitable for being applied to the fields of textile clothing, home textiles, outdoor products and the like, and widens the application range of the aerogel.
Drawings
FIG. 1 is a photomicrograph of aerogel-containing insulation as provided in a preferred embodiment of the present invention.
Detailed Description
The invention provides an aerogel-containing heat-insulating composite material and a preparation method thereof, wherein graphene aerogel powder, a phase-change microcapsule material and a foaming material with excellent heat-insulating property are combined to obtain the composite material with excellent heat-insulating effect, the composite material is mainly applied to the low-temperature condition of natural environment to play the role of heat insulation and warm keeping, is particularly suitable for being used as a cold-proof warm-keeping material in the textile field, and has multiple functions, is light and thin, has good heat-insulating property, can be bent and washed by water. The invention widens the application field of the aerogel material. The conception, the specific structure, and the technical effects produced by the present invention will be further described below to fully understand the objects, the features, and the effects of the present invention.
[ selection of raw materials ]
The combination of Nitrile Butadiene Rubber (NBR) and polyvinyl chloride (PVC) is a precursor for rubber and plastic, and has been in history for more than 70 years. From thermodynamic compatibility analysis, the solubility parameters of the nitrile rubber and the polyvinyl chloride are close, the nitrile rubber and the polyvinyl chloride have thermodynamic miscibility, and the nitrile rubber and the polyvinyl chloride can be foamed together to integrate the advantages of the nitrile rubber and the polyvinyl chloride, so that the product has good performances such as good rebound resilience, low density, small shrinkage deformation rate, good heat preservation property and the like. Therefore, nitrile rubber and polyvinyl chloride are preferably selected as the foaming main materials in the present invention.
According to the invention, graphene aerogel powder and phase change microcapsule powder are used as modified fillers, NBR-PVC rubber and plastic blended materials are used as base materials, the proportion of nitrile rubber and polyvinyl chloride and the amount of foaming agents are controlled, and the size and the opening rate of foam pores are further controlled, so that an ideal heat preservation and insulation effect is achieved.
The aerogel heat insulation material comprises 100 parts of nitrile-butadiene rubber (NBR) and polyvinyl chloride (PVC), wherein the nitrile-butadiene rubber accounts for 50-80 parts, and the polyvinyl chloride accounts for 20-50 parts. Preferably, the nitrile rubber and the polyvinyl chloride respectively account for 50 parts, and the obtained foaming material has relatively low density, relatively large foam holes, thinner foam walls and lighter weight under the same volume, and is more suitable for being used as a cold-proof and warm-keeping material. The polymerization degree of the polyvinyl chloride raw material is 700-1500, and the preferred polymerization degree is 1000. As the degree of polymerization increases, the cells of the foamed material become smaller and the open cell content decreases, and the foaming agent exerts a preferable effect at around 1000 degrees of polymerization. The nitrile rubber is prepared from butadiene and acrylonitrile by an emulsion polymerization method. Because the material of the invention is mainly applied to cold-resistant warm-keeping materials, the acrylonitrile content does not need to be too high, so as to improve the condition that the foaming material becomes hard under the low-temperature condition. In the nitrile rubber used in the invention, the acrylonitrile content is less than or equal to 35 percent, and the lower the acrylonitrile content is, the better the cold resistance of the obtained product is.
12-20 parts of plasticizer trioctyl trimellitate (TOTM) besides the raw materials of nitrile rubber and polyvinyl chloride; the calcium/zinc heat stabilizer takes 5 percent of the dosage of the polyvinyl chloride; 3-5 parts of zinc oxide; 1-2 parts of stearic acid; 10-20 parts of foaming agent Azodicarbonamide (AC); 1-5 parts of sulfur; 0.5-1 part of promoter TMTD (TT); 1-2 parts of a promoter (CZ), chemical name: n-cyclohexyl-2-benzothiazolesulfenamide; 3 parts of an anti-aging agent; 5-15 parts of graphene aerogel; 5-15 parts of phase change microcapsules; 15-35 parts of light calcium carbonate (the particle size is 50-100 nm); 10-20 parts of white carbon black; 1-2 parts of a deodorant. The raw materials are calculated by weight, and the total weight of the nitrile rubber and the polyvinyl chloride is 100 parts.
The melting temperature of the phase-change material in the phase-change microcapsule is 25-35 ℃, preferably 29-31 ℃, and the melting enthalpy is more than or equal to 15 kJ/kg. The heat-insulating material provided by the invention is mostly used as an intermediate layer material of winter cold-proof coats in consideration of application scenes, and the temperature between the body surface of a human body and the outer coat is kept at about 30 ℃ so that the human body is comfortable. Under certain conditions, when the temperature is reduced, the phase-change material can be solidified to release heat, the heat is returned to a human body, the heating effect is generated, and the body is kept warm; when the temperature rises, the phase-change material can melt, absorbs heat to generate a cooling effect, so that a human body feels cool, and the phase-change material has a buffering effect on temperature change. The phase-change material is added, so that when the heat-insulating material is applied to the field of clothes, the wearing comfort is greatly improved, and the condition that a wearer feels overheat due to the fact that the heat-insulating performance of the aerogel composite material is too good can be remarkably improved.
The average particle size of the phase-change microcapsules and the graphene aerogel powder needs to be less than 15 micrometers, and the preferred average particle size range is 100-500 nm.
[ Process steps ]
Step one, pre-swelling polyvinyl chloride
Heating polyvinyl chloride to 60 ℃, adding triisooctyl trimellitate plasticizer (TOTM) and calcium/zinc heat stabilizer as plasticizers, fully and uniformly mixing the raw materials in a mechanical stirring machine at a rotation speed of about 400r/min for more than 5min to prepare paste, and then placing the paste in an oven at 40 ℃ for 2 h.
When the polyvinyl chloride is processed at the temperature of more than 130 ℃, violent thermal degradation can occur, and the polyvinyl chloride cannot be directly mixed at high temperature in an open mill, so that the polyvinyl chloride must be firstly swelled, namely, the polyvinyl chloride, the micromolecule plasticizer and the heat stabilizer are added into stirring equipment for mixing, so that the micromolecule plasticizer enters into a macromolecular chain, and the interaction force among macromolecules is reduced. The heat stabilizer can improve the thermal stability of the polyvinyl chloride and the thermal decomposition temperature of the polyvinyl chloride. Polyvinyl chloride which is fully swelled is a soft mixture which is loose and elastic and is easy to mix with soft rubber.
Step two, polyvinyl chloride plasticization
And (3) putting the swelled polyvinyl chloride into an internal mixer for plasticizing for 3-5 min, and then thinly passing the polyvinyl chloride until the polyvinyl chloride is uniform and transparent. The temperature of the banburying chamber is 130-145 ℃, and the stirring speed is 40-60 r/min.
Step three, melt blending
Mixing the plasticized nitrile-butadiene rubber with the three sections with the plasticized polyvinyl chloride, adding zinc oxide, stearic acid, an anti-aging agent, white carbon black, calcium carbonate and the like for densification at the temperature of 140-170 ℃, stirring at the speed of 60-80r/min for 7-15 min, blanking to prepare NBR/PVC master batch, and placing to room temperature.
Step four, low-temperature open mixing
Adding a foaming agent, a deodorant, a vulcanizing agent, an accelerant, graphene aerogel and a phase-change microcapsule material into the NBR/PVC master batch, mixing at a low temperature of 50-60 ℃ at a roll speed of 20r/min, thinly passing for 3-5 times, then discharging, standing for 24h, and cutting according to the size of a mold.
Step five, mould pressing foaming
And putting the prepared sheet into a mold, and then placing the mold on a flat vulcanizing machine for mold pressing, foaming and vulcanizing at the temperature of 150-165 ℃, under the pressure of 7-12 MPa for 8-15 min to obtain the product.
Step six, slicing
The product is cut by a slicer to obtain a sheet-like composite material with uniform thickness, and the thickness can be 0.5mm at the thinnest.
Compared with the traditional materials applied in the textile field, the invention has the following obvious advantages:
(1) the graphene aerogel and the foaming material are combined to prepare the foaming composite material containing the aerogel, so that the synergistic effect of the graphene aerogel and the foaming material can be exerted, the heat preservation performance is improved, and the far infrared heating function and the adsorption performance of the graphene are realized;
(2) compared with the traditional down feather material, the composite material obtained by the invention is not limited by environment, can cope with low-temperature environment in nature, and can still exert better cold-proof and warm-keeping effects under wet condition;
(3) compared with the traditional heat-insulating material, the heat-insulating composite material provided by the invention has the same heat-insulating effect and smaller volume, so that the made clothes are thinner and lighter, and the activity in a low-temperature environment is facilitated;
(4) the addition of the phase-change material can effectively improve the situation of body overheating in certain states, such as outdoor sports;
(5) the novel functional heat-insulation material applicable to the textile field is realized, more design choices are provided for textile cold-resisting products, and the requirements of different people are better met;
(6) the addition of the deodorant and the graphene aerogel ensures that the obtained foaming composite material almost has no peculiar smell, and can be better applied to the field of cold protection and heat preservation around human bodies.
Example 1
The formula of the raw materials in parts by mass is as follows:
NBR (acrylonitrile content 25%, 50 parts)/PVC (polymerization degree 1000, 50 parts), 100 parts of NBR and PVC, 14 parts of plasticizer TOTM, 2.5 parts of PVC dosage of calcium/zinc heat stabilizer, 5 parts of zinc oxide, 1.5 parts of stearic acid, 15 parts of foaming agent AC, 1.5 parts of sulfur, 1 part of accelerator TMTD (TT), 1.2 parts of accelerator CZ, 3 parts of anti-aging agent, 8 parts of graphene aerogel, 8 parts of phase change microcapsule, 20 parts of light calcium carbonate (average particle size 70nm), 10 parts of white carbon black and 2 parts of odor removing agent.
The preparation process of the aerogel-containing heat insulation material comprises the following steps:
step one, PVC pre-swelling
Heating PVC to 60 deg.C, adding plasticizer triisooctyl trimellitate (TOTM) and calcium/zinc heat stabilizer, mixing the raw materials in mechanical stirring machine at 400r/min for 5min to obtain paste, and placing in oven at 40 deg.C for 2 h.
Step two, PVC plasticization
And (3) plasticizing the pre-swelled PVC in an internal mixer for 4min, and performing thin-pass plasticizing on a high-temperature internal mixer until the mixture is uniform and transparent, wherein the temperature of an internal mixing chamber is 135 ℃, and the stirring speed is 40 r/min.
Step three, melt blending
Mixing the plasticated NBR in three sections with the plasticated PVC, adding zinc oxide, stearic acid, an anti-aging agent, white carbon black, calcium carbonate and the like for densification, stirring at the temperature of 150 ℃ and the stirring speed of 60r/min for 9min, blanking to prepare NBR/PVC master batch, and placing to room temperature.
Step four, low-temperature open mixing
Adding a foaming agent, a deodorant, a vulcanizing agent, an accelerant, graphene aerogel and a phase-change microcapsule material into the NBR/PVC master batch, mixing at a low temperature of 50 ℃, rolling at a speed of 20r/min, thinly passing for 3-5 times, then taking the mixture out, standing for 24 hours, and cutting according to the size of a mold.
Step five, mould pressing foaming
And putting the prepared sheet into a mold, and then placing the mold on a flat vulcanizing machine for mold pressing, foaming and vulcanizing at the temperature of 155 ℃, under the pressure of 9MPa for 10min to obtain the product.
Step six, slicing
After slicing, the flaky foaming material with the thickness of 2mm, namely the finished product of the aerogel-containing composite material, is obtained.
The aerogel-containing composite finished product was tested and the SEM image is shown in FIG. 1, where the cell size was relatively uniform. The density of the composite material is measured to be 0.059g/cm3Thermal resistance 0.0407m2K/W. The contrast sample is dupont SORONA flocculus-shaped cotton with excellent heat preservation performance in the current market and the gram weight of 200g/m2And the thickness is 3cm, and the thermal resistance values are equivalent. The gram weight of the composite material of the invention is 118g/m2The thickness is only 1/15 of DuPont cotton, so that the cold-proof effect is excellent, and the thickness of the textile finished product can be greatly reduced when the fabric is applied to textile products.
In addition, the composite material is tested for far infrared heating function and peculiar smell removal function. The far infrared heating function is tested according to GB/T30127-2013, the far infrared emissivity is 0.89, and the far infrared heating material has far infrared performance. According to the odor eliminating function of the product tested by GB/T33610.2-2017, the concentration reduction rate of the ammonia odor component is 96.5%, and the concentration reduction rate of the acetic acid odor component is 99.2%, so that the product has a good odor eliminating function.
Example 2
The formula of the raw materials in parts by mass is as follows:
NBR (acrylonitrile content 25%, 50 parts)/PVC (polymerization degree 1000, 50 parts), 100 parts of NBR and PVC, 14 parts of plasticizer TOTM, 2.5 parts of PVC dosage of calcium/zinc heat stabilizer, 5 parts of zinc oxide, 1.5 parts of stearic acid, 13 parts of foaming agent AC, 1.5 parts of sulfur, 1 part of accelerator TMTD (TT), 1.2 parts of accelerator CZ, 3 parts of anti-aging agent, 10 parts of graphene aerogel, 8 parts of phase change microcapsule, 20 parts of light calcium carbonate (average particle size 70nm), 10 parts of white carbon black and 2 parts of odor removing agent.
The preparation process of the aerogel-containing heat insulation material comprises the following steps:
step one, PVC pre-swelling
Heating PVC to 60 deg.C, adding plasticizer triisooctyl trimellitate (TOTM) and calcium/zinc heat stabilizer, mixing the raw materials in mechanical stirring machine at 400r/min for 5min to obtain paste, and placing in oven at 40 deg.C for 2 h.
Step two, PVC plasticization
And (3) plasticizing the pre-swelled PVC in an internal mixer for 4min, and performing thin-pass plasticizing on a high-temperature internal mixer until the mixture is uniform and transparent, wherein the temperature of an internal mixing chamber is 135 ℃, and the stirring speed is 40 r/min.
Step three, melt blending
Mixing the plasticated NBR in three sections with the plasticated PVC, adding zinc oxide, stearic acid, an anti-aging agent, white carbon black, calcium carbonate and the like for densification, stirring at the temperature of 150 ℃ and the stirring speed of 60r/min for 9min, blanking to prepare NBR/PVC master batch, and placing to room temperature.
Step four, low-temperature open mixing
Adding a foaming agent, a deodorant, a vulcanizing agent, an accelerant, graphene aerogel and a phase-change microcapsule material into the NBR/PVC master batch, mixing at a low temperature of 50 ℃, rolling at a speed of 20r/min, thinly passing for 3-5 times, then taking the mixture out, standing for 24 hours, and cutting according to the size of a mold.
Step five, mould pressing foaming
And putting the prepared sheet into a mold, and then placing the mold on a flat vulcanizing machine for mold pressing, foaming and vulcanizing at the temperature of 155 ℃, under the pressure of 9MPa for 10min to obtain the product.
Step six, slicing
After slicing, the flaky foaming material with the thickness of 2mm, namely the finished product of the aerogel-containing composite material, is obtained.
The aerogel-containing composite material finished product is tested, and the density of the composite material is measured to be 0.048g/cm3Thermal resistance of 0.0457m2K/W. The contrast sample is dupont SORONA flocculus-shaped cotton with excellent heat preservation performance in the current market and the gram weight of 200g/m2And the thickness is 3cm, and the thermal resistance values are equivalent. The gram weight of the composite material of the invention is 118g/m2The thickness is only 1/15 of DuPont cotton, so that the cold-proof effect is excellent, and the thickness of the textile finished product can be greatly reduced when the fabric is applied to textile products.
In addition, the composite material is tested for far infrared heating function and peculiar smell removal function. The far infrared heating function is tested according to GB/T30127-2013, the far infrared emissivity is 0.89, and the far infrared heating material has far infrared performance. According to the odor eliminating function of the product tested by GB/T33610.2-2017, the reduction rate of the ammonia odor component concentration is 96.2%, and the reduction rate of the acetic acid odor component concentration is 98.9%, so that the product has a good odor eliminating function.
Example 3
The formula of the raw materials in parts by mass is as follows:
NBR (acrylonitrile content 25%, 60 parts)/PVC (polymerization degree 1000, 40 parts), 100 parts of NBR and PVC, 14 parts of plasticizer TOTM, 2.5 parts of PVC dosage of calcium/zinc heat stabilizer, 5 parts of zinc oxide, 1.5 parts of stearic acid, 15 parts of foaming agent AC, 1.5 parts of sulfur, 1 part of accelerator TMTD (TT), 1.2 parts of accelerator CZ, 3 parts of anti-aging agent, 8 parts of graphene aerogel, 8 parts of phase change microcapsule, 20 parts of light calcium carbonate (average particle size 70nm), 13 parts of white carbon black and 2 parts of odor removing agent.
The preparation process of the aerogel-containing heat insulation material comprises the following steps:
step one, PVC pre-swelling
Heating PVC to 60 deg.C, adding plasticizer triisooctyl trimellitate (TOTM) and calcium/zinc heat stabilizer, mixing the raw materials in mechanical stirring machine at 400r/min for 5min to obtain paste, and placing in oven at 40 deg.C for 2 h.
Step two, PVC plasticization
And (3) plasticizing the pre-swelled PVC in an internal mixer for 4min, and performing thin-pass plasticizing on a high-temperature internal mixer until the mixture is uniform and transparent, wherein the temperature of an internal mixing chamber is 135 ℃, and the stirring speed is 40 r/min.
Step three, melt blending
Mixing the plasticated NBR in three sections with the plasticated PVC, adding zinc oxide, stearic acid, an anti-aging agent, white carbon black, calcium carbonate and the like for densification, stirring at the temperature of 150 ℃ and the stirring speed of 60r/min for 9min, blanking to prepare NBR/PVC master batch, and placing to room temperature.
Step four, low-temperature open mixing
Adding a foaming agent, a deodorant, a vulcanizing agent, an accelerant, graphene aerogel and a phase-change microcapsule material into the NBR/PVC master batch, mixing at a low temperature of 50 ℃, rolling at a speed of 20r/min, thinly passing for 3-5 times, then taking the mixture out, standing for 24 hours, and cutting according to the size of a mold.
Step five, mould pressing foaming
And putting the prepared sheet into a mold, and then placing the mold on a flat vulcanizing machine for mold pressing, foaming and vulcanizing at the temperature of 155 ℃, under the pressure of 9MPa for 10min to obtain the product.
Step six, slicing
After slicing, the flaky foaming material with the thickness of 2mm, namely the finished product of the aerogel-containing composite material, is obtained.
The aerogel-containing composite finished product was tested and the SEM image is shown in FIG. 1, where the cell size was relatively uniform. The density of the composite material is measured to be 0.061g/cm3Thermal resistance of 0.0398m2K/W. The contrast sample is dupont SORONA flocculus-shaped cotton with excellent heat preservation performance in the current market and the gram weight of 200g/m2And the thickness is 3cm, and the thermal resistance values are equivalent. The gram weight of the composite material of the invention is 118g/m2The thickness is only 1/15 of DuPont cotton, so that the cold-proof effect is excellent, and the thickness of the textile finished product can be greatly reduced when the fabric is applied to textile products.
In addition, the composite material is tested for far infrared heating function and peculiar smell removal function. The far infrared heating function is tested according to GB/T30127-2013, the far infrared emissivity is 0.89, and the far infrared heating material has far infrared performance. According to the odor eliminating function of the product tested by GB/T33610.2-2017, the concentration reduction rate of ammonia odor components is 96%, and the concentration reduction rate of acetic acid odor components is 98.8%, so that the product has a good odor eliminating function.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (10)
1. The aerogel-containing heat insulation material is characterized by comprising an organic foaming material base material, and graphene aerogel particles and phase-change microcapsules which are dispersed in the base material.
2. The aerogel-containing insulation material of claim 1, wherein the average particle size of the graphene aerogel particles and the phase-change microcapsules is less than 15 μm.
3. The aerogel-containing insulation material of claim 2, wherein the average particle size of the graphene aerogel particles and the phase-change microcapsules is in the range of 100 to 500 nm.
4. The aerogel-containing heat insulating material as claimed in claim 1, wherein the organic foam material is a blend foam material of nitrile rubber and polyvinyl chloride.
5. The aerogel-containing heat insulating material as claimed in claim 4, wherein the blend of the nitrile rubber and the polyvinyl chloride is foamed to form a material in which the nitrile rubber is present in an amount of 50 to 80 parts by weight and the polyvinyl chloride is present in an amount of 20 to 50 parts by weight.
6. The aerogel-containing insulation material of claim 5, wherein the nitrile rubber is present in an amount of 50 parts by weight, and the polyvinyl chloride is present in an amount of 50 parts by weight.
7. The aerogel-containing insulating material of claim 4, wherein the degree of polymerization of the polyvinyl chloride before foaming is 700 to 1500.
8. The aerogel-containing insulation material of claim 7, wherein the degree of polymerization of the polyvinyl chloride before foaming is 1000.
9. The preparation method of the aerogel-containing heat insulation material is characterized by comprising the following steps of:
firstly, pre-swelling polyvinyl chloride;
step two, plasticizing polyvinyl chloride;
thirdly, melting and blending the polyvinyl chloride and the nitrile rubber to obtain a master batch;
step four, adding a foaming agent, a deodorant, a vulcanizing agent, an accelerator, graphene aerogel particles and a phase-change microcapsule into the master batch, and fully mixing to obtain a foaming precursor;
and step five, foaming and vulcanizing the foaming precursor.
10. The method of claim 9, comprising the steps of:
step one, heating polyvinyl chloride to above 60 ℃, adding a plasticizer and a heat stabilizer, and fully and uniformly mixing to complete pre-swelling;
secondly, performing thin-pass plasticization on the pre-swelled polyvinyl chloride on an internal mixer until the polyvinyl chloride is uniform and transparent, and completing the plasticization; the banburying temperature is 130-145 ℃, and the stirring speed is 40-60 r/min;
mixing the plasticized nitrile rubber and the plasticized polyvinyl chloride, and adding zinc oxide, stearic acid, an anti-aging agent, white carbon black and calcium carbonate for banburying to obtain the masterbatch; banburying temperature is 140-170 ℃, stirring speed is 60-80r/min, and time is 7-15 min;
step four, adding a foaming agent, a deodorant, a vulcanizing agent, an accelerant, graphene aerogel particles and a phase-change microcapsule material into the master batch, and fully mixing; the temperature is 50-60 ℃, the roller speed is 20r/min, the sheet is taken out after passing through the roller for 3-5 times, and the sheet is placed for 24 hours; cutting a sample according to the size of the mould to obtain the foaming precursor;
putting the foaming precursor into a mold, and then placing the mold on a flat vulcanizing machine for mold pressing foaming and vulcanizing; the temperature is 150-165 ℃, the pressure is 7-12 MPa, and the time is 8-15 min, so as to obtain a foamed product;
and step six, cutting the foamed product into sheet materials with uniform thickness through a slicing machine, namely the aerogel-containing heat insulation material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112961656A (en) * | 2021-02-20 | 2021-06-15 | 青岛尼希米生物科技有限公司 | Composite phase-change temperature-regulating material and preparation method thereof, multiple phase-change temperature-regulating fiber and preparation method and application thereof |
| CN113354909A (en) * | 2021-06-24 | 2021-09-07 | 青岛新材料科技工业园发展有限公司 | Foaming door seal and preparation method thereof |
| CN113717459A (en) * | 2021-09-15 | 2021-11-30 | 智筑汇创(上海)新材料科技有限公司 | Thermal insulation material and preparation method thereof |
| CN115368652A (en) * | 2022-10-24 | 2022-11-22 | 北京中科海势科技有限公司 | Light and thin warm-keeping temperature-regulating modified polymer aerogel composite material and preparation method thereof |
| CN116120620A (en) * | 2023-03-07 | 2023-05-16 | 北京清冠科技有限公司 | Preparation method of low-density aerogel/polyvinyl chloride foam composite material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102875859A (en) * | 2012-09-28 | 2013-01-16 | 河北建强科技有限公司 | Nitrile butadiene rubber and polyvinyl chloride blended rubber and preparation method thereof |
| CN104223359A (en) * | 2014-08-22 | 2014-12-24 | 云南中烟工业有限责任公司 | Novel cigarette heater provided with aerogel heat-insulating layer |
| CN108129628A (en) * | 2017-12-20 | 2018-06-08 | 福建师范大学泉港石化研究院 | From fire-retardant heat insulation aqueous polyurethane composition, foaming body and preparation method thereof |
| CN109385254A (en) * | 2018-11-26 | 2019-02-26 | 同济大学 | A kind of graphene elastomeric polymer phase change composite material and preparation method thereof |
| CN110724350A (en) * | 2019-11-14 | 2020-01-24 | 航天特种材料及工艺技术研究所 | High-performance heat insulation material and preparation method thereof |
-
2020
- 2020-05-14 CN CN202010405721.6A patent/CN111471251A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102875859A (en) * | 2012-09-28 | 2013-01-16 | 河北建强科技有限公司 | Nitrile butadiene rubber and polyvinyl chloride blended rubber and preparation method thereof |
| CN104223359A (en) * | 2014-08-22 | 2014-12-24 | 云南中烟工业有限责任公司 | Novel cigarette heater provided with aerogel heat-insulating layer |
| CN108129628A (en) * | 2017-12-20 | 2018-06-08 | 福建师范大学泉港石化研究院 | From fire-retardant heat insulation aqueous polyurethane composition, foaming body and preparation method thereof |
| CN109385254A (en) * | 2018-11-26 | 2019-02-26 | 同济大学 | A kind of graphene elastomeric polymer phase change composite material and preparation method thereof |
| CN110724350A (en) * | 2019-11-14 | 2020-01-24 | 航天特种材料及工艺技术研究所 | High-performance heat insulation material and preparation method thereof |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112961656A (en) * | 2021-02-20 | 2021-06-15 | 青岛尼希米生物科技有限公司 | Composite phase-change temperature-regulating material and preparation method thereof, multiple phase-change temperature-regulating fiber and preparation method and application thereof |
| CN113354909A (en) * | 2021-06-24 | 2021-09-07 | 青岛新材料科技工业园发展有限公司 | Foaming door seal and preparation method thereof |
| CN113354909B (en) * | 2021-06-24 | 2023-09-01 | 青岛捷晟新材料科技有限公司 | Foaming door seal and preparation method thereof |
| CN113717459A (en) * | 2021-09-15 | 2021-11-30 | 智筑汇创(上海)新材料科技有限公司 | Thermal insulation material and preparation method thereof |
| CN113717459B (en) * | 2021-09-15 | 2023-10-13 | 智筑汇创(上海)新材料科技有限公司 | Thermal insulation material and preparation method thereof |
| CN115368652A (en) * | 2022-10-24 | 2022-11-22 | 北京中科海势科技有限公司 | Light and thin warm-keeping temperature-regulating modified polymer aerogel composite material and preparation method thereof |
| CN115368652B (en) * | 2022-10-24 | 2023-01-24 | 北京中科海势科技有限公司 | Light and thin warm-keeping temperature-regulating modified polymer aerogel composite material and preparation method thereof |
| US11912872B1 (en) * | 2022-10-24 | 2024-02-27 | Sycoreto Cas Co., Ltd. | Light, thin, warm-keeping and temperature-adjusting modified polymer aerogel composite material and preparation method thereof |
| CN116120620A (en) * | 2023-03-07 | 2023-05-16 | 北京清冠科技有限公司 | Preparation method of low-density aerogel/polyvinyl chloride foam composite material |
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